CN109734933B - Organic silicon emulsion for surface smooth treatment of synthetic leather and preparation method thereof - Google Patents
Organic silicon emulsion for surface smooth treatment of synthetic leather and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- 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
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- 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
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/46—Block-or graft-polymers containing polysiloxane sequences containing polyether sequences
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- 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
- D06M15/6433—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing carboxylic groups
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- 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
- D06M15/647—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing polyether sequences
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/10—Block- or graft-copolymers containing polysiloxane sequences
- C08J2383/12—Block- or graft-copolymers containing polysiloxane sequences containing polyether sequences
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Textile Engineering (AREA)
- Engineering & Computer Science (AREA)
- Dispersion Chemistry (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Silicon Polymers (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Treatment And Processing Of Natural Fur Or Leather (AREA)
Abstract
The invention discloses an organic silicon emulsion for surface smoothing treatment of synthetic leather and a preparation method thereof, wherein the organic silicon emulsion comprises the following components in percentage by mass: carboxyl silicone oil crude oil: emulsifier: water is 30-35: 2-8: 50-65 parts; the carboxyl silicone oil crude oil is formed by performing polycondensation on a dimethyl siloxane mixed ring body, an end capping agent, a carboxyl silane coupling agent and a catalyst. The water-based organic silicon emulsion applied to the surface of the synthetic leather has good adhesive force with the surface of the artificial leather, and the hand feeling retention degree is high after the grain is kneaded; and the preparation process is simple, the prepared emulsion has fine particle size, does not float oil in the printing process, and has good stability.
Description
Technical Field
The invention relates to an organic silicon emulsion and a preparation method thereof, in particular to an organic silicon emulsion for surface smoothing treatment of synthetic leather and a preparation method thereof.
Background
Hydroxyl silicone oil, methyl silicone oil and amino silicone oil emulsion are mostly adopted as surface treatment agents for slip treatment at present, but the main defects are that:
(1) the particle size of the hydroxyl methyl silicone oil emulsion is large, and the printing property is poor;
(2) the existing hydroxyl silicone oil, methyl silicone oil and amino silicone oil can cause demulsification due to the extrusion of a blade and a roller in the printing process, so that the final finished leather surface has oil spots;
(3) the adhesion force of the hydroxyl silicone oil and the methyl silicone oil emulsion to leather is poor, and the hand feeling retention degree is weak.
Therefore, the development of the organic silicon emulsion with simple preparation process, good printing property and good adhesive force has important significance for the surface treatment of the synthetic leather artificial leather.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides an organic silicon emulsion for surface smoothing treatment of synthetic leather and a preparation method thereof, so as to improve the printing property, the adhesive force and the stability of a surface treatment agent.
In order to realize the purpose, the invention adopts the technical scheme that the organic silicon emulsion for the surface smooth treatment of the synthetic leather comprises the following components:
comprises the following components in percentage by mass:
carboxyl silicone oil crude oil: emulsifier: water is 30-35: 2-8: 50-65 parts;
the carboxyl silicone oil crude oil comprises the following components in parts by weight:
in an embodiment of the present invention, the structural formula of the carboxyl silane coupling agent is Si-PEG-COOH.
In one embodiment of the present invention, the structure of the carboxyl silane coupling agent is (OMe)3Si(CH2)2NHCONH(CH2)2(EO) mCOOH or (OEt)3Si(CH2)2NHCONH(CH2)2(EO) mCOOH, wherein m is more than or equal to 3.
In an embodiment of the present invention, the capping agent is hexamethyldisiloxane.
In one embodiment of the present invention, the catalyst is an acidic cation exchange resin.
In an embodiment of the present invention, the emulsifier is fatty alcohol-polyoxyethylene ether.
The preparation method of the organic silicon emulsion is characterized by comprising the following steps:
a. mixing and polycondensing the dimethyl siloxane mixed ring body, the end capping agent, the carboxyl silane coupling agent and the acidic cation exchange resin in a container, and carrying out polycondensation reaction to obtain a polycondensation reaction product;
b. c, carrying out reduced pressure distillation on the polycondensation product obtained in the step a, ending the distillation after the quality is constant, and cooling to obtain carboxyl silicone oil crude oil;
c. and c, adding the carboxyl silicone oil obtained in the step b, an emulsifier and water into a container, and stirring and emulsifying to obtain the transparent carboxyl silicone oil emulsion.
In an embodiment of the present invention, the stirring in step c is mechanical stirring performed at normal temperature.
In one embodiment of the present invention, the reaction temperature of the polycondensation is 100-200 ℃.
The technical scheme has the following beneficial effects:
the invention synthesizes a carboxyl silicone oil emulsion, which is prepared by carrying out condensation polymerization reaction on a carboxyl silane coupling agent, a dimethyl siloxane mixed ring body, a sealing agent and a catalyst at a certain temperature to obtain carboxyl silicone oil with a carboxyl side chain, and emulsifying the carboxyl silicone oil by an emulsifier. The invention solves the problem of instability caused by emulsification and compounding of hydroxyl silicone oil and methyl silicone oil through a large amount of emulsifying agents, and the obtained carboxyl silicone oil emulsion has good stability, strong adhesive force, small particle size, good printability and no oil spots generated in the printing process.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
Preparation of carboxyl silicone oil crude oil:
mixing octamethylcyclotetrasiloxane, hexamethyldisiloxane, carboxyl silane coupling agent and acidic cation exchange resin in a container for polycondensation, wherein the mass ratio of octamethylcyclotetrasiloxane to hexamethyldisiloxane to carboxyl silane coupling agent to acidic cation exchange resin is 4000:15:250:1, the reaction temperature of polycondensation is 120 ℃, and the reaction time is 4 hours. And obtaining the required carboxyl silicone oil crude oil after reduced pressure distillation. In this embodiment, the general formula of the carboxyl silane coupling agent is Si-PEG-COOH, specifically (OMe)3Si (CH2)2NHCONH (CH2)2(EO) mCOOH, where m is greater than or equal to 3.
Preparation of a carboxyl silicone oil emulsion:
adding the prepared carboxyl silicone oil crude oil, fatty alcohol-polyoxyethylene ether and water into a container, wherein the mass ratio of the raw oil to the water is 32:4:64, mechanically stirring and emulsifying at normal temperature, the stirring speed is 1000r/min, and the stirring time is 1 hour, so as to obtain a transparent and stable carboxyl silicone oil emulsion, namely emulsion 1.
Application test:
the carboxy silicone oil emulsion was subjected to the following performance tests: (1) testing the centrifugal stability, wherein the testing condition is that the rotating speed is 3000r/min, and the time is 30 min; (2) printing property test under 300 mesh roller printing for 30min, and observing whether there is oily matter at the knife edge
(3) And (3) evaluating and testing hand feeling, wherein the testing condition is that the emulsion is printed on the surface of the synthetic leather by 300 meshes and is dried and kneaded for 30 minutes at the temperature of 80 ℃. And (3) testing results: the emulsion 1 is not delaminated by centrifugation, and the printing knife edge has no oily spot, and the leather surface is rich in hand feeling and strong in oil and moisture feeling.
Example 2
Preparation of carboxyl silicone oil crude oil:
octamethylcyclotetrasiloxane, hexamethyldisiloxane, carboxyl silane coupling agent and acidic cation exchange resin are mixed and polycondensed in a container, the mass ratio is 3500:20:250:1, the reaction temperature of the polycondensation is 120 ℃, and the reaction time is 4 hours. And obtaining the required carboxyl silicone oil crude oil after reduced pressure distillation. In this embodiment, the general formula of the carboxyl silane coupling agent is Si-PEG-COOH, specifically (OMe)3Si (CH2)2NHCONH (CH2)2(EO) mCOOH, where m is greater than or equal to 3.
Preparation of a carboxyl silicone oil emulsion:
adding the prepared carboxyl silicone oil crude oil, fatty alcohol-polyoxyethylene ether and water into a container, wherein the mass ratio of the raw oil to the water is 33:3:64, mechanically stirring and emulsifying at normal temperature, the stirring speed is 1000r/min, and the stirring time is 1 hour, so as to obtain a transparent and stable carboxyl silicone oil emulsion, namely emulsion 2.
Application test:
the carboxy silicone oil emulsion was subjected to the following performance tests: (1) testing the centrifugal stability, wherein the testing condition is that the rotating speed is 3000r/min, and the time is 30 min; (2) printing property test under 300 mesh roller printing for 30min, and observing whether there is oily matter at the knife edge
(3) And (3) evaluating and testing hand feeling, wherein the testing condition is that the emulsion is printed on the surface of the synthetic leather by 300 meshes and is dried and kneaded for 30 minutes at the temperature of 80 ℃. And (3) testing results: emulsion 2 does not delaminate after centrifugation, and no oil stain is generated at a printing edge, but the molecular weight of the synthesized carboxyl silicone oil is lower due to excessive end capping agents, so that the leather surface hand feeling is poorer than that of emulsion 1, and the oil feeling is insufficient.
Example 3
Preparation of carboxyl silicone oil crude oil:
octamethylcyclotetrasiloxane, hexamethylsiloxane, carboxyl silane coupling agent and acidic cation exchange resin are mixed and polycondensed in a container, the mass ratio is 4500:10:150:1, the reaction temperature of the polycondensation is 120 ℃, and the reaction time is 4 hours. And obtaining the required carboxyl silicone oil crude oil after reduced pressure distillation. In this embodiment, the general formula of the carboxyl silane coupling agent is Si-PEG-COOH, specifically (OEt)3Si (CH2)2NHCONH (CH2)2(EO) mCOOH, where m is greater than or equal to 3.
Preparation of a carboxyl silicone oil emulsion:
adding the prepared carboxyl silicone oil crude oil, fatty alcohol-polyoxyethylene ether and water into a container, wherein the mass ratio of the raw oil to the water is 35:7:58, mechanically stirring and emulsifying at normal temperature, the stirring speed is 1000r/min, and the stirring time is 1 hour, so as to obtain a semitransparent stable carboxyl silicone oil emulsion, namely emulsion 3.
Application test:
the carboxy silicone oil emulsion was subjected to the following performance tests: (1) testing the centrifugal stability, wherein the testing condition is that the rotating speed is 3000r/min, and the time is 30 min; (2) printing property test under 300 mesh roller printing for 30min, and observing whether there is oily matter at the knife edge
(3) And (3) evaluating and testing hand feeling, wherein the testing condition is that the emulsion is printed on the surface of the synthetic leather by 300 meshes and is dried and kneaded for 30 minutes at the temperature of 80 ℃. And (3) testing results: the emulsion 3 is slightly layered in a centrifugal mode, the centrifugal stability is poor, and the content of the carboxyl silane coupling agent is low when the emulsion is synthesized with carboxyl silicone oil, so that the silicone oil is not easy to emulsify. Meanwhile, a small amount of oil stains are separated out from the printing knife edge, and the hand feeling is greasy.
Comparative example
Preparation of methyl silicone oil emulsion:
adding commercially available methyl silicone oil with the viscosity of 5000cps, fatty alcohol-polyoxyethylene ether and water into a container at the mass ratio of 35:7:58, mechanically stirring and emulsifying at normal temperature at the stirring speed of 1000r/min for 1 hour to obtain milky methyl silicone oil emulsion, and recording the emulsion 4.
Application test:
methyl silicone oil emulsions were subjected to the following performance tests: (1) testing the centrifugal stability, wherein the testing condition is that the rotating speed is 3000r/min, and the time is 30 min; (2) printing property test under 300 mesh roller printing for 30min, and observing whether there is oily matter at the knife edge
(3) And (3) evaluating and testing hand feeling, wherein the testing condition is that the emulsion is printed on the surface of the synthetic leather by 300 meshes and is dried and kneaded for 30 minutes at the temperature of 80 ℃. And (3) testing results: emulsion 4 has serious centrifugal layering and poor centrifugal stability, a large amount of oil spots are separated out at the edge of a knife after 5 minutes of printing, and emulsion 4 is used for printing on the surface of synthetic leather, so that the synthetic leather has very greasy hand feeling and is uncomfortable.
Compared with the existing preparation method of the carboxyl silicon oil, the carboxyl silicon oil is prepared by innovatively selecting the carboxyl silane coupling agent and adopting a bulk polymerization method, and the preparation method has the advantages of simple production process and less side reaction. The carboxyl silicone oil contains polyether bonds, so that the hydrophilicity is improved, and the emulsified silicone oil emulsion is more stable; the emulsion has fine particle size and does not float oil in the printing process. Meanwhile, the adhesive force with the surface of the artificial leather is good, and the hand feeling retention degree is high after the grain is kneaded. It is also seen from the above examples and comparative examples that the silicone emulsions prepared according to the present invention have greatly improved stability and thus greater applicability in industrial applications.
The above-described embodiments are intended to be illustrative, rather than restrictive, of the present invention, and any alterations and modifications that do not create an inventive feature are intended to be included within the spirit of the invention and the scope of the appended claims.
Claims (8)
1. The organic silicon emulsion for the surface slip treatment of the synthetic leather is characterized by comprising the following components in percentage by mass:
carboxyl silicone oil crude oil: emulsifier: water is 30-35: 2-8: 50-65 parts;
the carboxyl silicone oil crude oil is prepared from the following components in parts by weight:
3500 parts of dimethyl siloxane mixed ring body and 4500 parts of dimethyl siloxane mixed ring body;
10-20 parts of a sealing agent;
150 portions of carboxyl silane coupling agent and 280 portions of carboxyl silane coupling agent;
0.1-2 parts of catalyst.
The general formula of the carboxyl silane coupling agent is Si-PEG-COOH; the concrete structure of the carboxyl silane coupling agent is (OMe)3Si(CH2)2NHCONH(CH2)2(EO) mCOOH or (OEt)3Si(CH2)2NHCONH(CH2)2(EO) mCOOH, wherein m is more than or equal to 3.
2. The silicone emulsion for surface smoothing treatment of synthetic leather according to claim 1, wherein the end-capping agent is hexamethyldisiloxane.
3. The silicone emulsion for surface smoothing treatment of synthetic leather according to claim 1, wherein the catalyst is an acidic cation exchange resin.
4. The silicone emulsion for surface smoothing treatment of synthetic leather according to claim 1, wherein the emulsifier is fatty alcohol-polyoxyethylene ether.
5. The preparation method of the organic silicon emulsion for the surface smoothing treatment of the synthetic leather according to any one of claims 1 to 4 is characterized by comprising the following steps:
a. mixing and polycondensing the dimethyl siloxane mixed ring body, the end capping agent, the carboxyl silane coupling agent and the acidic cation exchange resin in a container, and carrying out polycondensation reaction to obtain a polycondensation reaction product;
b. c, carrying out reduced pressure distillation on the polycondensation product obtained in the step a, ending the distillation after the quality is constant, and cooling to obtain carboxyl silicone oil crude oil;
c. and c, adding the carboxyl silicone oil obtained in the step b, an emulsifier and water into a container, and stirring and emulsifying to obtain the transparent carboxyl silicone oil emulsion.
6. The method for preparing the silicone emulsion for surface smoothing treatment of synthetic leather according to claim 5, wherein the stirring in step c is mechanical stirring performed at normal temperature.
7. The method for preparing the silicone emulsion for surface smoothing treatment of synthetic leather according to claim 5, wherein the reaction temperature of polycondensation is 100-200 ℃.
8. The method for preparing the silicone emulsion for the surface smoothing treatment of synthetic leather according to claim 5, wherein the time of the polycondensation reaction is 3.5-4.5 h.
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| CN201811622975.2A CN109734933B (en) | 2018-12-28 | 2018-12-28 | Organic silicon emulsion for surface smooth treatment of synthetic leather and preparation method thereof |
| CN202111210998.4A CN113788959B (en) | 2018-12-28 | 2018-12-28 | Preparation method of organic silicon emulsion |
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| CN115109363B (en) * | 2022-08-11 | 2023-04-28 | 安徽九牛塑业科技有限公司 | High-toughness plastic master batch for optical cable |
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| CN109734933A (en) | 2019-05-10 |
| CN113788959A (en) | 2021-12-14 |
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