CN114892418A - Organic silicon synthetic leather foamed coating and preparation method thereof - Google Patents
Organic silicon synthetic leather foamed coating and preparation method thereof Download PDFInfo
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- CN114892418A CN114892418A CN202210428866.7A CN202210428866A CN114892418A CN 114892418 A CN114892418 A CN 114892418A CN 202210428866 A CN202210428866 A CN 202210428866A CN 114892418 A CN114892418 A CN 114892418A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
- D06N3/142—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes mixture of polyurethanes with other resins in the same layer
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0043—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by their foraminous structure; Characteristics of the foamed layer or of cellular layers
- D06N3/005—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by their foraminous structure; Characteristics of the foamed layer or of cellular layers obtained by blowing or swelling agent
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/007—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by mechanical or physical treatments
- D06N3/0077—Embossing; Pressing of the surface; Tumbling and crumbling; Cracking; Cooling; Heating, e.g. mirror finish
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0086—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the application technique
- D06N3/0088—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the application technique by directly applying the resin
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/128—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with silicon polymers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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- Engineering & Computer Science (AREA)
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- Dispersion Chemistry (AREA)
- Synthetic Leather, Interior Materials Or Flexible Sheet Materials (AREA)
Abstract
The invention belongs to the technical field of synthetic leather, and particularly relates to an organic silicon synthetic leather foaming coating and a preparation method thereof. The invention disperses aqueous polyurethane into A component hydroxyl silicone oil of organosilicon bi-component room temperature/low temperature vulcanized rubber to form water-in-oil emulsion; and adding the component B curing agent and the catalyst into the water-in-oil emulsion, heating to remove water in the dispersed phase and leaving foam holes after the continuous phase is completely cured, thus obtaining the organosilicon-polyurethane interpenetrating network foaming coating. According to the invention, the organic silicon-polyurethane interpenetrating network foaming coating is constructed in situ by virtue of the water-in-oil system precursor, on one hand, the vulcanization and foaming can be carried out step by step, and the problem that the foaming and vulcanization rates are difficult to coordinate in the traditional process is solved; on the other hand, the introduction of the waterborne polyurethane not only causes pores, but also improves the polarity and the mechanical property of the organic silicon foaming coating, thereby improving the adhesive force between the organic silicon foaming coating and the polar base material of the synthetic leather and laying a material foundation for the manufacture of the organic silicon synthetic leather with high physical property.
Description
Technical Field
The invention belongs to the technical field of synthetic leather, and particularly relates to an organic silicon synthetic leather foaming coating and a preparation method thereof.
Background
Organic silicon is used as an organic chemical material which can be produced without depending on petroleum resources, has a plurality of excellent performances such as high and low temperature resistance, aging resistance, wear resistance, hydrophobicity, physiological inertia and the like due to a specific-Si-O-Si-structure, and is widely applied to the field of leather/synthetic leather in the form of an auxiliary agent for many years. With the continuous advance of the industrial cleaning of synthetic leather and the continuous improvement of the manufacturing technology, in recent years, organosilicon materials are beginning to be applied to the manufacturing of synthetic leather in the form of coating, i.e. a new generation of organosilicon synthetic leather. The organosilicon synthetic leather coating is mainly constructed based on a hydrosilylation reaction system between vinyl silicone oil and hydrogen-containing silicone oil, no organic solvent is needed in the production process, no gas is generated, the environmental pollution can be greatly reduced, and Volatile Organic Compounds (VOCs) are not produced in the product. In view of unique resources, performance and environmental protection advantages, the synthetic leather based on the organic silicon coating material can meet the market demand of the current high-quality ecological synthetic leather, and has great development prospect.
However, as an emerging product, the development process of the organic silicon synthetic leather is not long. There are still more imperfections than the polyurethane synthetic leather which is currently the mainstream in the market. In the synthetic leather structure aspect, the traditional polyurethane synthetic leather is generally composed of five parts, namely a surface effect layer, a surface layer, an intermediate foaming layer, an adhesive layer and a base material, and each part plays an important role in the overall performance of the synthetic leather. However, due to the mismatch between the manufacturing technology and the coating material, the existing foaming coating technology applicable to the organic silicon synthetic leather is relatively deficient. The foaming layer plays a key role in endowing the synthetic leather with full hand feeling, foam feeling and fullness, and improving the quality and market competitiveness of the synthetic leather. Therefore, the preparation technology of the organic silicon foaming coating is enriched by combining the physical property requirement and the process characteristic of the synthetic leather, and an important foundation is laid for further popularization and application of the organic silicon synthetic leather.
Chinese patent CN111691193A discloses a foamed organic silicon synthetic leather and a preparation method thereof; the invention discloses foamed organic silicon synthetic leather which is composed of a surface layer, a foaming layer and a base layer which are sequentially stacked; the surface layer comprises vinyl polysiloxane, vinyl MQ silicon resin, white carbon black, hydrogen-containing polysiloxane, a platinum catalyst and an inhibitor; the foaming layer comprises vinyl polysiloxane, vinyl MQ silicon resin, alpha, omega-dihydroxy polysiloxane, hydroxyl silicone oil, white carbon black, hydrogen-containing polysiloxane, a platinum catalyst, an inhibitor and a tackifier. The foaming organosilicon synthetic leather is prepared by chemical foaming, the size distribution of foam holes of the foaming layer is uniform, the shape of the foaming layer is uniform and spherical, the usage amount of organosilicon is reduced, the cost is further reduced, and the foaming organosilicon synthetic leather has the characteristics of good mechanical property and light weight. The invention also provides a preparation method of the foaming organic silicon synthetic leather, which is simple and easy to operate, easy to popularize, low in equipment site cost investment and suitable for industrial mass production.
In the prior art, a chemical foaming method based on a dehydrogenation gas principle of reaction between silicon hydrogen and hydroxyl is used for foaming. The method has the advantages that foaming and coating vulcanization are carried out synchronously, the problems that foaming and vulcanization rates are difficult to coordinate and the foaming process is difficult to control exist, and further the actual process operation difficulty is increased, and the size of foam holes and the physical properties of a coating are difficult to regulate and control.
In the prior art, the foaming layer is prepared by adopting a single component of organic silicon, and the organic silicon is a non-polar polymer, and the synthetic leather base material is mostly a polar material such as polyethylene terephthalate (PET), nylon and the like, so the problems of insufficient mechanical strength of the coating and insufficient interlayer bonding force exist.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of an organic silicon synthetic leather foamed coating by fully combining the physical property requirements of the synthetic leather foamed coating, which comprises the following steps:
(1) adding the waterborne polyurethane into the hydroxyl silicone oil at the speed of 10-50mL/h, and mixing to obtain hydroxyl silicone oil-waterborne polyurethane oil-in-water emulsion; the mass ratio of the waterborne polyurethane to the hydroxyl silicone oil is 30-50: 50-70 parts of;
(2) adding a curing agent and a catalyst into the hydroxyl silicone oil-waterborne polyurethane water-in-oil emulsion, mixing, and coating on the surface of release paper to obtain a coating to be cured; the mass ratio of the hydroxyl silicone oil to the curing agent to the catalyst is 100: 2: 0.1-0.3;
(3) and baking and drying the coating to be cured to obtain the organic silicon synthetic leather foamed coating.
Preferably, in the step (1), 50-70 parts of hydroxyl silicone oil is added into the dosing tank and placed under a dispersing machine, and is fully stirred at the rotating speed of 100-500 r/min. Under the condition of continuous stirring, slowly adding 30-50 parts of waterborne polyurethane into the hydroxyl silicone oil by adopting a peristaltic pump at the speed of 10-50mL/h, and obtaining the hydroxyl silicone oil-waterborne polyurethane water-in-oil emulsion after the addition is finished.
Preferably, in the step (2), the thickness of the coating is 0.8-1.0 mm.
Preferably, in the step (3), the baking temperature is 50-80 ℃ and the baking time is 3-5 min.
Preferably, in the step (3), the drying temperature is 100-120 ℃ and the drying time is 1-2 min.
Preferably, the hydroxyl silicone oil is alpha, omega-dihydroxy polysiloxane, and the viscosity is 5000-20000 mPas.
Preferably, the waterborne polyurethane is polyester waterborne polyurethane or polyether waterborne polyurethane, and the solid content is 20-40 wt%; the introduction of the waterborne polyurethane not only causes pores, but also improves the polarity and mechanical property of the organic silicon foaming coating, thereby improving the adhesive force between the organic silicon foaming coating and the polar base material of the synthetic leather and laying a material foundation for the manufacture of the organic silicon synthetic leather with high physical property.
Preferably, the curing agent is one or more of methyl orthosilicate, ethyl orthosilicate and butyl orthosilicate.
Preferably, the catalyst is bismuth isooctanoate and/or bismuth neodecanoate.
The invention also provides the organic silicon synthetic leather foamed coating prepared by the preparation method.
According to the invention, the organic silicon synthetic leather foaming coating is constructed in situ by means of the water-in-oil system precursor, so that the vulcanization and foaming can be carried out step by step, and the problem that the foaming and vulcanization rates are difficult to coordinate in the traditional process is solved.
Compared with the prior art, the technical scheme of the invention has the following advantages:
(1) the in-situ preparation method of the water-in-oil type organic silicon foaming coating is firstly provided, and the method does not need any emulsifier or foaming agent, and is used for forming pores by utilizing the volatilization of water in a double-component room temperature/low temperature curing silicon rubber system, so that a new idea is provided for the construction of the organic silicon synthetic leather foaming coating.
(2) The introduction of the Waterborne Polyurethane (WPU) not only causes holes, but also can form an interpenetrating network with the organic silicon component, thereby effectively improving the polarity and mechanical property of the organic silicon foaming coating and the adhesive force between the organic silicon foaming coating and the polar base material, and laying a material foundation for the manufacture of the organic silicon synthetic leather with high physical property.
(3) The foaming coating in-situ construction method based on the water-in-oil system can realize the step-by-step vulcanization and foaming, effectively overcomes the problem that the foaming and vulcanizing rates are difficult to coordinate in the traditional foaming process, and the cellular structure and the coating physical property have better controllability.
Drawings
FIG. 1 is a flow chart of in-situ preparation of the organic silicon synthetic leather foaming coating.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Example 1
(1) Preparing the hydroxyl silicone oil-water polyurethane water-in-oil emulsion:
70 parts of alpha, omega-dihydroxy polysiloxane of 5000 mPas is added into a batching tank and placed under a dispersion machine, and the alpha, omega-dihydroxy polysiloxane is fully stirred at the rotating speed of 100 r/min. Under the condition of continuous stirring, slowly adding 30 parts of aliphatic polyester waterborne polyurethane with the solid content of 20 wt% into alpha, omega-dihydroxy polysiloxane by adopting a peristaltic pump at the speed of 10mL/h, and obtaining hydroxyl silicone oil-waterborne polyurethane water-in-oil emulsion after the addition is finished;
(2) in-situ preparation of the organosilicon-polyurethane interpenetrating network foaming coating:
adding methyl orthosilicate into the water-in-oil emulsion prepared in the step (1), controlling the mass ratio of hydroxyl silicone oil to methyl orthosilicate to be 100:2, then adding 0.3 part of new bismuth decanoate, mixing uniformly, then quickly coating the mixture on the surface of release paper, controlling the thickness of a coating film to be 0.8mm, then placing the release paper in a 50 ℃ oven for curing for 3min, after the organosilicon component is completely cured, raising the temperature of the oven to 100 ℃, and continuously drying for 2min to remove internal moisture, thus obtaining the organosilicon-polyurethane interpenetrating network foamed coating.
The coating does not use any organic solvent in the preparation and use processes, and through comparison tests, compared with a single-component organic silicon foaming coating, the mechanical strength of the coating is improved from 1.8MPa to 2.8MPa, and the peel strength of the coating and a base fabric is improved from 35N/3cm to 45N/3 cm.
Example 2:
(1) preparing the hydroxyl silicone oil-water polyurethane water-in-oil emulsion:
60 parts of 10000 mPas alpha, omega-dihydroxy polysiloxane are added into a preparation tank and placed under a dispersion machine, and the mixture is fully stirred at the rotating speed of 200 r/min. Under the condition of continuous stirring, slowly adding 40 parts of aliphatic polyether type waterborne polyurethane with the solid content of 30 wt% into alpha, omega-dihydroxy polysiloxane by adopting a peristaltic pump at the speed of 20mL/h, and obtaining hydroxyl silicone oil-waterborne polyurethane water-in-oil emulsion after the addition is finished;
(2) in-situ preparation of the organosilicon-polyurethane interpenetrating network foaming coating:
adding tetraethoxysilane into the water-in-oil emulsion prepared in the step (1), controlling the mass ratio of hydroxyl silicone oil to tetraethoxysilane to be 100:2, then adding 0.2 part of new bismuth decanoate, mixing uniformly, then quickly coating the mixture on the surface of release paper, controlling the thickness of a coating film to be 0.8mm, then placing the release paper in an oven at 60 ℃ for curing for 3min, after the organosilicon components are cured completely, raising the temperature of the oven to 110 ℃, and continuously drying for 1min to remove internal moisture, thus obtaining the organosilicon-polyurethane interpenetrating network foaming coating.
The coating does not use any organic solvent in the preparation and use processes, and through comparison tests, compared with a single-component organic silicon foaming coating, the mechanical strength of the coating is improved from 1.8MPa to 3.2MPa, and the peel strength of the coating and a base fabric is improved from 35N/3cm to 48N/3 cm.
Example 3:
(1) preparing the hydroxyl silicone oil-water polyurethane water-in-oil emulsion:
50 parts of 20000 mPas alpha, omega-dihydroxy polysiloxane are added into a preparation tank and placed under a dispersion machine, and the mixture is fully stirred at the rotating speed of 500 r/min. Under the condition of continuous stirring, slowly adding 50 parts of aromatic polyether type waterborne polyurethane with the solid content of 40 wt% into alpha, omega-dihydroxy polysiloxane by adopting a peristaltic pump at the speed of 50mL/h, and obtaining hydroxyl silicone oil-waterborne polyurethane water-in-oil emulsion after the addition is finished;
(2) in-situ preparation of the organosilicon-polyurethane interpenetrating network foaming coating:
adding butyl orthosilicate into the water-in-oil emulsion prepared in the step (1), controlling the mass ratio of hydroxyl silicone oil to butyl orthosilicate to be 100:2, then adding 0.1 part of bismuth isooctanoate, mixing uniformly, then quickly coating the mixture on the surface of release paper, controlling the thickness of a coating film to be 1.0mm, then placing the release paper in an oven at 80 ℃ for curing for 5min, after the organosilicon components are cured completely, raising the temperature of the oven to 120 ℃, and continuously drying for 1min to remove internal moisture, thus obtaining the organosilicon-polyurethane interpenetrating network foaming coating.
The coating does not use any organic solvent in the preparation and use processes, and through comparison tests, compared with a single-component organic silicon foaming coating, the mechanical strength of the coating is improved from 1.8MPa to 3.9MPa, and the peel strength of the coating and a base fabric is improved from 35N/3cm to 50N/3 cm.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the spirit or scope of the invention.
Claims (10)
1. The preparation method of the organic silicon synthetic leather foaming coating is characterized by comprising the following steps:
(1) adding the waterborne polyurethane into the hydroxyl silicone oil at the speed of 10-50mL/h, and mixing to obtain hydroxyl silicone oil-waterborne polyurethane oil-in-water emulsion; the mass ratio of the waterborne polyurethane to the hydroxyl silicone oil is 30-50: 50-70 parts of;
(2) adding a curing agent and a catalyst into the hydroxyl silicone oil-water polyurethane water-in-oil emulsion, mixing, and coating on the surface of release paper to obtain a coating to be cured; the mass ratio of the hydroxyl silicone oil to the curing agent to the catalyst is 100: 2: 0.1-0.3;
(3) and baking and drying the coating to be cured to obtain the organic silicon synthetic leather foamed coating.
2. The method as claimed in claim 1, wherein the hydroxy silicone oil is stirred at a speed of 100-500r/min before being mixed in step (1).
3. The method according to claim 1, wherein in the step (2), the coating is applied to a thickness of 0.8 to 1.0 mm.
4. The method according to claim 1, wherein in the step (3), the baking temperature is 50-80 ℃ and the baking time is 3-5 min.
5. The method as claimed in claim 1, wherein the drying temperature in step (3) is 100-120 ℃ and the drying time is 1-2 min.
6. The method according to claim 1, wherein the hydroxy silicone oil is an α, ω -dihydroxy polysiloxane having a viscosity of 5000-.
7. The method according to claim 1, wherein the aqueous polyurethane is a polyester-based aqueous polyurethane or polyether-based aqueous polyurethane, and the solid content is 20 to 40 wt%.
8. The method of claim 1, wherein the curing agent is one or more of methyl orthosilicate, ethyl orthosilicate, and butyl orthosilicate.
9. The method according to claim 1, wherein the catalyst is bismuth isooctanoate and/or bismuth neodecanoate.
10. A silicone synthetic leather foamed coating prepared according to the preparation method of any one of claims 1 to 9.
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| CN115787311A (en) * | 2022-12-28 | 2023-03-14 | 四川大学 | Foaming method of organic silicon synthetic leather coating |
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| CN115787311A (en) * | 2022-12-28 | 2023-03-14 | 四川大学 | Foaming method of organic silicon synthetic leather coating |
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