CN107629462A - A kind of preparation method of environmental-protection flame-retardant synergist - Google Patents

A kind of preparation method of environmental-protection flame-retardant synergist Download PDF

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Publication number
CN107629462A
CN107629462A CN201711018191.4A CN201711018191A CN107629462A CN 107629462 A CN107629462 A CN 107629462A CN 201711018191 A CN201711018191 A CN 201711018191A CN 107629462 A CN107629462 A CN 107629462A
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environmental
protection flame
retardant synergist
preparation
parts
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CN201711018191.4A
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李晓东
余立峰
赵亚琼
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Zhejiang Weisikang Plastic Co Ltd
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Zhejiang Weisikang Plastic Co Ltd
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Abstract

The present invention relates to field of fire-proof technology, more particularly to a kind of preparation method of environmental-protection flame-retardant synergist, comprise the following steps:(1)Prepare organo montmorillonite;(2)Prepare phosphoprotein;(3)By Organosilicon Polymers, zinc stannate, organo montmorillonite, molybdenum base hydrotalcite and phosphoprotein carry out combination drying, after grinding is refined to 50 ~ 300 μm, with 1 ~ 10mol/L hydrochloric acid conditioning solution PH to 3 ~ 6, stirring, filters, dry, obtain environmental-protection flame-retardant synergist.Raw material sources of the present invention are wide, and biomass resource utilization rate is high, reduces the use of chemical reagent, more green;Technique is simple, and condition is easily controllable, is produced on a large scale;The flame-retardant smoke inhibition effect of obtained environmental-protection flame-retardant synergist is good, and security performance is high.

Description

A kind of preparation method of environmental-protection flame-retardant synergist
Technical field
The present invention relates to field of fire-proof technology, more particularly to a kind of technique is simple, environmental-protection flame-retardant with suppression hood The preparation method of synergist.
Background technology
Fire proofing is a kind of protection materials, and it is can to prevent to burn and be not easy to the material of burning itself, is one Kind can make combustible material burning slow down, terminate or be difficult to the material to burn.At present, bromide fire retardant is the most wide resistance of application Fire one of agent, be to have little to no effect the mechanical property of composite the advantages of bromide fire retardant.According to fire retardant mechanism, bromine Flame retardant can significantly reduce the content of HBr in combustion gas, and the based flame retardant and matrix resin compatibility are good, even in harshness Under conditions of also without precipitation phenomenon.Its decomposition temperature is poly- with various height in the range of 200 DEG C ~ 300 DEG C
The decomposition temperature of thing matches, therefore can play good fire retardation, there is that addition is small, effect is good, and bromine hinders The performance and price for firing agent have very big advantage.Although bromine series flame retardant material shows superior anti-flammability, it is to ring The harm of border and people are very important.Advocating " green " life, harmonious society at this stage, it is fire-retardant for bromine system both at home and abroad The arguement of agent never stopped, and its focal issue is exactly PBDEs(PBDPO)Poisonous, cause whether can be produced in burning The PBDF of cancer(PBDF)With more bromo Ben Bing Evil Young(PBDD).Therefore, the research and development of environment friendly flame retardant have Important Research Significance.
The content of the invention
A kind of the problem of present invention is in order to overcome traditional bromide fire retardant to environment and people with endangering, there is provided technique letter The preparation method of environmental-protection flame-retardant synergist single, that there is suppression hood.
To achieve these goals, the present invention uses following technical scheme:
A kind of preparation method of environmental-protection flame-retardant synergist, comprises the following steps:
(1)Calculate by weight, take 1.5 ~ 3 parts of modifying agent to be scattered in the mixed solution of second alcohol and water, hydrolyze 5 ~ 8h, Ran Houjia Enter 10 ~ 30 parts of montmorillonites, heated backflow, filtering, washing, organo montmorillonite is obtained after drying;
(2)Take 5 ~ 10 parts of biological materials to be added in high-speed organization mixer to be crushed, add the analysis of saturated ammonium sulfate solution Go out precipitation, be dried after being washed with acetone, isolate and purify to obtain phosphoprotein;
(3)According to weight, by Organosilicon Polymers, zinc stannate, step(1)Obtained organo montmorillonite, molybdenum base neatly Stone and step(2)Obtained phosphoprotein carries out combination drying, after grinding is refined to 50 ~ 300 μm, is adjusted with 1 ~ 10mol/L hydrochloric acid Solution PH is saved to 3 ~ 6, stirring, filters, environmental-protection flame-retardant synergist is obtained after drying.
Preferably, step(1)In, the modifying agent is selected from cationic surfactant, and anion surfactant is non- Ionic surface active agent, the one or more in polymer monomer and coupling agent.
Preferably, step(1)In, the mass ratio of second alcohol and water is in the mixed solution of the second alcohol and water(2~9):1.
Preferably, step(2)In, the biological material is selected from milk, soybean, in the plant roots of saponin(e and gummy One or more.
Preferably, step(3)In, the weight is:20 ~ 30 parts of Organosilicon Polymers, 5 ~ 15 parts of zinc stannate, 2 ~ 10 parts of 15 ~ 25 parts of organo montmorillonite, 10 ~ 20 parts of molybdenum base hydrotalcite and phosphoprotein.
Preferably, step(3)In, the molybdenum base hydrotalcite is by hydrotalcite and ammonium octamolybdate, molybdenum trioxide and eight molybdic acids One or more in melamine are modified obtained.
Preferably, step(3)In, the Organosilicon Polymers are selected from silicones, amido silicon oil and polysiloxanes polymerization One or more in thing.
Therefore, the present invention has the advantages that:Raw material sources are wide, and biomass resource utilization rate is high, reduce chemistry examination The use of agent, it is more green;Technique is simple, and condition is easily controllable, is produced on a large scale;Obtained environmental-protection flame-retardant synergistic The flame-retardant smoke inhibition effect of agent is good, and security performance is high.
Embodiment
Below by specific embodiment, technical scheme is described in further detail.
In the present invention, if not refering in particular to, all devices and raw material are commercially available or the industry is conventional, following Method in embodiment, it is this area conventional method unless otherwise instructed.
Embodiment 1
(1)Cationic surfactant 1.3g is taken to be scattered in mass ratio for 2:In the mixed solution of 1 second alcohol and water, 5h is hydrolyzed, Then 10g montmorillonites are added, heated backflow, filtering, washing, organo montmorillonite are obtained after drying;
(2)Take the plant roots of 5g gummies)It is added in high-speed organization mixer and is crushed, adds the analysis of saturated ammonium sulfate solution Go out precipitation, be dried after being washed with acetone, isolate and purify to obtain phosphoprotein;
(3)According to following proportioning, by silicones 20g, zinc stannate 5g, organo montmorillonite 15g, molybdenum base hydrotalcite(Ammonium octamolybdate changes Property)10g and phosphoprotein 2g carries out combination drying, after grinding is refined to 50 μm, with 1mol/L hydrochloric acid conditioning solution PH to 6, stirs Mix, filter, environmental-protection flame-retardant synergist is obtained after drying.
Embodiment 2
(1)Anion surfactant 1g, coupling agent 2g is taken to be scattered in mass ratio for 9:In the mixed solution of 1 second alcohol and water, 8h is hydrolyzed, 30g montmorillonites is then added, heated backflow, filtering, washing, organo montmorillonite is obtained after drying;
(2)Take milk 2g, soybean 3g and saponin(e 5g to be added in high-speed organization mixer to be crushed, it is molten to add saturated ammonium sulfate Liquation goes out precipitation, is dried after being washed with acetone, isolates and purifies to obtain phosphoprotein;
(3)According to following proportioning, by amido silicon oil 15g, polysiloxane polymer 15g, zinc stannate 15g, organo montmorillonite 25g, Molybdenum base hydrotalcite(Molybdenum trioxide and eight molybdic acids are cyanurotriamide modified)20g and phosphoprotein 10g.Carry out combination drying, grinding refinement To after 300 μm, with 10mol/L hydrochloric acid conditioning solution PH to 3, stirring, filter, environmental-protection flame-retardant synergist is obtained after drying.
Embodiment 3
(1)Negated ionic surface active agent 1g and polymer monomer 1g are scattered in mass ratio for 5:The mixing of 1 second alcohol and water is molten In liquid, 7h is hydrolyzed, 20g montmorillonites is then added, heated backflow, filtering, washing, organo montmorillonite is obtained after drying;
(2)Take saponin(e 8g to be added in high-speed organization mixer to be crushed, add saturated ammonium sulfate solution and separate out precipitation, with third Ketone is dried after washing, and isolates and purifies to obtain phosphoprotein;
(3)According to proportioning, by polysiloxane polymer 25g, zinc stannate 10g, organo montmorillonite 20g, molybdenum base hydrotalcite(Hydrotalcite With ammonium octamolybdate, molybdenum trioxide and eight molybdic acids are cyanurotriamide modified)15g and phosphoprotein 6g.Combination drying is carried out, grinding is refined to After 200 μm, with 5mol/L hydrochloric acid conditioning solution PH to 5, stirring, filter, environmental-protection flame-retardant synergist is obtained after drying.
The performance indications of environmental-protection flame-retardant synergist made from embodiment 1-3 are detected, as a result as shown in table 1:
The testing result of table 1.
Performance indications Embodiment 1 Embodiment 2 Embodiment 3
Fire-retardant index V-0 V-0 V-0
Smoke density grade(SDR) ≤75 ≤75 ≤75
As can be seen from Table 1, the environmental-protection flame-retardant synergist obtained using preparation technology of the present invention has good fire-retardant and suppression Smoke performance.
Raw material sources of the present invention are wide, and biomass resource utilization rate is high, reduces the use of chemical reagent, more green; Technique is simple, and condition is easily controllable, is produced on a large scale;The flame-retardant smoke inhibition effect of obtained environmental-protection flame-retardant synergist is good, peace Full performance is high.
Presently preferred embodiments of the present invention is the foregoing is only, any formal limitation not is made to the present invention, not surpassed There are other variants and remodeling on the premise of going out the technical scheme described in claim.

Claims (7)

1. a kind of preparation method of environmental-protection flame-retardant synergist, it is characterised in that comprise the following steps:
(1)Calculate by weight, take 1.5 ~ 3 parts of modifying agent to be scattered in the mixed solution of second alcohol and water, hydrolyze 5 ~ 8h, Ran Houjia Enter 10 ~ 30 parts of montmorillonites, heated backflow, filtering, washing, organo montmorillonite is obtained after drying;
(2)Take 5 ~ 10 parts of biological materials to be added in high-speed organization mixer to be crushed, add the analysis of saturated ammonium sulfate solution Go out precipitation, be dried after being washed with acetone, isolate and purify to obtain phosphoprotein;
(3)According to weight, by Organosilicon Polymers, zinc stannate, step(1)Obtained organo montmorillonite, molybdenum base neatly Stone and step(2)Obtained phosphoprotein carries out combination drying, after grinding is refined to 50 ~ 300 μm, is adjusted with 1 ~ 10mol/L hydrochloric acid Solution PH is saved to 3 ~ 6, stirring, filters, environmental-protection flame-retardant synergist is obtained after drying.
A kind of 2. preparation method of environmental-protection flame-retardant synergist according to claim 1, it is characterised in that step(1)In, The modifying agent is selected from cationic surfactant, anion surfactant, nonionic surfactant, polymer monomer and One or more in coupling agent.
A kind of 3. preparation method of environmental-protection flame-retardant synergist according to claim 1, it is characterised in that step(1)In, The mass ratio of second alcohol and water is in the mixed solution of the second alcohol and water(2~9):1.
A kind of 4. preparation method of environmental-protection flame-retardant synergist according to claim 1, it is characterised in that step(2)In, The biological material is selected from milk, soybean, the one or more in the plant roots of saponin(e and gummy.
A kind of 5. preparation method of environmental-protection flame-retardant synergist according to claim 1, it is characterised in that step(3)In, The weight is:20 ~ 30 parts of Organosilicon Polymers, 5 ~ 15 parts of zinc stannate, 15 ~ 25 parts of organo montmorillonite, molybdenum base neatly 2 ~ 10 parts of 10 ~ 20 parts of stone and phosphoprotein.
A kind of 6. preparation method of environmental-protection flame-retardant synergist according to claim 1 or 5, it is characterised in that step(3) In, by hydrotalcite and ammonium octamolybdate, the one or more in molybdenum trioxide and eight molybdic acid melamines change the molybdenum base hydrotalcite Property is made.
A kind of 7. preparation method of environmental-protection flame-retardant synergist according to claim 1 or 5, it is characterised in that step(3) In, the Organosilicon Polymers are selected from silicones, the one or more in amido silicon oil and polysiloxane polymer.
CN201711018191.4A 2017-10-25 2017-10-25 A kind of preparation method of environmental-protection flame-retardant synergist Pending CN107629462A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101649088A (en) * 2009-09-17 2010-02-17 公安部四川消防研究所 Halogen-free intumescent flame-retardant polypropylene/ethylene vinyl acetate cable material
TW201040223A (en) * 2009-05-12 2010-11-16 Nanya Plastics Corp PVC(polyvinyl chloride) resin composition and product thereof
CN102504751A (en) * 2011-11-22 2012-06-20 东莞市普赛达密封粘胶有限公司 Flame-retardant polyurethane sealant and preparation method thereof
CN104086920A (en) * 2014-07-18 2014-10-08 东北林业大学 Flame-retardant smoke-suppression type PVC-based wood-plastic composite material and preparation method thereof
CN105237865A (en) * 2015-10-21 2016-01-13 上海至正道化高分子材料股份有限公司 Ultraviolet light cross-linking color low-smoke halogen-free flame-retardant cable material, cable product and preparation method of cable material
JP5989063B2 (en) * 2014-11-10 2016-09-07 株式会社朝日ラバー Silicone resin base material

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TW201040223A (en) * 2009-05-12 2010-11-16 Nanya Plastics Corp PVC(polyvinyl chloride) resin composition and product thereof
CN101649088A (en) * 2009-09-17 2010-02-17 公安部四川消防研究所 Halogen-free intumescent flame-retardant polypropylene/ethylene vinyl acetate cable material
CN102504751A (en) * 2011-11-22 2012-06-20 东莞市普赛达密封粘胶有限公司 Flame-retardant polyurethane sealant and preparation method thereof
CN104086920A (en) * 2014-07-18 2014-10-08 东北林业大学 Flame-retardant smoke-suppression type PVC-based wood-plastic composite material and preparation method thereof
JP5989063B2 (en) * 2014-11-10 2016-09-07 株式会社朝日ラバー Silicone resin base material
CN105237865A (en) * 2015-10-21 2016-01-13 上海至正道化高分子材料股份有限公司 Ultraviolet light cross-linking color low-smoke halogen-free flame-retardant cable material, cable product and preparation method of cable material

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Application publication date: 20180126