CN102443147A - A kind of preparation method of anti-ultraviolet, anti-aging polyester chips - Google Patents
A kind of preparation method of anti-ultraviolet, anti-aging polyester chips Download PDFInfo
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- CN102443147A CN102443147A CN2011102774361A CN201110277436A CN102443147A CN 102443147 A CN102443147 A CN 102443147A CN 2011102774361 A CN2011102774361 A CN 2011102774361A CN 201110277436 A CN201110277436 A CN 201110277436A CN 102443147 A CN102443147 A CN 102443147A
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Abstract
本发明涉及一种抗紫外线、抗老化聚酯切片的制备方法，其包括依次进行的酯化反应工序和聚合反应工序，其中：在酯化反应中引入具有较大空间位阻的第三单体；在酯化反应之后、预聚反应之前，加入高含量消光剂二氧化钛和受阻胺类光稳定剂和受阻酚类抗氧剂；在聚合反应工序的预聚合结束之后、终聚合之前，加入紫外线吸收剂；由本发明方法所得聚酯切片纺成的聚酯纤维具有优异的抗紫外线、抗老化能性能，将其织成针织及机织面料后，经测试其相关技术指标为：紫外光透过率≤5.0％，可适合户外阳光直射条件下，具有良好的防护与抗老化功能。The invention relates to a method for preparing an anti-ultraviolet and anti-aging polyester chip, which comprises an esterification reaction process and a polymerization reaction process which are carried out in sequence, wherein: a third monomer with relatively large steric hindrance is introduced into the esterification reaction; after the esterification reaction and before the prepolymerization reaction, a high-content matting agent titanium dioxide, a hindered amine light stabilizer and a hindered phenol antioxidant are added; after the prepolymerization of the polymerization reaction process is finished and before the final polymerization, an ultraviolet absorber is added; the polyester fiber spun from the polyester chip obtained by the method of the invention has excellent anti-ultraviolet and anti-aging performances, and after being woven into knitted and woven fabrics, the relevant technical indicators thereof are tested as follows: ultraviolet light transmittance is ≤5.0%, which is suitable for outdoor direct sunlight conditions and has good protection and anti-aging functions.
Description
Technical field
The present invention relates to a kind of preparation method of PET Resin/Poyester Chips Bottle Grade, the preparation method of particularly a kind of Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade.
Background technology
Since the autopolyester fiber comes out; Rely on its good intensity, good wrinkle resistance, draping property and wash and wear performance and be widely used in apparel textile; Through the tremendous development of nearly decades, the PET trevira has become at present the synthesizing polyester kind that output is maximum in the world, range of application is the widest.But trevira is compared with various natural fibers and also existed many deficiencies: feel is hardened, water absorbability is poor, anti-ultraviolet property is poor, be prone to produce static, be prone to balling-up, be difficult to dyeing etc.Though and natural fiber has good dyeing behavior, lining like cotton, real silk, hair, fiber crops etc. and has ventilation property, the absorbing sweat performance of keeping humidity is good, no static, the characteristics that comfortableness is good exist to be prone to wrinkle, to lead deficiencies such as wet and rapid-drying properties difference.
Along with the progressively expansion of trevira range of application, from the seventies in last century, developed country is to the above-mentioned deficiency of trevira; Plurality of advantages with natural fiber is a target; Aspect the wearing comfort of fiber, start with from three aspects, improve the wear behavior of trevira.On the one hand: through the innovation of spinning technique technology; Produce various differential fibre; Progressively develop thin dawn, superfine Denier fibre spining technology; Produce a series of differential spinning kinds such as sea-island fibre, tangerine lobe fiber, bicomponent composite fibre, modified cross-section fibre through composite spinning technology, make polyester fabric obtain rapid progress in function aspects such as flexibility, elasticity, emulation silks; On the other hand: through the co-blended spinning of different components, produce various fiber species, also can give lining brand-new function through the back arrangement of lining with specific function with the physical blending mode; The third aspect: through copolyreaction, improve this body structure of polyester macromolecule chain, through introducing the copolymerization component group to improve trevira lining performance, permanently give fiber various properties.At present, comprise fire-retardant, cation-dyeable, highly shrink, a series of functional polyalkylene ester fibers such as dispersed dye are prone to dye, antistatic, Ginkgo Biloba Leaf Extract, far infrared thermal insulation that trevira and lining are segmented market has produced material impact.
The chemical fibre market of China is through reform and opening-up rapid progress in decades; In 68% level that has reached Gross World Product aspect the normal polyester fiber production; But in the development and application field of functional polyalkylene ester fiber, China also is in the starting stage at present, is limited to the exploitation of single functional polyester and fiber at present more; Like anti-ultraviolet polyester fiber, anti-static polyester fiber etc.And for the exploitation with complex function, high added value functional fiber, then also need the scientific research personnel badly and make a breakthrough in the multifunctional composite fiber field.
Notification number is that the Chinese invention patent of CN1204196C discloses a kind of uvioresistant zinc oxide complex polyester and preparation method thereof; This method at first prepares the suspension-s of anti ultraviolet agent midbody zinc subcarbonate terepthaloyl moietie; Then before the PET polyester synthetic esterification stage finishes back, rough vacuum polymerization; The suspension-s of anti ultraviolet agent midbody zinc subcarbonate terepthaloyl moietie is added, and when polyreaction generated polyester, zinc subcarbonate decomposed generation zinc oxide; Obtain Ginkgo Biloba Leaf Extract zinc oxide complex polyester, wherein zinc oxide content is 0.1%～5% of a PET Resin/Poyester Chips Bottle Grade weight.In this method gained polyester, zinc oxide can keep less granularity, strengthens thereby absorb ultraviolet performance.Yet this method is decomposed in order to make zinc subcarbonate, must make to be aggregated in more than 285 ℃ and carry out; And zinc subcarbonate will resolve into carbonic acid gas, water and zinc oxide, and in whole collecting process, carbonic acid gas can influence vacuum tightness and cause section to contain great amount of bubbles on the one hand; Polycondensation final stage on the other hand, produces large quantity of moisture can produce DeR; Have a strong impact on quality product, simultaneously, the zinc subcarbonate that does not decompose fully will continue to decompose in spinning process; The fiber spinnability variation, breaking tenacity reduces.
Publication number is that the Chinese invention patent application of CN101864067A discloses a kind of preparation method with polyester of anti-ultraviolet function, and it comprises the manufacturing of (1) compound anti ultraviolet agent: compound anti ultraviolet agent is made up of agent of inorganic anti ultraviolet shielding and organic uv absorbers; The composition of inorganic anti ultraviolet shielding agent is nano level TiO
2And Al
2O
3Or SiO
2Inorganic oxide; Organic uv absorbers is the benzotriazole category organic substance; The weight ratio of agent of inorganic anti ultraviolet shielding and organic uv absorbers is 1: 1, takes by weighing this compound anti ultraviolet agent and terepthaloyl moietie and is made into slurries, places ball mill to disperse then 0.5-1 hour; (2), the esterification operation: fused terephthalic acid and terepthaloyl moietie, continuously or the intermittent entry esterifying kettle,, carry out esterification under the pressure 0.3Mpa 160～220 ℃ of temperature, water byproduct to be steamed reaches 90% o'clock of theoretical amount, esterification stops; (3) polyreaction operation: obtain terephthalic acid dihydroxyl ethyl ester monomer after the esterification operation; Add compound anti ultraviolet agent; Add catalyst acetic acid antimony simultaneously, send into polymerization process, in terephthalic acid weight %; The catalyzer add-on is 0.03-0.04%, and the add-on of compound anti ultraviolet agent is at 1.5-2.0%; Monomer earlier carries out prepolymerization under 215～225 ℃ of normal pressures in polymeric kettle, then in absolute pressure less than 150pa, carry out polymerization under 285 ± 2 ℃ of the temperature, impel reaction to reach certain polymerization degree, the terepthaloyl moietie of generation reclaims behind condensing surface; (4) after condensation reaction finished, material made the uvioresistant polyester section through Cast Strip, cooling, pelletizing, drying.The deficiency of this method is: benzotriazole is an organic phenolic compound, exists as the protonic acid form under the hot conditions, can destroy inorganic nanometer powder TiO
2And Al
2O
3Or SiO
2Surperficial organic agent, cause the reunion of inorganic nanometer powder in the pre-polymerization process.In addition, because inorganic nanometer powder in polymerization process, continues 4～6 hours time under hot conditions; Nanoparticle generation agglomeration is obvious, and under low temperature ultra-dispersed condition, the inorganic nano ion is to make light when passing lining, produce strong diffuse scattering effect with huge specific surface area; Reach anti-ultraviolet purpose, but through after the long pyroreaction, inorganic nanometer powder is originally reunited in a large number and has been formed micro-size particles; Diffuse scattering effect to light significantly reduces, and in addition, this method adds the benzotriazole type organic before prepolymerization reaction; In the prepolymerization reaction process, can be drawn out of system because of a large amount of EG evaporations.
Notification number is that the Chinese invention patent of CN100503910C discloses a kind of Nano titanium nitride anti-ultraviolet polyester fiber, and it is through master batch method spinning uvioresistant fiber.Notification number is that the Chinese invention patent of CN1300246C discloses the method that a kind of original position generation nano titanium oxide prepares uvioresistant polyester, though terepthaloyl moietie salt of its preparation titanium carries out surface treatment through organic agent or silane coupling agent, titanium ethylene glycolate is as polymerizing catalyst; The PET polyreaction had strong katalysis and side reaction Degradation; Be prone to cause PET section hue difference, MWD wide, in addition, in-situ hydrolysis generates Nano titanium dioxide in the polymerization process; The water molecules of the decomposition in polymerization later stage generation has a strong impact on polyreaction on the one hand; On the other hand, the Nano titanium dioxide that this method is processed is good organic matter of sewage decompose material, and section is after long-time solar radiation; Viscosity degradation produces and decomposes.Publication number is the application for a patent for invention of CN101864067A, discloses anti-ultraviolet superfine terylene and preparation method thereof, is a kind of Ginkgo Biloba Leaf Extract additive co-blended spinning technology of crossing through coupling agent treatment.Notification number is that the patent of invention of CN101735578B discloses a kind of fire-retardant Ginkgo Biloba Leaf Extract matrix material and preparation method thereof, use be to be ultraviolet scattering material with the inorganic nano ultraviolet ray-resistant material, produce certain Ginkgo Biloba Leaf Extract effect.
To sum up; Thereby prior art mainly all is the huge specific surface area that relies on inorganic nanometer powder to have produces the Ginkgo Biloba Leaf Extract effect for the basis produces diffuse scattering to ultraviolet ray; The stability of uvioresistant effect and efficient remain to be improved; This just need start with from Ginkgo Biloba Leaf Extract mechanism, the polyester that preparation has more excellent uvioresistant effect and has good spinnability.In addition, also need exploitation badly when having anti-ultraviolet function, have other function for example resistance to deterioration, absorbing fast-drying property concurrently, static resistance, the complex function polyester of anti-pilling.
Summary of the invention
Technical problem to be solved by this invention is the deficiency that overcomes prior art, and the preparation method of a kind of Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade is provided.
For solving above technical problem, the present invention takes following technical scheme:
The preparation method of a kind of Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade comprises the esterification operation and the polyreaction operation of carrying out successively, wherein:
Said esterification operation is implemented as follows: terephthalic acid, terepthaloyl moietie and the 3rd monomer are joined in the reaction kettle of the esterification; Under 250 ℃～265 ℃, carry out esterification; The molar ratio of said terephthalic acid, terepthaloyl moietie is 1: 1.2～1.3; Described the 3rd monomer is for being selected from m-phthalic acid, 1; 4-cyclohexane cyclohexanedimethanodibasic, oreinol dioctyl phthalate, NSC 6366 and 2, one or more in the 3-butyleneglycol, and its add-on is 0.3%～3.5% of a terephthalic acid weight;
Said polyreaction operation is implemented as follows: after the esterification operation is accomplished; At first add weight and be 0.5%～2.6% titanium oxide matting agent of PET Resin/Poyester Chips Bottle Grade weight; Add polymerizing catalyst then; Add the hindered amine light stabilizer of 10～300ppm (weight with PET Resin/Poyester Chips Bottle Grade is benchmark) and the Hinered phenols antioxidant of 10～300ppm (weight with PET Resin/Poyester Chips Bottle Grade is benchmark) simultaneously, deliver to prepolymerization kettle after stirring and carry out prepolymerization reaction; Prepolymerization reaction is closed vacuum system, under nitrogen protection and negative pressure after finishing; Liquid state or fused UV light absorber are injected, mixed, after the pre-polymerization strainer filters; Get into terminal polymerization kettle, the add-on of said UV light absorber is 0.1%～2.0% of a PET Resin/Poyester Chips Bottle Grade weight; At last, in terminal polymerization kettle, pressure 40～100pa carries out the final polymerization reaction under 270 ℃～285 ℃ of the temperature, after the final polymerization reaction is accomplished, the discharging pelletizing, Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade.
According to the present invention, described the 3rd monomer is preferably m-phthalic acid, 1,4 cyclohexanedicarboxylic acid, oreinol dioctyl phthalate, NSC 6366 and 2, the combination more than two kinds in the 3-butyleneglycol, the for example combination of m-phthalic acid and NSC 6366.
According to the present invention, described UV light absorber can be one or more the combination in the UV light absorber of following kind: benzotriazole category UV light absorber:
326,
234,
350,
320,
328; Low volatility benzotriazole category UV light absorber
360; Red shift benzotriazole category UV light absorber
327; And
UV-P; The special UV light absorber CYASORB of cyanogen UV-3638F; Triazine series UV light absorber UV-1577, the preferred add-on of UV light absorber is 0.15%～1.10% of a PET Resin/Poyester Chips Bottle Grade weight.Preferably, select one or more compound uses of following UV light absorber: benzotriazole category UV light absorber:
234,
320,
328; Low volatility benzotriazole category UV light absorber
360; Red shift benzotriazole category UV light absorber
327; And
UV-P; The special UV light absorber CYASORB of cyanogen UV-3638F, triazine series UV light absorber UV-1577 etc.Preferred especially, select one or more compound uses of the UV light absorber of following kind: the benzotriazole category UV light absorber:
234,
320,
328; And
UV-P, the special UV light absorber CYASORB of cyanogen UV-3638F.Add UV light absorber churning time afterwards and be preferably 3～8 minutes.
According to the present invention; Described hindered amine light stabilizer can be for being selected from non-aggretion type high molecular weight hindered amine light stabilizer
119FL; 770 pairs (2 of polymerized hindered amine photostabilizer Chimassorb944, Tinuvin 788 and photostabilizers; 2; 6; 6-tetramethyl-4-piperidyl) one or more in the sebate; Being preferably the composite light stabilizer that photostabilizer mixes more than two kinds, for example is Tinuvin 788 and the mixture of
119FL by weight 1: 1.The add-on of described hindered amine light stabilizer is preferably 15～90ppm (is benchmark with PET Resin/Poyester Chips Bottle Grade weight).Described Hinered phenols antioxidant can be Irganox 1076; Among Irganox 1010 and the Irgafos168 one or more; Be preferably the composite antioxidant that the oxidation inhibitor more than two kinds mixes, for example Irganox1076 and Irganox 1010 were by weight 1: 3 mixture.The add-on of Hinered phenols antioxidant is 30～250ppm (is benchmark with PET Resin/Poyester Chips Bottle Grade weight).Preferably, the add-on of hindered amine light stabilizer is 35～60ppm, and the add-on of Hinered phenols antioxidant is 75～180ppm.A certain amount of hindered amine light stabilizer and Hinered phenols antioxidant can produce synergistic effect with UV light absorber as auxiliary component, have guaranteed that polyester has good photostabilization and antioxidant property.
According to the present invention, polymerizing catalyst can be that known various polyester is used polymerizing catalyst.Particularly in the present invention, polymerizing catalyst uses antimony glycol, and its add-on is generally 450～550ppm (weight with PET Resin/Poyester Chips Bottle Grade is benchmark).
The material chemical property of gained PET Resin/Poyester Chips Bottle Grade according to the present invention can be spun into three leaves or modified cross-section fibre such as cross special-shaped with PET Resin/Poyester Chips Bottle Grade.Compare decline to some extent with conventional PET polyester according to its fusing point of PET Resin/Poyester Chips Bottle Grade of gained of the present invention, in spinning process, spinning condition is adjusted, implement the more common PTT trevira of condition of spinning, screw rod is respectively distinguished 8～15 ℃ of temperature downward modulations.Corresponding drawing and setting temperature also will be reduced.Those skilled in the art can adjust corresponding spinning condition according to the fusing point of concrete PET Resin/Poyester Chips Bottle Grade.
Because the utilization of technique scheme, the present invention compared with prior art has following advantage:
1, to Ginkgo Biloba Leaf Extract, anti-aging copolyesters and fiber thereof in the prior art in exploitation and use; Use inorganic nano material; Through increasing the specific surface area light reflection ultraviolet, reach anti-ultraviolet function, existing under the pyroreaction condition nanoparticle very easily reunite, the unsettled deficiency of product effect; The invention provides a kind of and anti-ultraviolet polyester fiber prior art has the uvioresistant mechanism of obvious difference aspect mechanism; Promptly being through in the polyester building-up process, is main with UV light absorber, the ultraviolet light in the sunlight is converted to the light of other wavelength; And auxiliary with the penetrating amount of high-load titanium oxide matting agent reduction sunlight, further improved polyester Ginkgo Biloba Leaf Extract effect.
2, with after esterification, promptly to add anti ultraviolet agent different in the past; The present invention is after prepolymerization reaction is accomplished, and gathers eventually to add liquid or fused UV light absorber before reaction is carried out, so; Effectively reduce the residence time of UV light absorber; And significantly reduce the volatilization of UV light absorber, because melt kinematic viscosity after prepolymerization reaction is accomplished is less, also guaranteed UV light absorber good dispersion effect in melt simultaneously.
3, the present invention adds a certain amount of photostabilizer and inhibitor, they and UV light absorber are collaborative, has improved the made fabric lining of the polyester ageing resistance under the sunlight direct projection condition out of doors.Compare with anti-ultraviolet polyester in the past, this product good spinnability in spinning process, intensity is high, even dyeing, row yielding is high.
4, the present invention's interpolation has than large space sterically hindered the 3rd monomer; Reduced the crystal property of trevira; Prevent that out of doors the fiber predisposition is led the strength degradation that crystallization causes under the condition; Lining is eliminated because of crystallization causes the influence of lining intensity reduction under the sunlight direct projection condition out of doors, improved the endurable performance of clothes.
5, the prepared PET Resin/Poyester Chips Bottle Grade of the present invention can be spun into spring and summer clothes and use trevira; Have good Ginkgo Biloba Leaf Extract, anti-aging function; To be made into knitting and woven fabric by the fiber of this PET Resin/Poyester Chips Bottle Grade preparation; Through its correlation technique index of test be: uv transmittance≤5.0% can be fit to have favorable protection and anti-aging function under the outdoor sunlight direct projection condition.As the various modified cross-section fibres of weaving, can give fiber good hydroscopic fast-drying function, lining is through test, measure wicking height >=120mm, vaporator rate >=0.20g/hr.
Embodiment
The present invention relates to the preparation method of Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade.In the process of synthetic polyethylene terephthalate; Use a certain amount of UV light absorber as trevira Ginkgo Biloba Leaf Extract additive major constituent; This UV light absorber comprises one or more compound uses that mainly are adapted to the polyester interpolation, and its add-on is 0.1～2.0% of a PET Resin/Poyester Chips Bottle Grade weight.For guaranteeing that polyester has good photostabilization and antioxidant property; UV light absorber and a certain amount of hindered amine light stabilizer and Hinered phenols antioxidant are used as auxiliary component; Produce synergistic effect; Make lining have anti-aging function out of doors, such promoter addition is controlled at 10～300ppm respectively.Simultaneously, use m-phthalic acid, 1,4 cyclohexanedicarboxylic acid, NSC 6366 etc. to have than large space sterically hindered diprotic acid or divalent alcohol as reducing the fibre crystallinity modified component, add-on is 0.3～3.5% of terephthalic acid (PTA) weight; And adding high-content titanium oxide matting agent, content is 0.5～2.6%, when playing photoextinction, reduces light penetration, has further improved the anti-ultraviolet function of product.Can adopt the normal polyester production technique to produce, special, UV light absorber with liquid state or molten state injected system, gets into terminal polymerization kettle after filtering and accomplishes polyreaction after prepolymerization reaction is accomplished, and promptly gets Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade.This PET Resin/Poyester Chips Bottle Grade spins three leaves or the trevira with good Ginkgo Biloba Leaf Extract, absorbing fast-drying complex function such as cross special-shaped through the spinning jet of crystallization in advance, drying, use particular design.
Below in conjunction with specific embodiment the present invention is done further detailed explanation, but the present invention is not limited to following examples.
Embodiment 1
Present embodiment provides the preparation method of a kind of Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade, and it comprises the steps:
(1), esterification operation: get 18kg pure terephthalic acid (PTA), 0.45kg m-phthalic acid, 0.05kg NSC 6366,7.05kg terepthaloyl moietie (EG) add in 70 liters of reaction kettle of the esterification, after stirring; Begin to heat up and be forced into 0.3Mpa; Carry out esterification, esterification temperature is controlled at 250 ℃～265 ℃, finishes to the esterification water outlet; Reply normal pressureization, finish to react polymerization single polymerization monomer.
(2), polyreaction operation: after esterification is accomplished; At first add the titanium oxide matting agent; Add-on is 1.5% of a PET Resin/Poyester Chips Bottle Grade weight; Add polymerizing catalyst then; And add 1.125g composite light stabilizer (Tinuvin 788 mixes by weight 1: 1 with
119FL), 3.375g composite antioxidant (Irganox 1076 and Irganox 1010 mix by weight 1: 3).Deliver to prepolymerization kettle intensification polymerization after stirring, 260 ℃～275 ℃ of controlled temperature, open vacuum pump; In 40 minutes, slowly reduce to 2Kpa, the rough vacuum polyreaction finishes, and closes vacuum system; Under nitrogen protection and negative pressure condition,,, mix after 5 minutes by the specific equipment injected system with 113g benzotriazole category UV light absorber
234 liquid or that fusion is good; After the pre-polymerization strainer filters, get into terminal polymerization kettle, open high vacuum, pressure is 40～100pa; Under 270 ℃～285 ℃ conditions, carry out conventional polymerization; To reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction is accomplished; Obtain Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade 22.5kg, its test result is seen table 1.
Embodiment 2
Present embodiment provides the preparation method of a kind of Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade, and it comprises the steps:
(1), esterification operation: get 18kg pure terephthalic acid (PTA), 0.45kg1,4-cyclohexane cyclohexanedimethanodibasic, 0.05kg NSC 6366,70 liters of reaction kettle of the esterification of 7.05kg terepthaloyl moietie (EG) adding; After stirring, begin to heat up and be forced into 0.3Mpa, carry out esterification; Esterification temperature is controlled at 250 ℃～265; Finish to the esterification water outlet, reply normal pressureization, finish to react polymerization single polymerization monomer.
(2), polyreaction operation: after esterification is accomplished; At first add the titanium oxide matting agent; Add-on is 1.5% of a PET Resin/Poyester Chips Bottle Grade weight; Add polymerizing catalyst then; And add 1.125g composite light stabilizer (Tinuvin 788 mixes by weight 1: 1 with
119FL), 3.375g composite antioxidant (Irganox 1076 and Irganox 1010 mix by weight 1: 3).Deliver to prepolymerization kettle intensification polymerization after stirring, 260 ℃～275 ℃ of controlled temperature, open vacuum pump; In 40 minutes, slowly reduce to 2Kpa, the rough vacuum polyreaction finishes, and closes vacuum system; Under nitrogen protection and negative pressure condition,,, mix after 5 minutes by the specific equipment injected system with 226g benzotriazole category UV light absorber
234 liquid or that fusion is good; After the pre-polymerization strainer filters, get into terminal polymerization kettle, open high vacuum, pressure is 40～100pa; Under 270 ℃～285 ℃ conditions, carry out conventional polymerization; To reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction is accomplished; Obtain Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade 22.5kg, its test result is seen table 1.
Embodiment 3
Present embodiment provides the preparation method of a kind of Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade, and it comprises the steps:
(1), esterification operation: get 18kg pure terephthalic acid (PTA), 0.45kg m-phthalic acid, 0.05kg NSC 6366,7.05kg terepthaloyl moietie (EG) add 70 liters of reaction kettle of the esterification, after stirring; Begin to heat up and be forced into 0.3Mpa; Carry out esterification, esterification temperature is controlled at 250 ℃～265 ℃, finishes to the esterification water outlet; Reply normal pressureization, finish to react polymerization single polymerization monomer.
(2), polyreaction operation: after esterification is accomplished; At first add the titanium oxide matting agent; Add-on is 1.5% of a PET Resin/Poyester Chips Bottle Grade weight; Add polymerizing catalyst then; And add 1.125g composite light stabilizer (Tinuvin 788 mixes by weight 1: 1 with
119FL), 3.375g composite antioxidant (Irganox 1076 and Irganox 1010 mix by weight 1: 3).Deliver to prepolymerization kettle intensification polymerization after stirring, 260 ℃～275 ℃ of controlled temperature, open vacuum pump; In 40 minutes, slowly reduce to 2Kpa, the rough vacuum polyreaction finishes, and closes vacuum system; Under nitrogen protection and negative pressure condition,,, mix after 5 minutes by the specific equipment injected system with 113g UV light absorber
320 liquid or that fusion is good; After the pre-polymerization strainer filters, get into terminal polymerization kettle, open high vacuum, pressure is 40～100pa; Under 270 ℃～285 ℃ conditions, carry out conventional polymerization; To reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction is accomplished; Obtain Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade 22.5kg, its test result is seen table 1.
Embodiment 4
Present embodiment provides the preparation method of a kind of Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade, and it comprises the steps:
(1), esterification operation: get 18kg pure terephthalic acid (PTA), 0.45kg 1,4 cyclohexanedicarboxylic acid, 0.05kg NSC 6366,7.05kg terepthaloyl moietie (EG) add 70 liters of reaction kettle of the esterification; After stirring, begin to heat up and be forced into 0.3Mpa, carry out esterification; Esterification temperature is controlled at 250 ℃～265 ℃; Finish to the esterification water outlet, reply normal pressureization, finish to react polymerization single polymerization monomer.
(2) polyreaction operation: after esterification is accomplished; At first add the titanium oxide matting agent; Add-on is 1.5% of a PET Resin/Poyester Chips Bottle Grade weight; Add polymerizing catalyst then; And add 1.125g composite light stabilizer (Tinuvin 788 mixes by weight 1: 1 with
119FL), 3.375g composite antioxidant (Irganox 1076 and Irganox 1010 mix by weight 1: 3).Deliver to prepolymerization kettle intensification polymerization after stirring, 260 ℃～275 ℃ of controlled temperature, open vacuum pump; In 40 minutes, slowly reduce to 2Kpa, the rough vacuum polyreaction finishes, and closes vacuum system; Under nitrogen protection and negative pressure condition,,, mix after 5 minutes by the specific equipment injected system with 226g UV light absorber
320 liquid or that fusion is good; After the pre-polymerization strainer filters, get into terminal polymerization kettle, open high vacuum, pressure is 40～100pa; Under 270 ℃～285 ℃ conditions, carry out conventional polymerization; To reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction is accomplished; Obtain Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade 22.5kg, its test result is seen table 1.
Embodiment 5
Present embodiment provides the preparation method of a kind of Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade, and it comprises the steps:
(1), esterification operation: get 18kg pure terephthalic acid (PTA), 0.45kg m-phthalic acid, 0.05kg NSC 6366,7.05kg terepthaloyl moietie (EG) add 70 liters of reaction kettle of the esterification, after stirring; Begin to heat up and be forced into 0.3Mpa; Carry out esterification, esterification temperature is controlled at 250 ℃～265 ℃, finishes to the esterification water outlet; Reply normal pressureization, finish to react polymerization single polymerization monomer.
(2), polyreaction operation: after esterification is accomplished; At first add the titanium oxide matting agent; Add-on is 1.0% of a PET Resin/Poyester Chips Bottle Grade weight; Add polymerizing catalyst then; And add 1.125g composite light stabilizer (Tinuvin 788 mixes by weight 1: 1 with
119FL), 3.375g composite antioxidant (Irganox 1076 and Irganox 1010 mix by weight 1: 3).Deliver to prepolymerization kettle intensification polymerization after stirring, 260 ℃～275 ℃ of controlled temperature, open vacuum pump; In 40 minutes, slowly reduce to 2Kpa; The rough vacuum polyreaction finishes, and closes vacuum system, under nitrogen protection and negative pressure condition with liquid or fusion is good the 113g UV light absorber (mixture of
234 and
320; The ratio of the two weight is 1: 1); By the specific equipment injected system, mix after 5 minutes,, the pre-polymerization strainer gets into terminal polymerization kettle after filtering; Open high vacuum; Pressure is 40～100pa, under 270 ℃～285 ℃ conditions, carries out conventional polymerization, to reaching regulation viscosity; Stop polyreaction; Discharging pelletizing after polyreaction is accomplished obtains Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade 22.5kg, and its test result is seen table 1.
Embodiment 6
Present embodiment provides the preparation method of a kind of Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade, and it comprises the steps:
(1), esterification operation: get 18kg pure terephthalic acid (PTA), 0.45kg m-phthalic acid, 0.05kg NSC 6366,7.05kg terepthaloyl moietie (EG) add 70 liters of reaction kettle of the esterification, after stirring; Begin to heat up and be forced into 0.3Mpa; Carry out esterification, esterification temperature is controlled at 250 ℃～265 ℃, finishes to the esterification water outlet; Reply normal pressureization, finish to react polymerization single polymerization monomer.
(2), polyreaction operation: after esterification is accomplished; At first add the titanium oxide matting agent; Add-on is 1.0% of a PET Resin/Poyester Chips Bottle Grade weight; Add polymerizing catalyst then; And add 1.125g composite light stabilizer (Tinuvin 788 mixes by weight 1: 1 with
119FL), 3.375g composite antioxidant (Irganox 1076 and Irganox 1010 mix by weight 1: 3).Deliver to prepolymerization kettle intensification polymerization after stirring, 260～275 ℃ of controlled temperature, open vacuum pump; In 40 minutes, slowly reduce to 2Kpa; The rough vacuum polyreaction finishes, and closes vacuum system, under nitrogen protection and negative pressure condition with 226g UV light absorber (
234 and
320 mixtures liquid or that fusion is good; The ratio of the two weight is 1: 1); By the specific equipment injected system, mix after 5 minutes,, the pre-polymerization strainer gets into terminal polymerization kettle after filtering; Open high vacuum; Pressure is 40～100pa, under 270 ℃～285 ℃ conditions, carries out conventional polymerization, to reaching regulation viscosity; Stop polyreaction; Discharging pelletizing after polyreaction is accomplished obtains Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade 22.5kg, and its test result is seen table 1.
Embodiment 7
Present embodiment provides the preparation method of a kind of Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade, and it comprises the steps:
(1), esterification operation: get 18kg pure terephthalic acid (PTA), 0.45kg m-phthalic acid, 0.05kg NSC 6366,7.05kg terepthaloyl moietie (EG) add in 70 liters of reaction kettle of the esterification, after stirring; Begin to heat up and be forced into 0.3Mpa; Carry out esterification, esterification temperature is controlled at 250～265 ℃, finishes to the esterification water outlet; Reply normal pressureization, finish to react polymerization single polymerization monomer.
(2), polyreaction operation: after esterification is accomplished; At first add the titanium oxide matting agent; Add-on is 1.0% of a PET Resin/Poyester Chips Bottle Grade weight; Add polymerizing catalyst then; And add 1.125g composite light stabilizer (Tinuvin 788 mixes by 1: 1 with
119FL weight ratio), 3.375g composite antioxidant (Irganox 1076 and Irganox 1010 mix by weight 1: 3)).Deliver to prepolymerization kettle intensification polymerization after stirring, 260 ℃～275 ℃ of controlled temperature, open vacuum pump; In 40 minutes, slowly reduce to 2Kpa, the rough vacuum polyreaction finishes, and closes vacuum system; Under nitrogen protection and negative pressure condition with 113g UV light absorber (
234 and the special UV light absorber CYASORB of cyanogen UV-3638F, the ratio of the two weight is 2: 1) liquid or that fusion is good, by the specific equipment injected system; Mix after 5 minutes; After the pre-polymerization strainer filters, get into terminal polymerization kettle, open high vacuum, pressure is 40～100pa; Under 270 ℃～285 ℃ conditions, carry out conventional polymerization; To reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction is accomplished; Obtain Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade 22.5kg, its test result is seen table 1.
Embodiment 8
Present embodiment provides the preparation method of a kind of Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade, and it comprises the steps:
(1), esterification operation: get 18kg pure terephthalic acid (PTA), 0.45kg m-phthalic acid, 0.05kg NSC 6366,7.05kg terepthaloyl moietie (EG) add 70 liters of reaction kettle of the esterification, after stirring; Begin to heat up and be forced into 0.3Mpa; Carry out esterification, esterification temperature is controlled at 250 ℃～265 ℃, finishes to the esterification water outlet; Reply normal pressureization, finish to react polymerization single polymerization monomer.
(2), polyreaction operation: after esterification is accomplished; At first add the titanium oxide matting agent; Add-on is 1.0% of a PET Resin/Poyester Chips Bottle Grade weight; Add polymerizing catalyst then; And add 1.125g composite light stabilizer (Tinuvin 788 mixes by weight 1: 1 with
119FL), 3.375g composite antioxidant (Irganox 1076 and Irganox 1010 mix by weight 1: 3).Deliver to prepolymerization kettle intensification polymerization after stirring, 260 ℃～275 ℃ of controlled temperature, open vacuum pump; In 40 minutes, slowly reduce to 2Kpa, the rough vacuum polyreaction finishes, and closes vacuum system; Under nitrogen protection and negative pressure condition with liquid or fusion is good 226g UV light absorber (mixture of
234 and the special UV light absorber CYASORB of cyanogen UV-3638F, the ratio of the two weight is 2: 1), by the specific equipment injected system; Mix after 5 minutes; After the pre-polymerization strainer filters, get into terminal polymerization kettle, open high vacuum, pressure is 40～100pa; Under 270～285 ℃ of conditions, carry out conventional polymerization; To reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction is accomplished.Obtain Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade 22.5kg, its test result is seen table 1.
Comparative Examples 1
This Comparative Examples provides a kind of preparation method of PET Resin/Poyester Chips Bottle Grade, and it comprises the steps:
(1), esterification operation: get 18kg pure terephthalic acid (PTA), 0.45kg m-phthalic acid, 0.05kg NSC 6366,7.05kg terepthaloyl moietie (EG) add 70 liters of reaction kettle of the esterification, after stirring; Begin to heat up and be forced into 0.3Mpa; Carry out esterification, esterification temperature is controlled at 250～265 ℃, finishes to the esterification water outlet; Reply normal pressureization, finish to react polymerization single polymerization monomer.
(2), polyreaction operation: after esterification is accomplished; At first add the titanium oxide matting agent; Add-on is 1.5% of a PET Resin/Poyester Chips Bottle Grade weight; Add polymerizing catalyst then; And add 1.125g composite light stabilizer (Tinuvin 788 mixes by weight 1: 1 with
119FL), 3.375g composite antioxidant (Irganox 1076 and Irganox 1010 mix by weight 1: 3).With 113g UV light absorber
234 liquid or that fusion is good,, mix after 5 minutes by the specific equipment injected system; 260～275 ℃ of controlled temperature, the open vacuum pump was slowly reduced to 2Kpa in 40 minutes; The rough vacuum polyreaction finishes, and opens high vacuum, and pressure is 40～100pa; Under 270～285 ℃ of conditions, carry out conventional polymerization; To reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction is accomplished; Obtain PET Resin/Poyester Chips Bottle Grade 22.5kg, its test result is seen table 1.
Comparative Examples 2
This Comparative Examples provides a kind of preparation method of PET Resin/Poyester Chips Bottle Grade, and it comprises the steps:
(1), esterification operation: get 18kg pure terephthalic acid (PTA), 0.45kg m-phthalic acid, 0.05kg NSC 6366,7.05kg terepthaloyl moietie (EG) add 70 liters of reaction kettle of the esterification, after stirring; Begin to heat up and be forced into 0.3Mpa; Carry out esterification, esterification temperature is controlled at 250～265 ℃, finishes to the esterification water outlet; Reply normal pressureization, finish to react polymerization single polymerization monomer.
(2), polyreaction operation: after esterification is accomplished; At first add the titanium oxide matting agent; Add-on is 1.5% of a PET Resin/Poyester Chips Bottle Grade weight; Add polymerizing catalyst then; And add 1.125g composite light stabilizer (Tinuvin 788 mixes by weight 1: 1 with
119FL), 3.375g composite antioxidant (Irganox 1076 and Irganox 1010 mix by weight 1: 3).With 113g UV light absorber (mixture of the special UV light absorber CYASORBUV-3638F of
234 and cyanogen, the ratio of the two weight is 2: 1) liquid or that fusion is good, by the specific equipment injected system; Mix after 5 minutes 260～275 ℃ of controlled temperature, open vacuum pump; In 40 minutes, slowly reduce to 2Kpa, the rough vacuum polyreaction finishes, and opens high vacuum; Pressure is 40～100pa, under 270～285 ℃ of conditions, carries out conventional polymerization, to reaching regulation viscosity; Stop polyreaction; Discharging pelletizing after polyreaction is accomplished obtains PET Resin/Poyester Chips Bottle Grade 22.5kg, and its test result is seen table 1.
The physical and chemical index of table 1 Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade
The quality index of the section through contrast the foregoing description and Comparative Examples can be found out; The PET Resin/Poyester Chips Bottle Grade of the present invention's preparation has kept the quality index of conventional PET PET Resin/Poyester Chips Bottle Grade basically, shows that the preparation method is reasonable, and in the Comparative Examples 1,2; Because the adding of UV light absorber; Caused the obvious flavescence of section form and aspect, fusing point and second-order transition temperature raise, and show that the part UV light absorber takes system in the rough vacuum stage out of with a large amount of evaporations of terepthaloyl moietie.
PET Resin/Poyester Chips Bottle Grade with the foregoing description 1～8 and Comparative Examples 1～2 is a raw material respectively; Make trevira through preparatory crystallization, drying, spinning, coiling, drawing and setting successively; Different with common PET polyester spinning technique, this section is owing to add modification UV light absorber, photostabilizer, oxidation inhibitor, the 3rd monomer and high-load titanium oxide matting agent, and its section second-order transition temperature is lower; Therefore must just can implement chip drying through preparatory crystallization.
Above-mentioned preparation method is specific as follows: at first PET Resin/Poyester Chips Bottle Grade is carried out preparatory crystallization, 110 ℃～125 ℃ of Tc controls, time are 3～5 hours in advance.Carry out drying then, 130 ℃～145 ℃ of drying temperatures, the time is 3.5～5.0 hours.Carry out spinning after accomplishing drying.Use special crosssection spinning jets such as three leaves, cross, five leaves.At first will spin the pre-oriented yarn (POY) of corresponding product, spinning temperature is controlled at 255 ℃～278 ℃, (because a large amount of modified additives are used in this section; The section fusing point descends, in spinning process, and be according to the fusing point of copolyester section; Spinning and condition are adjusted; The condition of implementing spinning compares the common PET trevira, and screw rod is respectively distinguished 8～15 ℃ of temperature downward modulations), POY fiber sprinning speed 2850m/min.The POY fiber of spinning stretches and texturing craft through corresponding through after 24 hours balances again, and draft temperature is 142 ℃～150 ℃, prepares corresponding drawing and setting temperature and also will reduce.The preparation specification is 40～111dtex/24～96f, have the low stretch network product of hydroscopic fast-drying function.Fiber quality is good.At last, trevira is through the knitting and woven lining of processing, and the performance of lining is seen table 2.
Table 2 trevira lining performance
Visible from table 2, according to the prepared lining of polyester of the present invention, its ultraviolet ray transmissivity significantly reduces, and anti-ultraviolet property is good.Generally speaking, uv transmittance≤5.0%, measure wicking height>=120mm, vaporator rate>=0.20g/hr is particularly suitable for making spring, summer fashionable dress.
Fiber according to PET Resin/Poyester Chips Bottle Grade of the present invention was spun into also can be used for making parasols, and curtain etc. have good result of use.
More than the present invention has been done detailed description, all equivalences of doing according to spirit of the present invention change or modify, and all should be encompassed in protection scope of the present invention.
Claims (10)
1. the preparation method of a Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade comprises the esterification operation and the polyreaction operation of carrying out successively, it is characterized in that:
Said esterification operation is implemented as follows: terephthalic acid, terepthaloyl moietie and the 3rd monomer are joined in the reaction kettle of the esterification; Under 250 ℃～265 ℃, carry out esterification; The molar ratio of said terephthalic acid, terepthaloyl moietie is 1: 1.2～1.3, and described the 3rd monomer is for being selected from m-phthalic acid, 1,4 cyclohexanedicarboxylic acid, oreinol dioctyl phthalate, NSC 6366 and 2; In the 3-butyleneglycol one or more, and its add-on is 0.3～3.5% of a terephthalic acid weight;
Said polyreaction operation is implemented as follows: after the esterification operation is accomplished; At first add weight and be 0.5%～2.6% titanium oxide matting agent of PET Resin/Poyester Chips Bottle Grade weight; Add polymerizing catalyst then; Add the hindered amine light stabilizer of 10～300ppm (weight with PET Resin/Poyester Chips Bottle Grade is benchmark) and the Hinered phenols antioxidant of 10～300ppm (weight with PET Resin/Poyester Chips Bottle Grade is benchmark) simultaneously, deliver to prepolymerization kettle after stirring and carry out prepolymerization reaction; Prepolymerization reaction is closed vacuum system, under nitrogen protection and negative pressure after finishing; Liquid state or fused UV light absorber are injected, mixed, after the pre-polymerization strainer filters; Get into terminal polymerization kettle, the add-on of said UV light absorber is 0.1%～2.0% of a PET Resin/Poyester Chips Bottle Grade weight; At last, in terminal polymerization kettle, pressure 40～100pa carries out the final polymerization reaction under 270 ℃～285 ℃ of the temperature, after the final polymerization reaction is accomplished, the discharging pelletizing, said Ginkgo Biloba Leaf Extract, anti-aging PET Resin/Poyester Chips Bottle Grade.
2. the preparation method of Ginkgo Biloba Leaf Extract according to claim 1, anti-aging PET Resin/Poyester Chips Bottle Grade is characterized in that: described UV light absorber is one or more the combination in the UV light absorber of following kind: benzotriazole category UV light absorber:
326,
234,
350,
320,
328; Low volatility benzotriazole category UV light absorber
360; Red shift benzotriazole category UV light absorber
327; And
UV-P; The special UV light absorber CYASORB of cyanogen UV-3638F, triazine series UV light absorber UV-1577.
3. the preparation method of Ginkgo Biloba Leaf Extract according to claim 1 and 2, anti-aging PET Resin/Poyester Chips Bottle Grade is characterized in that: the add-on of described UV light absorber is 0.15%～1.10% of a PET Resin/Poyester Chips Bottle Grade weight.
4. the preparation method of Ginkgo Biloba Leaf Extract according to claim 1 and 2, anti-aging PET Resin/Poyester Chips Bottle Grade is characterized in that: adding UV light absorber mixing time afterwards is 3～8 minutes.
5. the preparation method of Ginkgo Biloba Leaf Extract according to claim 1, anti-aging PET Resin/Poyester Chips Bottle Grade; It is characterized in that: described hindered amine light stabilizer is for being selected from non-aggretion type high molecular weight hindered amine light stabilizer
119FL; 770 pairs (2 of polymerized hindered amine photostabilizer Chimassorb 944, Tinuvin 788 and photostabilizers; 2; 6,6-tetramethyl-4-piperidyl) one or more in the sebate.
6. the preparation method of Ginkgo Biloba Leaf Extract according to claim 5, anti-aging PET Resin/Poyester Chips Bottle Grade is characterized in that: the add-on of described hindered amine light stabilizer is 15～90ppm.
7. the preparation method of Ginkgo Biloba Leaf Extract according to claim 1, anti-aging PET Resin/Poyester Chips Bottle Grade is characterized in that: described Hinered phenols antioxidant is Irganox 1076, one or more among Irganox 1010 and the Irgafos 168.
8. the preparation method of Ginkgo Biloba Leaf Extract according to claim 7, anti-aging PET Resin/Poyester Chips Bottle Grade is characterized in that: the add-on of described Hinered phenols antioxidant is 30～250ppm.
9. according to the preparation method of the described Ginkgo Biloba Leaf Extract of each claim, anti-aging PET Resin/Poyester Chips Bottle Grade in the claim 1,5 to 8; It is characterized in that: the add-on of described hindered amine light stabilizer is 35～60ppm, and the add-on of described Hinered phenols antioxidant is 75～180ppm.
10. according to the preparation method of the described Ginkgo Biloba Leaf Extract of each claim, anti-aging PET Resin/Poyester Chips Bottle Grade in the claim 1,5 to 8, it is characterized in that: described hindered amine light stabilizer is the composite light stabilizer that the photostabilizer more than two kinds mixes; Described Hinered phenols antioxidant is the composite antioxidant that the oxidation inhibitor more than two kinds mixes.
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