CN109608643A - A kind of organosilicon crude oil, siliceous stiffening agent and preparation method thereof - Google Patents
A kind of organosilicon crude oil, siliceous stiffening agent and preparation method thereof Download PDFInfo
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- CN109608643A CN109608643A CN201811537059.9A CN201811537059A CN109608643A CN 109608643 A CN109608643 A CN 109608643A CN 201811537059 A CN201811537059 A CN 201811537059A CN 109608643 A CN109608643 A CN 109608643A
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- CN
- China
- Prior art keywords
- crude oil
- siliceous
- stiffening agent
- parts
- organosilicon
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- 239000003351 stiffener Substances 0.000 title claims abstract description 43
- 239000010779 crude oil Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011118 polyvinyl acetate Substances 0.000 claims abstract description 20
- 229920002689 polyvinyl acetate Polymers 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 14
- 239000006185 dispersion Substances 0.000 claims abstract description 13
- 239000000839 emulsion Substances 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 4
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 150000004757 linear silanes Chemical class 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 10
- 239000000853 adhesive Substances 0.000 claims description 9
- 230000001070 adhesive effect Effects 0.000 claims description 9
- 239000003054 catalyst Substances 0.000 claims description 9
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 3
- 230000000996 additive effect Effects 0.000 claims description 3
- 150000001298 alcohols Chemical class 0.000 claims description 3
- 125000003368 amide group Chemical group 0.000 claims description 3
- 125000003700 epoxy group Chemical group 0.000 claims description 3
- 229920000768 polyamine Polymers 0.000 claims description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 3
- 229920002554 vinyl polymer Polymers 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical group [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- 230000036541 health Effects 0.000 claims description 2
- 229910000077 silane Inorganic materials 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000010790 dilution Methods 0.000 claims 1
- 239000012895 dilution Substances 0.000 claims 1
- 239000003921 oil Substances 0.000 claims 1
- 239000004744 fabric Substances 0.000 abstract description 13
- 239000007787 solid Substances 0.000 abstract description 8
- 239000002253 acid Substances 0.000 abstract description 7
- 238000005406 washing Methods 0.000 abstract description 6
- 239000003513 alkali Substances 0.000 abstract description 3
- 150000003839 salts Chemical class 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 239000004753 textile Substances 0.000 abstract description 2
- 230000006872 improvement Effects 0.000 description 13
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 12
- -1 Lauxite Polymers 0.000 description 8
- 238000001816 cooling Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000004743 Polypropylene Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- 239000007970 homogeneous dispersion Substances 0.000 description 4
- 229920001155 polypropylene Polymers 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 150000002191 fatty alcohols Chemical class 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229920000877 Melamine resin Polymers 0.000 description 2
- 239000004640 Melamine resin Substances 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 239000012295 chemical reaction liquid Substances 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 238000007790 scraping Methods 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000008340 white lotion Substances 0.000 description 2
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 description 1
- RUMACXVDVNRZJZ-UHFFFAOYSA-N 2-methylpropyl 2-methylprop-2-enoate Chemical compound CC(C)COC(=O)C(C)=C RUMACXVDVNRZJZ-UHFFFAOYSA-N 0.000 description 1
- LMVLVUPTDRWATB-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propan-1-ol Chemical compound CO[Si](C)(OC)CCCO LMVLVUPTDRWATB-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- HMZGPNHSPWNGEP-UHFFFAOYSA-N octadecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C(C)=C HMZGPNHSPWNGEP-UHFFFAOYSA-N 0.000 description 1
- 229920000447 polyanionic polymer Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 235000019394 potassium persulphate Nutrition 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 150000003376 silicon Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000009988 textile finishing Methods 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical compound COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
- C08G77/26—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen nitrogen-containing groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
- C08G77/18—Polysiloxanes containing silicon bound to oxygen-containing groups to alkoxy or aryloxy groups
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/327—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof
- D06M15/333—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof of vinyl acetate; Polyvinylalcohol
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/6436—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing amino groups
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/65—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing epoxy groups
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Cosmetics (AREA)
Abstract
The present invention discloses a kind of siliceous stiffening agent, belongs to textile auxiliary field, by weight, including following raw material: 10-30 parts of intermediate crude oil, 5-10 parts of polyvinyl acetate, 10-20 parts of ethyl acetate, 4-10 parts of emulsifier, 30-70 parts of deionized water；Preparation method is, first by organosilicon crude oil, polyvinyl acetate, ethyl acetate are uniformly mixed, and adds emulsifier, then uses high speed disperser, homogenizer 1~2h of dispersion and emulsion, water, which is then repeatedly added portionwise, makes its phase inversion at emulsion form.Siliceous stiffening agent of the invention has the chemical stabilities such as splendid acid and alkali resistance, salt, can assign fabric stiffening, smooth, thick and solid feel, washing fastness is excellent, by the fabric that siliceous stiffening agent is handled, be washed with water 5 times or more, can still keep enduring with all one's will, smoothly, the feel style of pendency.
Description
Technical field
The present invention relates to a kind of organosilicon crude oil, siliceous stiffening agent and preparation method thereof, belong to textile auxiliary field.
Background technique
Currently, hard finishing can assign the special stiffening bony of fabric and pendency appearance in spinning post-finishing field, it is
A kind of important textile finishing mode.The classification of existing stiffening agent includes: polyvinyl alcohol, polyvinyl acetate, polyacrylic resin,
Lauxite, melamine resin etc..Wherein, Lauxite and melamine resin are right due to will be slow release free formaldehyde
Human health will cause stealthy injury, and when use is increasingly restricted, therefore the fabric stiffening agent of formaldehydeless environmental protection is more by market
It welcomes.Polyvinyl alcohol and polyvinyl acetate and polyacrylic resins stiffening agent meet environmental requirement, and very degree of scraping, rebound
Property is all preferable, is received by the market.
Such as existing Chinese patent " a kind of stiffening agent and preparation method thereof " (application No. is 201711320178.4), preparation side
Method is as follows: (1) by stearyl methacrylate, Isobutyl methacrylate, n propyl methacrylate, maleic acid
Acid anhydride, lauryl acrylate, siloxanes triol alginate esters, lauric monoglyceride, modified soy bean lipoid, vanillic aldehyde, angle Huang matter and
Mixed liquor A is mixed to obtain in deionized water；(2) mixed liquid B is mixed to obtain in potassium peroxydisulfate, silver nitrate and deionized water；(3)
Half mixed liquor A and half mixed liquid B are mixed into heat preservation；(4) residual mixed liquor A and residual mixed liquor B is added dropwise, reacts to obtain reaction
Liquid C；(5) reaction liquid C is cooled to, sodium hydroxide solution stirring is added；(6) be added polyvinylpyrrolidone, polyethylene oxide,
Polyanion cellulose and polyvinyl alcohol stirring；(7) it is cooled to room temperature and discharges to obtain the final product.
But fabric, after the arrangement of traditional stiffening agent, although very degree of scraping significantly improves, feel is easy to become coarse, no cunning
Sense, no solid sense, and it is not washable.
Summary of the invention
In view of the above existing problems in the prior art, the present invention provides a kind of stiffening agents of crude oil containing organosilicon, can assign
Stiffening, thick and solid, the smooth feel of fabric, especially can be washable 5 times or more, keep stiffening, smooth feel style.
The present invention goes back while providing the preparation method of above-mentioned siliceous stiffening agent.
To achieve the goals above, a kind of organosilicon crude oil that the present invention uses, the organosilicon crude oil have following
Structural formula:
R therein is any one of amido, polyamines base, vinyl, epoxy group.
A kind of preparation method of the organosilicon crude oil, first by linear silane and silane coupling agent at 100-115 DEG C, instead
1-3h is answered, basic catalyst is added, vacuum is opened, is warming up to 130-140 DEG C, continues to vacuumize reaction 10-20h, obtain 100
Viscosity is greater than the organosilicon crude oil of 1,000,000 mPa.s at DEG C.
As an improvement, the linear silane using DOW CORNING linear body PMX 0156 or watt gram linear body WS
62M。
As an improvement, the dosage of the silane coupling agent is the 0.05~0.15% of linear silane weight.
As an improvement, the dosage of the basic catalyst is the 0.05~0.5% of linear silane weight；
The basic catalyst is the mixing of any one or more of potassium hydroxide, sodium hydroxide, lithium hydroxide.
A kind of siliceous stiffening agent, by weight, including following raw material: 10-30 parts of organosilicon crude oil, polyvinyl acetate
5-10 parts, 10-20 parts of ethyl acetate, 4-10 parts of emulsifier, 30-70 parts of deionized water.
As an improvement, the adjusting adhesive is higher boiling alcohols in use, the organosilicon crude oil adds adjusting adhesive to dilute,
The additive amount of adjusting adhesive is the 1~5% of organosilicon crude oil weight.
As an improvement, the molecular weight of the polyvinyl acetate is greater than 500,000.
As an improvement, the emulsifier uses emulsifier of the HLB value between 11~13.
A kind of preparation method of siliceous stiffening agent, first by organosilicon crude oil, polyvinyl acetate, ethyl acetate mixing are equal
It is even, emulsifier is added, then uses high speed disperser, homogenizer 1~2h of dispersion and emulsion, water, which is then repeatedly added portionwise, makes its turn
Coordinate emulsion form.
The principle of the present invention are as follows: organic silicon product has helical structure due to silicone molecule chain high crimp, point
In subchain methyl stretch to outside, silicon oxygen bond can with flexible rotating so that organosilicon product all have it is superior it is smooth sense and it is fluffy
Solid sense.In conjunction with the microcosmic mechanism of hard finishing, as long as will actually be fixed at the fiber and fiber interweaving in fabric, in fibre
Vitrifying crystallization is formed at dimension intertexture, so that it may make stiffening effect.Silicon class product is made accordingly stiffening effect to come, takes into account and knits
There is object corresponding sliding sense, solid sense and washing fastness, this kind of siliceous stiffening agent will have extraordinary after silicone finish
Development prospect.
Compared with prior art, siliceous stiffening agent of the invention, including organosilicon crude oil, and organosilicon crude oil passes through linearly
Silane is reacted with silane coupling agent to be made, therefore has the chemical stabilities such as splendid acid and alkali resistance, salt, can assign fabric it is stiffening,
Smoothly, thick and solid feel, washing fastness is excellent, by the fabric that siliceous stiffening agent is handled, is washed with water 5 times or more, still can be with
Keep stiffening, smooth, pendency feel style.
Specific embodiment
In order to make the objectives, technical solutions and advantages of the present invention clearer, the present invention is carried out below further detailed
It describes in detail bright.However, it should be understood that the specific embodiments described herein are merely illustrative of the present invention, it is not limited to this hair
Bright range.
Unless otherwise defined, all technical terms and scientific terms used herein are led with technology of the invention is belonged to
The normally understood meaning of the technical staff in domain is identical, and term as used herein in the specification of the present invention is intended merely to retouch
State the purpose of specific embodiment, it is not intended that in the limitation present invention.
A kind of organosilicon crude oil, the organosilicon crude oil have following structural formula:
R therein is any one of amido, polyamines base, vinyl, epoxy group.
A kind of preparation method of the organosilicon crude oil, first by linear silane and silane coupling agent at 100-115 DEG C, instead
1-3h is answered, basic catalyst is added, vacuum is opened, is warming up to 130-140 DEG C, continues to vacuumize reaction 10-20h, obtain 100
Viscosity is greater than the organosilicon crude oil of 1,000,000 mPa.s at DEG C, and room temperature is translucent solid-state.
As an improvement, the linear silane using DOW CORNING linear body PMX 0156 or watt gram linear body WS
62M。
As an improvement, the dosage of the silane coupling agent is the 0.05~0.15% of linear silane weight.
As an improvement, the dosage of the basic catalyst is the 0.05~0.5% of linear silane weight；
The basic catalyst is the mixing of any one or more of potassium hydroxide, sodium hydroxide, lithium hydroxide.
A kind of siliceous stiffening agent, by weight, including following raw material: 10-30 parts of organosilicon crude oil, polyvinyl acetate
5-10 parts, 10-20 parts of ethyl acetate, 4-10 parts of emulsifier, 30-70 parts of deionized water.
As an improvement, the adjusting adhesive is higher boiling alcohols in use, the organosilicon crude oil adds adjusting adhesive to dilute,
It is preferred that butyl, the additive amount of adjusting adhesive is the 1~5% of organosilicon crude oil weight.
As an improvement, the molecular weight of the polyvinyl acetate is greater than 500,000.
As an improvement, the emulsifier uses emulsifier of the HLB value between 11~13, it is preferred to use fatty alcohol polyoxy second
Alkene ether (9EO), C13 isomeric alcohol polyethenoxy ether (8EO).
A kind of preparation method of siliceous stiffening agent, first by organosilicon crude oil, polyvinyl acetate, ethyl acetate mixing are equal
It is even, emulsifier is added, then uses high speed disperser, homogenizer 1~2h of dispersion and emulsion, water, which is then repeatedly added portionwise, makes its turn
Coordinate emulsion form.
In the preparation method of the siliceous stiffening agent, high speed dispersion revolving speed need to reach 2000-3000 revs/min.In addition,
Since high speed dispersion can generate heat, need cooling with cooling system.
Embodiment 1
A kind of preparation method of siliceous stiffening agent, comprising the following steps:
1) in the 1L four-hole boiling flask equipped with thermometer, condenser pipe and electric mixer, 500g linear body PMX is added
0156 with 0.4g3- (2- aminoethyl)-aminopropyltriethoxy dimethoxysilane, 2h is reacted at 110 DEG C, later be added concentration be
50% potassium hydroxide solution 1.0g, opens vacuum and heats up, until 135 DEG C of reaction 12h, viscosimetric are glued online between 100-120 DEG C
Degree meter 1,000,000 mPa.s or more of display, viscosity is qualified (cooling room temperature is translucent solid-state), and 15g propylene glycol fourth is added into flask
Ether continues to stir 1h, obtains intermediate crude oil I；
2) equipped with condenser system, dispersion machine, homogenizer 2L beaker in, be added polyvinyl acetate (PVAC) 100g,
Ethyl acetate 150g, I 250g of intermediate crude oil, start dispersion machine, prior to 1500 revs/min stirring 0.5h, then add into beaker
Enter fatty alcohol polyoxyethylene ether (3EO) 20g, fatty alcohol polyoxyethylene ether (9EO) 30g, start homogenizer, and by dispersing speed
2000 revs/min are adjusted to, the cooling material of cooling water is opened, then such dispersion and emulsion 2h deionized water 50g is added into beaker,
Continue homogeneous dispersion 30 minutes, then deionized water 100g be added to beaker, continue homogeneous dispersion 30 minutes, so operation 3-4 times,
It is all added to water, material has become thick white lotion in beaker, and glacial acetic acid is added and adjusts pH value 6.5-7, obtains siliceous stiffening agent
YT-1。
Embodiment 2
A kind of preparation method of siliceous stiffening agent, comprising the following steps:
1) in the 1L four-hole boiling flask equipped with thermometer, condenser pipe and electric mixer, 500g linear body WS is added
62M and 0.3g y- glycidol ether hydroxypropyl methyl dimethoxysilane, 1h is reacted at 110 DEG C, lithium hydroxide is added later
1.0g opens vacuum and heats up, until 140 DEG C of reaction 16h, viscosimetric, in-line viscometer shows 1,000,000 between 100~120 DEG C
MPa.s or more, viscosity is qualified (cooling room temperature is translucent solid-state), and 10g butyl is added into flask, continues to stir
1h obtains intermediate crude oil II；
2) equipped with condenser system, dispersion machine, homogenizer 2L beaker in, be added polyvinyl acetate (PVAc) 80g, second
Acetoacetic ester 100g, II 300g of intermediate crude oil start dispersion machine, are first added in 1500 revs/min of stirring 0.5h, then into beaker
C13 isomeric alcohol polyethenoxy ether (6EO) 22g, C13 isomeric alcohol polyethenoxy ether (8EO) 28g, starts homogenizer, and by dispersion machine
Revolving speed is adjusted to 2000 revs/min, opens the cooling material of cooling water, then deionization is added in such dispersion and emulsion 1.5h into beaker
Water 50g continues homogeneous dispersion 30 minutes, then deionized water 100g is added to beaker, continues homogeneous dispersion 30 minutes, so operates
3~4 times, until water all adds, material has become thick white lotion in beaker, controls pH value 6.5-7, obtains siliceous stiffening agent YT-
2。
Embodiment 3
Comparison study test.
1) test material: siliceous stiffening agent YT-1 is made in embodiment 1；Siliceous stiffening agent YT-2 is made in embodiment 2；Poly-vinegar acid
Ethylene stiffening agent TF-6350 (comparison)；Commercial polypropylene acid esters stiffening agent (comparison)；Nylon cotton interwoven directly plays cloth.
2) test technology: an immersing and rolling bakes 2min sizing in 160 DEG C, compares stiffness and feel.
Cloth specimen after hard finishing is cut into 4cm*10cm batten respectively and carries out stiffness survey by L&W BENDING TESTER
Examination, specific test result is as follows shown in table 1-3.
1 stiffness comparing result of table
| Stiffness | |
| YT-1 | 2.0 |
| YT-2 | 2.2 |
| Polyvinyl acetate stiffening agent TF-6350 | 2.1 |
| Commercial polypropylene acid esters stiffening agent | 1.7 |
5 stiffness comparing results after table 2 is washed
| Stiffness | |
| YT-1 | 1.8 |
| YT-2 | 1.9 |
| Polyvinyl acetate stiffening agent TF-6350 | 1.0 |
| Commercial polypropylene acid esters stiffening agent | 0.5 |
3 feel comparing result of table
| Before washing | 5 times after washing | |
| YT-1 | ★★★★ | ★★★ |
| YT-2 | ★★★ | ★★★ |
| Polyvinyl acetate stiffening agent TF-6350 | ★ | ★ |
| Commercial polypropylene acid esters stiffening agent | ★ | ★ |
Note: the thick and solid sliding sense of ★ ★ ★ ★ five star representations of ★ is best.
Table in analysis is it is found that siliceous stiffening agent of the invention can be assigned with chemical stabilities such as splendid acid and alkali resistance, salt
Give stiffening, smooth, the thick and solid feel of fabric, washing fastness is excellent, by siliceous stiffening agent handle fabric, be washed with water 5 times with
On, can still keep enduring with all one's will, smoothly, the feel style of pendency, performance is much better than existing stiffening agent.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modification, equivalent replacement or improvement etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of organosilicon crude oil, which is characterized in that the organosilicon crude oil has following structural formula:
R therein is any one of amido, polyamines base, vinyl, epoxy group.
2. the preparation method of organosilicon crude oil described in a kind of claim 1, which is characterized in that first by linear silane with it is silane coupled
Agent reacts 1-3h at 100-115 DEG C, and basic catalyst is added, and opens vacuum, is warming up to 130-140 DEG C, continues to vacuumize anti-
10-20h is answered, the organosilicon crude oil that the viscosity at 100 DEG C is greater than 1,000,000 mPa.s is obtained.
3. the preparation method of organosilicon crude oil according to claim 2, which is characterized in that the linear silane uses road health
Peaceful linear body PMX 0156 or watt gram linear body WS 62M.
4. the preparation method of organosilicon crude oil according to claim 2, which is characterized in that the dosage of the silane coupling agent
It is the 0.05~0.15% of linear silane weight.
5. the preparation method of organosilicon crude oil according to claim 2, which is characterized in that the dosage of the basic catalyst
It is the 0.05~0.5% of linear silane weight；
The basic catalyst is the mixing of any one or more of potassium hydroxide, sodium hydroxide, lithium hydroxide.
6. a kind of siliceous stiffening agent, which is characterized in that by weight, including following raw material: described in claim any one of 1-5
10-30 parts of organosilicon crude oil, 5-10 parts of polyvinyl acetate, 10-20 parts of ethyl acetate, 4-10 parts of emulsifier, deionized water
30-70 parts.
7. a kind of siliceous stiffening agent according to claim 6, which is characterized in that in use, the organosilicon crude oil adds
Adjusting adhesive dilution, the adjusting adhesive are higher boiling alcohols, and the additive amount of adjusting adhesive is the 1~5% of organosilicon crude oil weight.
8. a kind of siliceous stiffening agent according to claim 6, which is characterized in that the molecular weight of the polyvinyl acetate is big
In 500,000.
9. a kind of siliceous stiffening agent according to claim 6, which is characterized in that the emulsifier using HLB value 11~
Emulsifier between 13.
10. a kind of preparation method of any one of claim 6-9 siliceous stiffening agent, which is characterized in that first by organosilicon original
Oil, polyvinyl acetate, ethyl acetate are uniformly mixed, and are added emulsifier, are then used high speed disperser, homogenizer dispersion and emulsion
1~2h, water, which is then repeatedly added portionwise, makes its phase inversion at emulsion form.
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