CN112920349B - Silicon-containing polymer additive and preparation method thereof - Google Patents
Silicon-containing polymer additive and preparation method thereof Download PDFInfo
- Publication number
- CN112920349B CN112920349B CN202110114609.1A CN202110114609A CN112920349B CN 112920349 B CN112920349 B CN 112920349B CN 202110114609 A CN202110114609 A CN 202110114609A CN 112920349 B CN112920349 B CN 112920349B
- Authority
- CN
- China
- Prior art keywords
- silicon
- leather
- containing polymer
- stirring
- auxiliary agent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 229920005573 silicon-containing polymer Polymers 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000654 additive Substances 0.000 title claims abstract description 14
- 230000000996 additive effect Effects 0.000 title claims abstract description 14
- 239000010985 leather Substances 0.000 claims abstract description 50
- 239000000178 monomer Substances 0.000 claims abstract description 20
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 18
- CERQOIWHTDAKMF-UHFFFAOYSA-N alpha-methacrylic acid Natural products CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 15
- 229920002545 silicone oil Polymers 0.000 claims abstract description 13
- -1 acrylic polyol ester Chemical class 0.000 claims abstract description 10
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims abstract description 8
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 6
- 238000007334 copolymerization reaction Methods 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 25
- 238000006243 chemical reaction Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000012153 distilled water Substances 0.000 claims description 15
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 239000000376 reactant Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 7
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 7
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 7
- 229920000191 poly(N-vinyl pyrrolidone) Polymers 0.000 claims description 7
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 3
- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims 1
- VEPKQEUBKLEPRA-UHFFFAOYSA-N VX-745 Chemical compound FC1=CC(F)=CC=C1SC1=NN2C=NC(=O)C(C=3C(=CC=CC=3Cl)Cl)=C2C=C1 VEPKQEUBKLEPRA-UHFFFAOYSA-N 0.000 claims 1
- FSAJWMJJORKPKS-UHFFFAOYSA-N octadecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C=C FSAJWMJJORKPKS-UHFFFAOYSA-N 0.000 claims 1
- 229920005862 polyol Polymers 0.000 abstract description 8
- 239000000835 fiber Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000001050 lubricating effect Effects 0.000 abstract description 3
- 150000003254 radicals Chemical class 0.000 abstract description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- 238000000034 method Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- 239000010775 animal oil Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 235000015112 vegetable and seed oil Nutrition 0.000 description 3
- 239000008158 vegetable oil Substances 0.000 description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 239000011630 iodine Substances 0.000 description 2
- 229910052740 iodine Inorganic materials 0.000 description 2
- 239000002649 leather substitute Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 1
- RZRNAYUHWVFMIP-KTKRTIGZSA-N 1-oleoylglycerol Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(O)CO RZRNAYUHWVFMIP-KTKRTIGZSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- JTHZUSWLNCPZLX-UHFFFAOYSA-N 6-fluoro-3-methyl-2h-indazole Chemical compound FC1=CC=C2C(C)=NNC2=C1 JTHZUSWLNCPZLX-UHFFFAOYSA-N 0.000 description 1
- DPUOLQHDNGRHBS-UHFFFAOYSA-N Brassidinsaeure Natural products CCCCCCCCC=CCCCCCCCCCCCC(O)=O DPUOLQHDNGRHBS-UHFFFAOYSA-N 0.000 description 1
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- URXZXNYJPAJJOQ-UHFFFAOYSA-N Erucic acid Natural products CCCCCCC=CCCCCCCCCCCCC(O)=O URXZXNYJPAJJOQ-UHFFFAOYSA-N 0.000 description 1
- 206010034018 Parosmia Diseases 0.000 description 1
- PHYFQTYBJUILEZ-UHFFFAOYSA-N Trioleoylglycerol Natural products CCCCCCCCC=CCCCCCCCC(=O)OCC(OC(=O)CCCCCCCC=CCCCCCCCC)COC(=O)CCCCCCCC=CCCCCCCCC PHYFQTYBJUILEZ-UHFFFAOYSA-N 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229920001436 collagen Polymers 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- DPUOLQHDNGRHBS-KTKRTIGZSA-N erucic acid Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCC(O)=O DPUOLQHDNGRHBS-KTKRTIGZSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 125000005456 glyceride group Chemical group 0.000 description 1
- 229940075529 glyceryl stearate Drugs 0.000 description 1
- PZDUWXKXFAIFOR-UHFFFAOYSA-N hexadecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCCCOC(=O)C=C PZDUWXKXFAIFOR-UHFFFAOYSA-N 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
- C08F283/124—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes on to polysiloxanes having carbon-to-carbon double bonds
-
- C—CHEMISTRY; METALLURGY
- C14—SKINS; HIDES; PELTS; LEATHER
- C14C—CHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
- C14C3/00—Tanning; Compositions for tanning
- C14C3/02—Chemical tanning
- C14C3/08—Chemical tanning by organic agents
- C14C3/22—Chemical tanning by organic agents using polymerisation products
Abstract
The invention provides a silicon-containing polymer auxiliary agent and a preparation method thereof, relates to the technical field of leather auxiliary agent production, and particularly discloses a silicon-containing polymer auxiliary agent for endowing leather with good softness and low density performance. The silicon-containing polymer additive is prepared by the free radical copolymerization of vinyl-rich silicone oil and monomers such as (methyl) acrylic acid, itaconic acid, acrylic polyol ester and the like. The polymer auxiliary agent is rich in carboxyl, long carbon chain, silicon oxygen bond group and other groups, has larger molecular weight, has stronger lubricating and softening assisting performance on leather fibers, gives full and soft hand feeling to finished leather, can reduce the density of the finished leather, and is suitable for market popularization and application.
Description
Technical Field
The invention relates to the technical field of leather assistant production, in particular to a silicon-containing polymer assistant and a preparation method thereof, and more particularly relates to a preparation method of a silicon-containing polymer assistant capable of endowing leather with good softness and low density performance.
Background
Leather fur products have been symbolized by identity and status since ancient times. In the leather industry, finished leather tanned based on chrome tanning agents has a good balance of properties and has been dominating in the tanning field since its application. However, the tanned leather needs to be retanned, dyed and fattened at a later stage and can become usable leather fabric after other processes. Among them, the fatliquoring is one of important processes, which can impart a soft hand to leather, silk, and the like.
In the leather greasing process, the greasing material becomes the most critical material in the greasing process. The commonly used greasing materials are natural animal oil, vegetable oil, modified substances of mineral oil and compound greasing agents which play a role in lubricating fibers in the leather, thereby improving the use performance of the leather. However, the main components of natural animal oil and vegetable oil are glyceryl stearate, glyceryl oleate, glyceride of erucic acid and the like, and the natural animal oil and vegetable oil have certain iodine value (the iodine value is related to the unsaturated degree of grease), so that the problems of oxidation, smell change, oil frost and the like easily occur in the tanning process or the leather storage process. Therefore, the superiority of grease quality directly determines the quality of finished leather. In addition, in the leather production, the addition amount of the greasing material is larger (the addition amount is about 20% of the weight of the shaving wet blue leather), so that the density of the finished leather is larger and is far larger than that of the superfine fiber synthetic leather.
Therefore, it is one of the demands of the leather industry to adopt a material which can not only impart the softness to the leather but also reduce the density of the leather, and how to prepare a silicon-containing polymer auxiliary agent which imparts the leather with good softness and low density is a technical problem to be solved by those skilled in the art.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a production method of a polymer auxiliary agent capable of endowing leather with good soft and low-density performance, so that the leather has good stability and is endowed with soft hand feeling and low-density texture.
In order to achieve the purpose, the invention adopts the following technical scheme:
the silicon-containing polymer auxiliary agent endows leather with good softness and low density performance, is prepared by the following raw materials through radical copolymerization, and comprises the following raw materials in parts by weight:
the synthesis mechanism of the silicon-containing polymer additive is as follows:
wherein R is 1 ＝-H，-CH 3 ；R 2 ＝-C 12 H 25 ，-C 16 H 33 ，-C 18 H 37 ；R 3 ＝-CH 3 ，-CH＝CH 2 。
The invention also provides a preparation method of the silicon-containing polymer additive for endowing leather with good softness and low density performance, the silicon-containing polymer additive is prepared by carrying out free radical copolymerization on polyvinyl silicone oil, a (methyl) acrylic acid monomer, itaconic acid, peregal O-25, sodium dodecyl benzene sulfonate, acrylic acid polyol ester and ammonium persulfate, and the preparation method comprises the following specific steps:
(1) Firstly, according to the raw material composition ratio of claim 1, (meth) acrylic acid monomer, itaconic acid and distilled water are put into a reaction kettle and stirred and mixed at room temperature, then the pH of the mixed solution is adjusted to 4.0-4.5 by 30% sodium hydroxide solution, and the mixed monomer solution is filtered for standby;
(2) Adding distilled water, peregal O-25 and sodium dodecyl benzene sulfonate in parts by weight into a reaction kettle, stirring and mixing, heating, then adding polyvinyl silicone oil, stirring and reacting, adding acrylic polyol ester, and stirring and reacting again to obtain a reactant I;
(3) Adding distilled water into the reactant I, stirring and mixing, then heating, dropwise adding the mixed monomer liquid and ammonium persulfate, stirring after dropwise adding, and continuing to react to obtain a reactant II;
(4) And after the reactant II is cooled, adjusting the pH value to 5.0-5.5 by using a 30% sodium hydroxide solution, filtering and discharging to obtain the silicon-containing polymer auxiliary agent endowing leather with good softness and low density performance.
Preferably, the temperature raising reaction temperature in the step (2) is 70 ℃ to 75 ℃, the first stirring reaction time is 30 to 60 minutes, and the second stirring reaction time is 30 to 60 minutes.
Preferably, in the step (3), the dropping temperature when the mixed monomer liquid is added is 80-85 ℃, and the dropping time is 90-120 minutes.
More preferably, the reaction temperature is 85 ℃ to 90 ℃ and the reaction time is 90 to 120 minutes.
Preferably, in the step (4), the temperature of the reactant II is reduced to 50-56 ℃.
Further, the above-mentioned meth) acrylic acid monomer is acrylic acid or methacrylic acid; the polyvinyl silicone oil is high vinyl silicone oil, wherein the vinyl content is 10-22%;
and the acrylic polyol ester is at least one of lauryl acrylate, cetyl acrylate and stearyl acrylate.
It is worth mentioning that the product prepared by the method is light yellow and semitransparent viscous liquid, wherein the content of effective substances is 40-45%, the pH value is 5.0-5.5, the product has anionic charge, and the leather which is acted independently is soft and full, compact in grain surface and low in density.
According to the technical scheme, compared with the prior art, the invention discloses a silicon-containing polymer auxiliary agent and a preparation method thereof, and the silicon-containing polymer auxiliary agent has the following excellent effects:
1. in the synthetic preparation process disclosed by the invention, reaction of high vinyl silicone oil and acrylic polyol ester with other monomers is adopted, a nonpolar chain and a silicon-oxygen bond with good flexibility are introduced, and a lubricating effect is achieved among collagen fibers.
2. The silicon-containing polymer auxiliary agent disclosed by the invention is rich in carboxyl, so that the silicon-containing polymer auxiliary agent can form a firm coordination bond with chrome tanned leather.
3. The leather processed by the silicon-containing polymer additive disclosed by the invention has low density and soft and elegant hand feeling.
4. The silicon-containing polymer additive prepared by the method disclosed by the application meets the requirements of all light leather processing required in the current market, and the physical and mechanical indexes of finished leather reach the chrome tanning standard issued by the ministry of light industry in 2005.
Detailed Description
The technical solutions in the present invention will be described clearly and completely with reference to the embodiments of the present invention, and it should be apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention discloses a preparation method of a silicon-containing polymer auxiliary agent for endowing leather with good softness and low density performance.
The preparation process and the excellent results of the present invention will be further illustrated with reference to specific examples, but the present invention is not limited to the following examples.
Example 1
A preparation method of a silicon-containing polymer auxiliary agent for endowing leather with good softness and low density performance comprises the following steps:
(1) Putting 120 kg of (methyl) acrylic acid monomer, 40 kg of itaconic acid and 100 kg of distilled water into a reaction kettle, stirring and mixing at room temperature, adjusting the pH to 4.0 by adopting 100 kg of 30% sodium hydroxide solution, and filtering for later use;
(2) Adding 140 kg of distilled water, 4 kg of peregal O-25 and 2 kg of sodium dodecyl benzene sulfonate into a reaction kettle, stirring and mixing, heating to 70 ℃, adding 24 kg of polyvinyl silicone oil, and stirring for 30 minutes. Then 90 kg of acrylic polyol ester was added and stirred for 30 minutes.
(3) Adding 100 kg of distilled water into the reaction kettle in the step (2), stirring, mixing, heating to 80 ℃, respectively dropwise adding the mixed monomer liquid in the step (1) and 5.0 kg of ammonium persulfate (dissolved by 15 times of water), wherein the dropwise adding time is 90 minutes, stirring at 85 ℃ after the dropwise adding is finished, and continuously reacting for 90 minutes;
(4) Cooling to 50 ℃, adjusting the pH value to 5.0 by 30-50 parts of 30% sodium hydroxide solution, filtering and discharging.
Example 2
A preparation method of a silicon-containing polymer auxiliary agent for endowing leather with good softness and low density performance comprises the following steps:
(1) Firstly, 160 kg of (methyl) acrylic acid monomer, 60 kg of itaconic acid and 120 kg of distilled water are placed in a reaction kettle and stirred and mixed at room temperature, then 120 kg of 30% sodium hydroxide solution is adopted to adjust the pH value to 4.5, and the mixture is filtered for standby;
(2) 160 kg of distilled water, 6 kg of peregal O-25 and 3 kg of sodium dodecyl benzene sulfonate are added into a reaction kettle, stirred and mixed, heated to 75 ℃, added with 30 kg of polyvinyl silicone oil and stirred for 60 minutes. Then, 110 kg of polyol acrylate was added and stirred for 60 minutes.
(3) Adding 120 kg of distilled water into the reaction kettle in the step (2), stirring, mixing, heating to 85 ℃, respectively dropwise adding the mixed monomer liquid in the step (1) and 8.0 kg of ammonium persulfate (dissolved by 15 times of water), wherein the dropwise adding time is 120 minutes, stirring at 90 ℃ after the dropwise adding is finished, and continuously reacting for 120 minutes;
(4) Cooling to 56 ℃, adjusting the pH value to 5.5 by using 50 kilograms of 30 percent sodium hydroxide solution, filtering and discharging.
Example 3
A preparation method of a silicon-containing polymer auxiliary agent for endowing leather with good softness and low density performance comprises the following steps:
(1) Putting 140 kg of (methyl) acrylic acid monomer, 50 kg of itaconic acid and 110 kg of distilled water into a reaction kettle, stirring and mixing at room temperature, adjusting the pH to 4.2 by adopting 110 kg of 30% sodium hydroxide solution, and filtering for later use;
(2) 150 kg of distilled water, 5 kg of peregal O-25 and 2.5 kg of sodium dodecyl benzene sulfonate are added into a reaction kettle, stirred and mixed, heated to 72.5 ℃, added with 27 kg of polyvinyl silicone oil and stirred for 45 minutes. Then 100 kg of acrylic polyol ester was added and stirred for 45 minutes.
(3) Adding 110 parts of distilled water into the reaction kettle in the step (2), stirring and mixing, heating to 82 ℃, respectively dropwise adding the mixed monomer liquid in the step (1) and 6.5 kilograms of ammonium persulfate (dissolved by 15 times of water), wherein the dropwise adding time is 105 minutes, stirring at 87.5 ℃ after dropwise adding, and continuously reacting for 105 minutes;
(4) Cooling to 53 ℃, adjusting the pH value to 5.2 by 40 parts of 30% sodium hydroxide solution, filtering and discharging.
In order to further disclose the excellent effects of the technical scheme, the inventor also performs an application effect experiment on the embodiment, and the specific experimental operation and result analysis are as follows:
the leather body of the finished leather which is acted by the product alone is soft and full, the grain surface is slightly compact, and the density is lower (the density is 0.49, the density of the common real leather is 0.6-0.8, and the density of the superfine fiber synthetic leather is 0.3-0.4).
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. The silicon-containing polymer auxiliary agent for endowing leather with good softness and low density performance is characterized by being prepared from the following raw materials in parts by weight through radical copolymerization:
120 to 160 portions of (methyl) acrylic acid monomer,
40 to 60 portions of itaconic acid, 40 to 60 portions,
4 to 6 portions of peregal O-25,
2 to 3 parts of sodium dodecyl benzene sulfonate,
24 to 30 portions of polyvinyl silicone oil,
90 to 110 portions of acrylic ester,
5.0-8.0 parts of ammonium persulfate;
the preparation process of the silicon-containing polymer additive comprises the following specific steps:
(1) Firstly, placing (methyl) acrylic acid monomer, itaconic acid and distilled water into a reaction kettle according to the composition ratio of the raw materials, stirring and mixing at room temperature, adjusting the pH of the mixed solution to 4.0-4.5 by using 30% sodium hydroxide solution, and filtering to obtain mixed monomer liquid for later use;
(2) Adding distilled water, peregal O-25 and sodium dodecyl benzene sulfonate in parts by weight into a reaction kettle, stirring and mixing, heating, then adding polyvinyl silicone oil, stirring and reacting, adding acrylic ester, and stirring and reacting again to obtain a reactant I; the acrylate is at least one of dodecyl acrylate, hexadecyl acrylate and octadecyl acrylate;
(3) Adding distilled water into the reactant I, stirring and mixing, then heating, dropwise adding the mixed monomer liquid and ammonium persulfate, stirring after dropwise adding, and continuing to react to obtain a reactant II;
(4) And after the reactant II is cooled, adjusting the pH value to 5.0-5.5 by using a 30% sodium hydroxide solution, filtering and discharging to obtain the silicon-containing polymer auxiliary agent endowing leather with good softness and low density performance.
2. The silicon-containing polymer additive for imparting excellent softness and low-density to leather according to claim 1, wherein the temperature-raising reaction temperature in the step (2) is 70 ℃ to 75 ℃, the first stirring reaction time is 30 to 60 minutes, and the second stirring reaction time is 30 to 60 minutes.
3. The silicon-containing polymer additive for imparting excellent softness and low-density property to leather according to claim 1, wherein the dropping temperature at the time of adding the mixed monomer liquid in the step (3) is 80 to 85 ℃ and the dropping time is 90 to 120 minutes.
4. The silicon-containing polymer additive for imparting good softness and low density to leather according to claim 3, wherein the reaction temperature is 85 to 90 ℃ and the reaction time is 90 to 120 minutes.
5. The silicon-containing polymer additive for imparting good softness and low density to leather as claimed in claim 1, wherein in step (4), the temperature of the reactant II is lowered to 50 ℃ to 56 ℃.
6. The silicon-containing polymer assistant for imparting good soft, low density properties to leather according to any of claims 1 to 5 wherein the (meth) acrylic monomer is acrylic acid or methacrylic acid.
7. The silicon-containing polymer additive for imparting good softness and low density to leather as claimed in any one of claims 1 to 5, wherein said polyvinyl silicone oil is a high vinyl silicone oil having a vinyl content of 10 to 22%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110114609.1A CN112920349B (en) | 2021-01-26 | 2021-01-26 | Silicon-containing polymer additive and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110114609.1A CN112920349B (en) | 2021-01-26 | 2021-01-26 | Silicon-containing polymer additive and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112920349A CN112920349A (en) | 2021-06-08 |
| CN112920349B true CN112920349B (en) | 2022-11-15 |
Family
ID=76167368
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110114609.1A Active CN112920349B (en) | 2021-01-26 | 2021-01-26 | Silicon-containing polymer additive and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112920349B (en) |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2350379A1 (en) * | 1976-05-04 | 1977-12-02 | Reichhold Chemicals Inc | Lacquer paints for impulse ray hardening - consisting of cpd(s). contg. hydroxyl or amino gps., unsaturated acids and photoinitiators |
| CN100480461C (en) * | 2007-02-15 | 2009-04-22 | 浙江工业大学 | Method of preparing fluorine and silicon containing hydrophobic and oil repellent fabric finishing agent |
| CN103254351B (en) * | 2013-05-06 | 2015-06-03 | 陕西科技大学 | Preparation method of carboxyl silicon modified acrylic resin emulsion |
| WO2015059084A1 (en) * | 2013-10-21 | 2015-04-30 | Basf Se | Precipitation polymerization in the presence of a tertiary amine and of an anhydride |
| CN103981710B (en) * | 2014-04-21 | 2016-07-06 | 孙德庆 | A kind of fabric finishing agent and preparation method thereof |
| CN104672403B (en) * | 2015-02-13 | 2018-01-19 | 杭州传化精细化工有限公司 | A kind of environmentally friendly silicone acrylic emulsion and preparation method thereof |
| CN106046912A (en) * | 2016-05-26 | 2016-10-26 | 清远市美乐仕油墨有限公司 | Waterproof slipping auxiliary for leather and method for preparing waterproof slipping auxiliary |
| CN107353762A (en) * | 2017-08-21 | 2017-11-17 | 四川达威科技股份有限公司 | Silicone-modified polyacrylate leather finishing agent, its preparation method and leather composite bed |
| CN108486293B (en) * | 2018-03-13 | 2020-06-19 | 齐河力厚化工有限公司 | Preparation method of polymer leather fatting agent |
| CN109722917A (en) * | 2019-01-31 | 2019-05-07 | 四川大学 | A kind of surface tension and recoatability method for improving of organosilicon synthetic leather coating |
-
2021
- 2021-01-26 CN CN202110114609.1A patent/CN112920349B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN112920349A (en) | 2021-06-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JPH03207800A (en) | Agent for making leather and fur hydrophobic | |
| CN101072803B (en) | Transparent copolymer resin, method for preparing the transparent copolymer resin, and resin blend composition including the transparent copolymer resin | |
| EP1745081A1 (en) | Polysiloxane graft polymer | |
| US5714560A (en) | Water-soluble or water-dispersible graft polymers of proteins as leather tanning agents | |
| CN112920349B (en) | Silicon-containing polymer additive and preparation method thereof | |
| EP0673395A1 (en) | Copolymers and their use in the treatment of leather. | |
| EP0156971A1 (en) | Process for the preparation of aqueous dispersions of acryl copolymers and their use in finishing leather | |
| CN102532786B (en) | Preparation method of bimodally-distributed modified ABS (acrylonitrile-butadiene-styrene) resin | |
| EP1658314B1 (en) | Use of 2-hydroxy-2-sulfinato acetic acid or the salts thereof as an initiator in w/o emulsions | |
| KR960014915B1 (en) | Acrylate tanning agent | |
| CN111057803A (en) | Amphoteric polymer retanning agent for ecological leather manufacturing and preparation method thereof | |
| CN108070683B (en) | Production method of filled and compact polymer tanning agent based on reactive emulsifier | |
| EP0529695A2 (en) | Process for preparing a polymer dispersion | |
| CN113088585B (en) | Modified wool acid fatting agent and preparation method thereof | |
| EP0607388B1 (en) | Use of graft polymers for stuffing and fulling leathers and fur pelts | |
| CN110592295B (en) | Flame-retardant pricklyash seed oil/carboxyl POSS (polyhedral oligomeric silsesquioxane) compound fatting agent and preparation method thereof | |
| US20080201864A1 (en) | Copolymers, Production and Use Thereof | |
| CN113278116A (en) | ASA non-breaking white high-rubber powder, ASA non-breaking white film and preparation method thereof | |
| CN1218050C (en) | Method for preparing lecithoid retanning agent with lipide being added | |
| CN113980201B (en) | Slump-retaining water reducer and preparation method thereof | |
| EP0108396B1 (en) | Stabilized graft copolymers | |
| EP1651781A1 (en) | Method for the production of leather by using polymers | |
| CN113402653B (en) | Self-fragrant multi-dendritic polymer fatting agent and preparation method thereof | |
| KR100604348B1 (en) | Application of lard oil is fleshing process | |
| CN113430306A (en) | Anti-yellowing titanium dioxide/fatty acid-based leather fatliquoring agent and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20231227 Address after: 276000, located in the Lushan project area of Yishui, Linyi City, Shandong Province, north of Changshan Road (South Second Ring Road) Patentee after: SHANDONG LINING TECHNOLOGY NEW MATERIALS CO.,LTD. Address before: 314000 2 building, Photovoltaic Science Park, 1288 Kang He road, Xiuzhou District, Jiaxing, Zhejiang. Patentee before: JIAXING University |
|
| TR01 | Transfer of patent right |