CN114263048B - Organic silicon synthetic leather surface layer, preparation method and organic silicon synthetic leather - Google Patents
Organic silicon synthetic leather surface layer, preparation method and organic silicon synthetic leather Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 84
- 239000002649 leather substitute Substances 0.000 title claims abstract description 77
- 239000002344 surface layer Substances 0.000 title claims abstract description 42
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 37
- 239000010703 silicon Substances 0.000 title claims abstract description 37
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 94
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 93
- 229920002545 silicone oil Polymers 0.000 claims abstract description 79
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000006229 carbon black Substances 0.000 claims abstract description 35
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 32
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 18
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 14
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 13
- 229920001971 elastomer Polymers 0.000 claims abstract description 13
- 229920002050 silicone resin Polymers 0.000 claims abstract description 11
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 10
- 230000001070 adhesive effect Effects 0.000 claims description 61
- 239000000853 adhesive Substances 0.000 claims description 60
- 239000002994 raw material Substances 0.000 claims description 36
- 239000002245 particle Substances 0.000 claims description 24
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 18
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 16
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 14
- 239000012790 adhesive layer Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 9
- 229920005989 resin Polymers 0.000 claims description 8
- 239000011347 resin Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 6
- 229920000747 poly(lactic acid) Polymers 0.000 claims description 6
- 239000004626 polylactic acid Substances 0.000 claims description 6
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000002210 silicon-based material Substances 0.000 abstract description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 30
- 239000010985 leather Substances 0.000 description 22
- 230000000052 comparative effect Effects 0.000 description 20
- PFTIVKCRALCOLB-UHFFFAOYSA-N [SiH4].[N] Chemical compound [SiH4].[N] PFTIVKCRALCOLB-UHFFFAOYSA-N 0.000 description 17
- 239000010410 layer Substances 0.000 description 13
- 238000004132 cross linking Methods 0.000 description 10
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- 238000002474 experimental method Methods 0.000 description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 8
- 238000005299 abrasion Methods 0.000 description 7
- 238000005259 measurement Methods 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000003112 inhibitor Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
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- 239000000126 substance Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
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- GJWAPAVRQYYSTK-UHFFFAOYSA-N [(dimethyl-$l^{3}-silanyl)amino]-dimethylsilicon Chemical compound C[Si](C)N[Si](C)C GJWAPAVRQYYSTK-UHFFFAOYSA-N 0.000 description 2
- 125000000852 azido group Chemical group *N=[N+]=[N-] 0.000 description 2
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- OGWVYCFORNDBRE-UHFFFAOYSA-N n,n-bis(trimethylsilyl)ethanamine Chemical compound CCN([Si](C)(C)C)[Si](C)(C)C OGWVYCFORNDBRE-UHFFFAOYSA-N 0.000 description 2
- ZSMNRKGGHXLZEC-UHFFFAOYSA-N n,n-bis(trimethylsilyl)methanamine Chemical compound C[Si](C)(C)N(C)[Si](C)(C)C ZSMNRKGGHXLZEC-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
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- 239000000377 silicon dioxide Substances 0.000 description 2
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229920001410 Microfiber Polymers 0.000 description 1
- ACIMRXKJKQGBGL-UHFFFAOYSA-N N-(2-aminoethyl)-5-chloro-1-naphthalenesulfonamide Chemical compound C1=CC=C2C(S(=O)(=O)NCCN)=CC=CC2=C1Cl ACIMRXKJKQGBGL-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Synthetic Leather, Interior Materials Or Flexible Sheet Materials (AREA)
Abstract
The application relates to the field of organic silicon materials, in particular to an organic silicon synthetic leather surface layer, a preparation method and organic silicon synthetic leather, wherein the organic silicon synthetic leather comprises base rubber, vinyl silicone oil B, a cross-linking agent, vinyl silicone resin, a catalyst, silicone wax and polytetrafluoroethylene powder, and the base rubber A comprises vinyl silicone oil, silazane and white carbon black. The organic silicon synthetic leather prepared from the organic silicon synthetic leather surface layer has good simulated hand feeling, and has good wear resistance, folding resistance and stain resistance.
Description
Technical Field
The application relates to the field of organic silicon materials, in particular to an organic silicon synthetic leather surface layer, a preparation method and organic silicon synthetic leather.
Background
Leather is a popular material, has wide application in the fields of clothing, decoration and the like, and has huge market. Artificial leather, i.e., synthetic leather, is a substitute for leather, which has a leather-like feel and appearance, and at the same time has the advantages of corrosion resistance, water resistance, high utilization rate, and low cost as compared to natural leather.
The organic silicon synthetic leather is a new member of large families of synthetic leather, has high-quality pollution resistance, acid-base resistance, aging resistance and hydrolysis resistance, and has obvious advantages compared with the traditional polyethylene synthetic leather, polyurethane synthetic leather and the like. In addition, the organic solvent is generally not needed in the preparation process of the organic silicon synthetic leather, and the organic solvent is carried out in an aqueous phase, so that the volatile solvent remained after the preparation is finished is less, and the organic silicon synthetic leather is more friendly to people and environment.
At present, the more widely applied organosilicon synthetic leather is limited in that the touch feeling of the organosilicon synthetic leather is still obviously different from that of real leather.
Disclosure of Invention
In order to improve the surface touch feeling of the organic silicon synthetic leather and enable the surface touch feeling to be more similar to that of natural leather, the application provides an organic silicon synthetic leather surface layer, a preparation method and organic silicon synthetic leather.
Firstly, the application provides organic silicon synthetic leather, wherein the raw materials of the synthetic leather surface layer comprise the following components in parts by mass:
base adhesive A:100 parts of
Vinyl silicone oil B: 2-10 parts;
crosslinking agent: 2 to 3.5 portions;
vinyl silicone resin: 2-6 parts;
catalyst: 0.5 to 5 parts
Silicon wax: 5-20 parts;
polytetrafluoroethylene powder: 5-20 parts;
wherein, the raw material of the base adhesive A is mainly vinyl silicone oil A, and further comprises white carbon black accounting for 20-30% of the mass fraction of the raw material of the base adhesive A and nitrogen silane accounting for 5-12% of the mass fraction of the raw material of the base adhesive A.
In the technical scheme, the base rubber A is taken as a base material, the main body of the base rubber A is vinyl silicone oil, and after adding the nitrogen silane and the white carbon black, a nitrogen silane-white carbon black composite system is formed, so that a firm silicon-based rubber system is formed, on the basis of the system, the overall viscosity is regulated through the vinyl silicone oil B, and then an overall silicon rubber structure is formed through a catalyst and a cross-linking agent. Under the action of silica wax and polytetrafluoroethylene powder, the whole surface gloss of the system is better, and the formed system is closer to natural leather and has better stain resistance and water resistance.
In the technical scheme, a more compact cross-linking structure is formed through the combination of silazane and white carbon black, after the cross-linking structure is formed, the uniform distribution of silicone wax and polytetrafluoroethylene powder can be better promoted, the feel similar to leather is formed, and in general, polytetrafluoroethylene powder with the grain diameter smaller than 30 mu m is preferably selected, and the polytetrafluoroethylene powder with the grain diameter larger causes roughness on the surface to a certain extent.
The vinyl silicone resin system is added to improve the toughness of the whole surface layer, and because the vinyl silicone resin has a complex crosslinking structure, compared with components of vinyl silicone oil, the strength is higher, and the positioning effect is easier to form in the system, so that the strength and the touch feeling of the surface layer can be better improved as a part of a base material.
The cross-linking agent can be hydrogen-containing silicone oil, and the catalyst is generally platinum catalyst and is used for catalyzing the reaction between vinyl silicone oil and hydrogen-containing silicone oil. Meanwhile, the inhibitor with the mass part not exceeding 0.2 can be added to inhibit the catalytic activity of the platinum catalyst so as to adjust the whole processing performance and obtain the corresponding curing speed. Among the silazane compounds, tetramethyldisilazane, hexamethyldisilazane, heptamethyldisilazane, bis (trimethylsilyl) ethylamine may be used, a series of cyclic silazanes may be used, and if necessary, a silazane system having vinyl groups and azido groups may be used. In order to promote the hydrolysis of silazane, deionized water with the mass part of 2-5 wt% can be further added into the system.
Optionally, the nitrogen silane at least comprises vinyl nitrogen silane accounting for 0.5-0.8% of the total mass of the raw material of the base adhesive A.
In the technical scheme, the vinyl nitrogen silane is added to form a cross-linking structure between the nitrogen silane and the base adhesive A, and because the nitrogen silane is combined with the surface of the white carbon black, the cross-linking structure is formed on the parts of the white carbon black and the vinyl silicone oil, so that the overall strength and the wear resistance are improved, the white carbon black is better dispersed in a surface layer system, the surface is more glossy, the components of the surface layer are uniformly cured, and the surface defect is not easy to form.
Optionally, the raw material of the base adhesive A also comprises hydroxyl silicone oil accounting for 2-8% of the total mass of the raw material of the base adhesive A.
In the technical scheme, the hydroxyl silicone oil can modify the surface of the white carbon black, so that the white carbon black can play a thixotropic role more stably, is not easy to solidify too fast on the one hand, improves the service processability of the base adhesive A, improves the stability and uniformity of white carbon black distribution, reduces agglomeration, further improves the flexibility and the simulation degree of the surface, and further improves the stain resistance and the hand feel of the artificial leather.
Optionally, the polytetrafluoroethylene has a particle size of no more than 5 μm.
Polytetrafluoroethylene particles not larger than 5 μm can make the surface smoother and more fit with the hand feeling of natural leather.
Optionally, the raw material of the synthetic leather surface layer further comprises 1-2 parts of silicon nitride particles, and the particle size of the silicon nitride particles is not more than 1 mu m.
In the technical scheme, the silicon nitride particles are added to facilitate the combined action with polytetrafluoroethylene, so that the wear resistance of the surface layer is further improved, and on one hand, the silicon nitride particles have better lubricity, so that the surface is smoother and dirt-resistant.
Optionally, the raw materials of the synthetic leather surface layer further comprise 3-5 parts of polylactic resin.
In the technical scheme, the polylactic acid resin can improve the viscosity of the surface layer, and the composite performance of the surface layer and other materials is improved under the condition that the whole touch feeling is not influenced, so that the whole strength of the organic silicon synthetic leather is improved. Meanwhile, the polylactic acid resin can improve the overall softness, so that the organic silicon synthetic leather has better hand feeling.
Optionally, in the base adhesive A, the components with different viscosities in the vinyl silicone oil A account for the following mass percent of the raw materials of the base adhesive A:
vinyl silicone oil A-1:20000 mpa.s 40-50%;
vinyl silicone oil A-2:300000 mpa.s 5-10%;
vinyl silicone oil A-3:100000 mpa.s 2-3%.
By adopting the proportion of the vinyl silicone oil, the overall viscosity is proper, the final configuration is most similar to the hand feeling of natural leather, and the overall performance is better in all aspects.
Further preferably, the specific surface area of the white carbon black is not less than 300, which is favorable for fully playing the thixotropic effect and has better reinforcing performance.
Preferably, the vinyl content of the vinyl silicone resin is not less than 2%, more preferably, the vinyl content of the vinyl silicone resin is not less than 2.7%. The increase of the vinyl content is beneficial to improving the crosslinking degree of the interior of the surface layer of the organic silicon synthetic leather, reducing the surface cracking in the preparation process,
In addition, the application also provides a preparation method of the organic silicon synthetic leather surface layer, which comprises the following steps:
preparation of base adhesive A: mixing 70-80% of vinyl silicone oil A-1 with vinyl silicone oil A-2, vinyl silicone oil A-3 and other components except white carbon black uniformly, adding white carbon black, heating to 120-170 ℃ after mixing uniformly, adding the residual vinyl silicone oil A-1, and stirring uniformly to obtain base rubber A.
In the system, the prepared organic silicon synthetic leather surface layer has soft texture, and the vinyl silicone oil A-1 is added twice in the preparation process of the base rubber A, so that the vinyl silicone oil A-1 has lower overall viscosity, can be rapidly dispersed in the premixed base rubber A system, and can promote the further uniform distribution of the white carbon black.
After the preparation of the base adhesive A is finished, the base adhesive A can be continuously mixed with other components and uniformly stirred, and then the preparation can be finished after vacuum defoaming for 0.5 to 2 hours.
In addition, the application also provides organosilicon synthetic leather, including the substrate, set up the adhesive linkage on the substrate and set up the surface course on the adhesive linkage, wherein the surface course is the organosilicon synthetic leather surface course of any one of claims 1 ~ 7, the adhesive linkage includes following component according to the part by mass:
base adhesive B:100 parts;
crosslinking agent: 1 to 3.5 minutes;
catalyst: 0.05-1 part;
silane coupling agent: 2-8 parts;
wherein the base adhesive B is mainly vinyl silicone oil C and at least comprises 20-30% of white carbon black by mass of the base adhesive B.
In the technical scheme, the vinyl silicone oil system is adopted as the bonding layer, the whole system is uniform, the bonding property is good, an organic solvent is basically not needed in the process, and the whole system is healthy and environment-friendly.
The base rubber B can be prepared by uniformly stirring the components in a kneader after mixing, and can be prepared by continuously adding other components and uniformly stirring, and then defoaming in vacuum for 0.5-2 hours.
Similarly to the surface layer, hydroxyl silicone oil can be added into the raw material of the base adhesive B, and the white carbon black is treated, wherein the addition amount of the hydroxyl silicone oil is preferably 0.1-1% of the total mass fraction of the base adhesive B.
In the adhesive layer, the inhibitor can be added with not more than 0.2 part, the cross-linking agent is hydrogen silicone oil, and the catalyst is platinum catalyst. Likewise, other cross-linking agents and catalysts may be used (e.g., polycarbomethylsilane may be used as the cross-linking agent and amine-based temporary catalysts may be used as the catalyst).
Optionally, the base adhesive B also comprises 5 to 11 percent of nitrogen silane compound and 0.1 to 1 percent of hydroxyl silicone oil in percentage by mass of the base adhesive B
In the above technical scheme, among the silazane compounds, tetramethyl disilazane, hexamethyl disilazane, heptamethyl disilazane and di (trimethylsilyl) ethylamine may be selected, or a series of cyclic silazanes may be selected, and if necessary, it is also possible to select a silazane system with vinyl and azido groups. Deionized water may also be added to promote hydrolysis of the silazane to form a better crosslinking system. The addition amount of deionized water is generally 0.5-4% of the total mass fraction of the base adhesive B;
after adding the nitrogen silicane, a cross-linking system of white carbon black and silica gel can be formed in the bonding layer, so that the whole structure is more compact, and the bonding performance between the bonding layer and the surface layer is improved.
In summary, the present application includes at least one of the following beneficial effects:
1. in the present application, a synthetic leather system having a good touch feeling can be formed by forming a base gum using vinyl silicone oil and white carbon black as main bodies, and adding components such as vinyl silicone resin, silicone wax, polytetrafluoroethylene powder, and the like. In addition, the nitrogen silane is added into the surface layer to form a firmer and tighter crosslinking system, and the whole surface layer has better wear resistance, dirt resistance, toughness and touch feeling.
2. In the further setting of the application, the system has higher crosslinking degree, better strength and wear resistance and more uniform and glossy surface through the combination of vinyl silazane and hexamethyldisilazane.
3. In this application further sets up, through adjusting vinyl silicone oil A's concrete ratio, forms the system that more laminates in natural leather sense of touch. In addition, the uniformity, the wear resistance and the wear resistance of the whole body can be improved by adding silicon nitride particles and polylactic resin,
Detailed Description
The present application is further described in detail in connection with and examples below.
In the following examples, the sources of some of the raw materials are shown in Table 1.
Table 1, materials information table
| Material | Manufacturer/model/parameter |
| Vinyl silicone oil A-1 | 20000 mpa.s, vinyl content 0.27%, xinanjiang chemical industry |
| Vinyl silicone oil A-2 | 300000 mpa.s, vinyl content 0.15%, xinanjiang chemical industry |
| Vinyl silicone oil A-3 | 100000mpa·s, vinyl content is 0.1%, xinanjiang chemical industry |
| Vinyl silicone oil B | 20000 mpa.s, vinyl content 0.27%, xinanjiang chemical industry |
| Vinyl silicone oil C | 100000 mpa.s with vinyl content of 0.15%, chemical industry of Xinanjiang |
| Vinyl silicone resin | 2.7% vinyl content, solids content 50%, viscosity 100000 mpa.s |
| Catalyst | 5000ppm platinum catalyst |
| Silane coupling agent | KH-550 |
| Silica wax | C28 silicone wax |
| White carbon black | 300 specific surface area, average grain size range of 100-200 nm |
| Inhibitors | TMDO |
| Polytetrafluoroethylene powder | Bo Long Fu material |
| Hydroxy silicone oil | A hydroxyl group content of 8.5%, |
| silicon nitride particles | Beijing porcelain |
| Polylactic acid resin | Sea positive organism REVODE290 |
| Crosslinking agent | Hydrogen-containing silicone oil containing 0.72% hydrogen and having a viscosity of 200 mPa.s |
The preparation A series is base adhesive A.
The raw material compositions of preparation examples A-1 to A-12 are shown in Table 2.
TABLE 2 component proportions (wt%) of base gums A in preparation examples A-1 to A-12
In preparation examples A-1 to A-12, the preparation method of the base adhesive A is as follows:
mixing vinyl silicone oil A-1 with the mass fraction of 80% with vinyl silicone oil A-2, vinyl silicone oil A-3, nitrogen silane, deionized water and hydroxyl silicone oil (if any) at room temperature, stirring for 20min in a kneader, adding white carbon black in five batches, keeping stirring at the interval of 2min between every two batches, heating to 120 ℃ after the addition is finished, adding the rest vinyl silicone oil A-1, and stirring for 5min.
In the above examples, the silazanes were all hexamethyldisilazane.
The mass of the single-time configuration base adhesive A in the laboratory is 0.5kg.
Preparation example A-13, which is used for preparing the base gum A, is different from preparation example A-1 in that, in the preparation process, after the white carbon black is added, the temperature is raised to 170 ℃.
Preparation A-14, which was used for the preparation of base gum A, was different from preparation A-1 in that all the components were directly mixed and stirred at 120℃for 20 minutes.
Preparation example A-15, which was used for preparing the base rubber A, was different from preparation example A-1 in that kneading treatment was continued at room temperature after the addition of the white carbon black.
Preparation A-16, which is used for preparing base gum A, differs from preparation A-1 in that the silazane is hexamethyldisilazane which accounts for 10% of the mass fraction of the raw material of base gum A and vinyl silazane which accounts for 0.5% of the mass fraction of the raw material of base gum A.
Preparation A-17, which is used for preparing base gum A, differs from preparation A-1 in that the silazane is hexamethyldisilazane which accounts for 5% of the mass fraction of the raw material of base gum A and vinyl silazane which accounts for 0.8% of the mass fraction of the raw material of base gum A.
Preparation A-18, which is used for preparing base gum A, differs from preparation A-1 in that the silazane is hexamethyldisilazane which accounts for 8% of the mass fraction of the raw material of base gum A and vinyl silazane which accounts for 1% of the mass fraction of the raw material of base gum A.
Preparation A-19, which is used to prepare base gum A, differs from preparation A-9 in that the silazane is hexamethyldisilazane, which is 10% by mass of the base gum A material, and vinyl silazane, which is 0.5% by mass of the base gum A material.
Preparation A-20, which is used for preparing base gum A, differs from preparation A-9 in that the silazane is hexamethyldisilazane which accounts for 5% of the mass fraction of the raw material of base gum A and vinyl silazane which accounts for 0.8% of the mass fraction of the raw material of base gum A.
Preparation B series, base gum B.
The components of preparation examples B-1 to B-8 are shown in Table 3.
TABLE 3 preparation methods of preparation examples B-1 to B-8
| Component (A) | Vinyl silicone oil C | White carbon black | Nitrogen silanes | Hydroxy silicone oil | Deionized water |
| Preparation example B-1 | Allowance of | 30 | 0 | 0 | 0 |
| PREPARATION EXAMPLE B-2 | Allowance of | 25 | 0 | 0 | 0 |
| Preparation example B-3 | Allowance of | 20 | 0 | 0 | 0 |
| PREPARATION EXAMPLE B-4 | Allowance of | 25 | 11 | 0.1 | 4 |
| PREPARATION EXAMPLE B-5 | Allowance of | 25 | 8 | 0.5 | 3 |
| PREPARATION EXAMPLE B-6 | Allowance of | 25 | 5 | 1 | 2 |
| PREPARATION EXAMPLE B-7 | Allowance of | 25 | 8 | 0 | 3 |
| PREPARATION EXAMPLE B-8 | Allowance of | 25 | 0 | 0.5 | 0 |
In preparation examples B-1 to B-8, the nitrogen silane was hexamethyldisilazane, and the vinyl silicone oil C was a vinyl silicone oil having a viscosity of 100000 mpa.s.
Preparation B-9, which is a base gum B, differs from preparation B-5 in that the nitrogen silane is hexamethyldisilazane, which is 8% by mass of the base gum B, and vinyl-nitrogen silane, which is 0.2% by mass of the base gum B.
Preparation B-10, which is a base gum B, differs from preparation B-5 in that the nitrogen silane is hexamethyldisilazane, which is 10% by mass of the base gum B, and vinyl-nitrogen silane, which is 0.1% by mass of the base gum B.
Preparation B-11, which is a base gum B, differs from preparation B-5 in that the nitrogen silane is hexamethyldisilazane, which is 5% by mass of the base gum B, and vinyl-nitrogen silane, which is 0.4% by mass of the base gum B.
In the preparation example B series, the preparation method of the base adhesive B is as follows: the above components were mixed and kneaded in a kneader for 10 minutes to obtain the final product.
The preparation example C series is an adhesive layer of organic silicon artificial leather, and is prepared by using a base adhesive B.
The components of preparation examples C-1 to C-11 are the same, except that the base gums B selected in preparation examples C-1 to C-11 are the base gums B in preparation examples B-1 to B-11, respectively.
In preparation examples C-1 to C-13, the amounts of the specific raw material components are shown in Table 4.
TABLE 4 preparation examples C-1 to C-13 Material Components
| Dosage (kg) | Base adhesive B | Crosslinking agent | Catalyst | Silane coupling agent | Inhibitors |
| Preparation examples C-1 to C-11 | 10 | 0.1 | 0.005 | 2 | 0.02 |
| PREPARATION EXAMPLE C-12 | 10 | 0.2 | 0.05 | 5 | 0.02 |
| PREPARATION EXAMPLE C-13 | 10 | 3.5 | 0.1 | 8 | 0.02 |
Wherein, in preparation examples C-12 to C-13, the base adhesive B in preparation example B-10 is selected.
The preparation methods of preparation examples C-1 to C-13 are as follows: and adding a cross-linking agent, a catalyst, a silane coupling agent and an inhibitor into the base adhesive B, uniformly stirring, and then, vacuum defoaming for 2 hours to obtain the bonding layer.
The example a series is a silicone synthetic leather facing.
The preparation examples A-1 to A-20 used the same amount of raw materials, except that the base adhesive A was selected differently. The specific components of the raw materials are shown in Table 5.
The base gums A prepared in preparation examples A-1 to A-20 were used in examples A-1 to A-20, respectively.
In examples A-21 to A-28, the raw material composition of the surface layer is shown in Table 5.
Table 5, raw material composition tables of examples A-1 to A-28
In examples A-21 to A-28, the base adhesive A used was the base adhesive A used in preparation example A-19. The particle size of the polytetrafluoroethylene powder was 5. Mu.m. In examples A-24, A-25 and A-28, the particle diameter of the silicon nitride particles was 1. Mu.m.
In examples A-1 to A-28, the preparation method of the organic silicon synthetic leather surface layer is as follows:
and adding all other components into the base adhesive A, uniformly stirring, and then, carrying out vacuum defoaming for 2 hours to obtain the adhesive.
Examples A-29 are different from examples A-28 in that the particle diameter of the silicon nitride particles is 5. Mu.m.
Example A-30 was different from example A-28 in that the particle size of polytetrafluoroethylene powder was 10. Mu.m.
Example A-31 was different from example A-28 in that the particle size of polytetrafluoroethylene powder was 20. Mu.m.
Comparative example a series is also a silicone synthetic leather facing.
Comparative example A-1 differs from example A-1 in that in the proportion of the base gum A, the silazane is replaced by vinyl silicone oil A by equal mass.
Comparative example A-2 differs from example A-1 in that in the proportion of the base rubber A, silazane accounts for 2% by mass of the base rubber A raw material.
Comparative example A-3 differs from example A-1 in that no vinyl silicone oil B was added.
Comparative example A-4 differs from example A-1 in that no vinyl silicone resin was added.
Comparative example A-5 differs from example A-1 in that no silicone wax was added.
Comparative example A-6 differs from example A-1 in that polytetrafluoroethylene powder was not added.
The example B series and the comparative example B series are both silicone synthetic leather.
The preparation method of the organic silicon synthetic leather comprises the following steps:
and (3) coating an organic silicon synthetic leather surface layer on release paper, wherein the coating thickness is 0.5mm, curing for 5min at 150 ℃ after coating, then coating an organic silicon synthetic leather bonding layer on the organic silicon synthetic leather surface layer, coating thickness is 0.1mm, attaching a microfiber fiber substrate after coating, curing for 5min at 150 ℃, and stripping the release paper after curing.
First, in order to select a material having a good adhesive property, examples A-1, A-10 and A-16 were combined with each other in preparation examples C-1 to C-13, respectively, to obtain the following examples.
Examples B-1-1 to B-1-13, the organosilicon synthetic leather surface layers are all examples A-1, and the bonding layers are respectively prepared from examples C-1 to C-13.
Examples B-10-1 to B-10-13, the organosilicon synthetic leather surface layers are all examples A-10, and the bonding layers are respectively prepared from examples C-1 to C-13.
Examples B-16-1 to B-16-13, the organosilicon synthetic leather surface layers are all examples A-16, and the bonding layers are respectively prepared from examples C-1 to C-13.
For the above examples, the bonding strength of the facing layer and the substrate was measured by referring to the B method of GB/T8808-1988 Soft composite Plastic Material peeling test method. The measurement temperature was 20 ℃.
In the above examples, the bonding strength is shown in Table 6.
TABLE 6 peel strength for some examples
As is clear from the above examples, in preparation examples C-4 to C-6, the addition of the nitrogen silane and the hydroxyl silicone oil to the base adhesive B, and the addition of deionized water to promote hydrolysis while adding the nitrogen silane, can greatly improve the adhesive strength between the adhesive layer and the surface layer. And the surface layer added with the hydroxyl silicone oil in the base adhesive A system has more obvious lifting effect, and can have stronger bonding capability between the hydroxyl silicone oils and the nitrogen silane, so that the overall bonding strength is enhanced. Further, when the nitrogen silane system in the base adhesive B is selected as the combination of hexamethyldisilazane and vinyl nitrogen silane, the overall adhesion is further improved, and especially in the series of examples B-16-N prepared in examples a-16, which also contain vinyl nitrogen silane in the system of the base adhesive a, the adhesion between the adhesive layer and the surface layer is greatly improved due to the inter-bonding capability between the vinyl nitrogen silanes. In the subsequent example settings, the adhesive layers of preparation C-10 were all selected for preparation.
In examples B-10-1 to B-10-31, the adhesive layers were the adhesive layers in preparation C-10, and the top layers were the top layers in examples A-1 to A-31, respectively.
The adhesive layers of comparative examples B-10-1 to B-10-6 were the adhesive layers of preparation C-10, and the facing layers were the facing layers of comparative examples A-1 to A-6, respectively.
For the above examples, the properties thereof were determined by the following experiments.
1. Leather simulation test 1, 30 volunteers (general consumers) were found, and one of the above artificial leather samples and five of the natural leather samples were placed in a black box while a natural leather control sample was placed outside the black box. Volunteers judge which piece of the artificial leather is the artificial leather by touching the sample in the black box and comparing the sample with the natural cow leather, and judge the simulation performance of the artificial leather through the accuracy.
2. And (3) carrying out leather simulation measurement, namely selecting 10 leather practitioners, grading the similarity degree of the artificial leather and leather, wherein five grades are closest, one grade is the least closest, and taking an average after grading is finished.
3. Abrasion resistance measurement, refer to QB-T2726-2005 determination of abrasion resistance of leather physical and mechanical test, and adopt CS10 grinding wheel, load weight 1000g, equipment friction rotation speed 70rpm, friction revolution 50000 r, refer to standard of section 6.6 Table 3 in GB/T40350-2021 general technical requirement of polyvinyl chloride artificial leather for household.
4. Folding resistance the above artificial leather was folded, taken down every thousand times and observed, and the time at which significant breakage occurred was recorded, with reference to "determination of folding fastness for physical and mechanical test of QB-T2714-2005 leather".
5. Stain resistance measurement, the stain resistance of the artificial leather to an oily pen, a water-based pen, alcohol, red wine, coffee, olive oil and fine sand mixture was measured by referring to the stain resistance measurement of the synthetic leather test method of QB/T5070-2017.
First, the above experiments were conducted on examples B-10-1 to B-10-7 and comparative examples B-10-1 to B-10-6, and the results are shown in Table 7.
Table 7, results of experiments of B-10-1 to B-10-7 and comparative examples B-10-1 to B-10-6
Further, specific scores were made according to the scale in experiment 2 for softness, smoothness and glossiness, and the scoring results of the above examples and preparations are shown in table 8.
Table 8, simulated specific dimension scoring for examples and comparative examples
| Scoring of specific dimensions | Softness and softness | Surface touch feeling | Gloss level |
| Example B-10-1 | 4.3 | 4.0 | 3.8 |
| Example B-10-2 | 4.4 | 3.9 | 3.8 |
| Example B-10-3 | 4.3 | 3.8 | 3.9 |
| Example B-10-4 | 4.2 | 4.0 | 3.9 |
| Example B-10-5 | 4.3 | 3.9 | 3.9 |
| Examples B to 10 to 6 | 4.3 | 3.9 | 4.0 |
| Examples B to 10 to 7 | 4.2 | 3.9 | 3.9 |
| Comparative example B-10-1 | 2.6 | 1.7 | 1.9 |
| Comparative example B-10-2 | 3.0 | 2.0 | 2.4 |
| Comparative example B-10-3 | 1.9 | 3.1 | 2.4 |
| Comparative example B-10-4 | 1.7 | 2.2 | 1.8 |
| Comparative example B-10-5 | 2.9 | 1.4 | 1.7 |
| Comparative example B-10-6 | 2.7 | 1.5 | 2.0 |
As is apparent from the above experiments, in the present application, the prepared artificial leather has a more similar appearance and feel to the natural leather than the artificial leather of the comparative example. The property comparison between artificial leather and natural leather mainly includes various dimensions of softness, glossiness, surface touch, etc., and in the above-described embodiments, mainly provides better surface touch and glossiness compared to polytetrafluoroethylene and silicone wax, while improving the overall stain resistance. The vinyl silicone oil B can adjust the overall softness, and the vinyl silicone resin adjusts the softness and the surface glossiness, so that the surface touch is obviously influenced. The above components work together to form an artificial leather having obvious natural leather properties.
Further, experiments 1 to 4 were performed on examples B-10-8 to B-10-20, and softness, gloss and surface touch were respectively scored, and the results are shown in Table 9.
Table 9, experimental results of B-10-8 to B-10-20
In the experiment, the hydroxyl silicone oil is added in the examples B-10-8-B-8-10, and the hydroxyl silicone oil is favorable for improving the strength and flexibility of the finished network structure, and has better flexibility in the molecular chain, so that the surface touch feeling is obviously improved. The hydroxyl silicone oil is used for carrying out certain modification on the white carbon black, so that the white carbon black is uniformly dispersed, is not easy to agglomerate, and forms a smoother surface. However, too much hydroxyl silicone oil in the embodiment B-10-10 can cause the decrease of the internal strength of the system, and has adverse effects on the wear resistance and the folding resistance.
In examples B-10-11 and B-10-12, the composition of vinyl silicone oil A was adjusted, which had a significant effect on the feel of the final artificial leather.
Examples B-10-13 to B-10-15 the preparation process was adjusted to a certain extent. In examples B-10-14, all the components were directly mixed so that the white carbon black in the base adhesive A exerted its thixotropic effect too quickly, resulting in an overall hard artificial leather with easily blemished surface. In the embodiment B-10-15, the temperature of the white carbon black is not increased after the white carbon black is added, but the white carbon black is treated at room temperature, so that the reaction of the whole internal network structure is poor, and in the subsequent curing process, the abrasion resistance and the folding resistance of the white carbon black are reduced due to insufficient surface toughness.
In examples B-10-16 to B-10-20, the nitrogen silane was selected from the group consisting of hexamethyldisilazane and vinyl nitrogen silane. Through the coupling effect between vinyl nitrogen silane and vinyl silicone oil under the action of a catalyst, the surface touch and glossiness of the synthetic leather are further improved, and meanwhile, the folding resistance and wear resistance of the synthetic leather are further improved. However, the vinyl nitrogen silane is added in an amount of 0.5 to 0.8% by mass based on the mass of the base adhesive A, which results in hardening of the whole.
Further, experiments 1 to 4 were conducted on examples B-10-21 to B-10-31, and softness, gloss and surface touch were respectively scored, and the results are shown in Table 10.
Table 10, B-10-21 to B-10-31 experimental results
In examples B-10-24 to B-10-28, silicon nitride and polylactic acid resin were further added. The silicon nitride is helpful for filling up small gaps on the surface, and further improves the flatness and smoothness of the surface. Meanwhile, the silicon nitride particles have better wear resistance, although the highest abrasion resistance grade is five in the abrasion resistance grade evaluation, the samples containing the silicon nitride particles further pass the stain resistance test after the abrasion resistance grade evaluation, and the stain resistance performance of the samples without the silicon nitride particles is still complete, and the surfaces of the samples without the silicon nitride particles are reduced in the stain resistance performance measurement after the abrasion resistance measurement, although the surfaces have no obvious loss. The polylactic acid resin is favorable for improving the overall softness, and meanwhile, the toughness is improved, so that the simulation degree and the folding resistance of the artificial leather are further improved.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.
Claims (7)
1. The organic silicon synthetic leather surface layer is characterized by comprising the following raw materials in parts by mass:
base adhesive A:100 parts of
Vinyl silicone oil B: 2-10 parts;
crosslinking agent: 2 to 3.5 portions;
vinyl silicone resin: 2-6 parts;
catalyst: 0.5 to 5 parts
Silicon wax: 5-20 parts;
polytetrafluoroethylene powder: 5-20 parts;
wherein, the raw material of the base adhesive A is mainly vinyl silicone oil A, and also comprises white carbon black accounting for 20-30% of the mass fraction of the raw material of the base adhesive A, silazane accounting for 5-12% of the mass fraction of the raw material of the base adhesive A, and hydroxyl silicone oil accounting for 2-8% of the total mass of the raw material of the base adhesive A; the silazane at least comprises vinyl silazane accounting for 0.5-0.8% of the total mass of the raw material of the base adhesive A;
in the base adhesive A, vinyl silicone oil A comprises three components with different viscosities and vinyl contents, namely vinyl silicone oil A-1, vinyl silicone oil A-2 and vinyl silicone oil A-3; the vinyl silicone oil A comprises the following components with different viscosities and vinyl contents in mass percentage of the raw materials of the base adhesive A:
vinyl silicone oil A-1:20000 The mpa.s, the vinyl content is 0.27 percent, and the mass fraction is 40-50 percent;
vinyl silicone oil A-2:300000 The mpa.s, the vinyl content is 0.15 percent, and the mass fraction is 5-10 percent;
vinyl silicone oil A-3:100000 The mass fraction of mpa.s is 2-3%, the vinyl content is 0.1%;
the viscosity of the vinyl silicone oil B is 20000 mpa.s, and the vinyl content is 0.27%.
2. The silicone synthetic leather facing according to claim 1, wherein the particle size of the polytetrafluoroethylene powder is not more than 5 μm.
3. The synthetic leather surface layer according to claim 1, wherein the raw material of the synthetic leather surface layer further comprises 1-2 parts of silicon nitride particles, and the particle size of the silicon nitride particles is not more than 1 μm.
4. The synthetic leather surface layer of claim 1, wherein the raw materials of the synthetic leather surface layer further comprise 3-5 parts of polylactic acid resin.
5. The method for preparing the organic silicon synthetic leather surface layer according to claim 1, comprising the following steps:
preparation of base adhesive A: mixing 70-80% of vinyl silicone oil A-1 with vinyl silicone oil A-2, vinyl silicone oil A-3 and other components except white carbon black uniformly, adding white carbon black, heating to 120-170 ℃ after mixing uniformly, adding the residual vinyl silicone oil A-1, and stirring uniformly to obtain base rubber A.
6. The organic silicon synthetic leather is characterized by comprising a base material, an adhesive layer arranged on the base material and a surface layer arranged on the adhesive layer, wherein the surface layer is the organic silicon synthetic leather surface layer according to any one of claims 1-4, and the adhesive layer comprises the following components in parts by mass:
base adhesive B:100 parts;
crosslinking agent: 1 to 3.5 minutes;
catalyst: 0.05-1 part;
silane coupling agent: 2-8 parts;
wherein the base adhesive B is mainly vinyl silicone oil C and at least comprises white carbon black accounting for 20-30% of the mass fraction of the base adhesive B; the viscosity of the vinyl silicone oil C is 100000 mpa.s, and the vinyl content is 0.15%.
7. The organic silicon synthetic leather according to claim 6, wherein the base adhesive B further comprises a silazane compound accounting for 5-11% of the mass fraction of the base adhesive B and hydroxyl silicone oil accounting for 0.1-1% of the mass fraction of the base adhesive B.
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