CN102604026B - Preparation method organic silicon-modified polyurethane resin for synthetic leather - Google Patents
Preparation method organic silicon-modified polyurethane resin for synthetic leather Download PDFInfo
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Abstract
The invention designs organic silicon-modified polyurethane resin for synthetic leather and a preparation method thereof, which relates to the field of processing of the synthetic leather and aims at solving the technical problems of poor anti-sticking property, water resistance, wear resistance and other properties of the existing synthetic leather. The organic silicon-modified polyurethane resin disclosed by the invention is characterized by comprising the following raw material ingredients in percentage by weight: 2%-30% of diisocyanate, 5%-40% of polyester or polyether type polylol, 0.5%-20% of hydroxyl-terminated organic silicon, 0%-10% of small molecular polylol chain extender, 0%-13% of small molecular polyamine chain extender, 0.01%-1% of catalyst and the balance of solvent, wherein the hydroxyl-terminated organic silicon adopts a polyether-polysiloxane copolymer with two ends which are of hydroxyl groups, and a polyether chain segment is of polyoxyethylene or polyoxypropylene. The glossiness and transparency of the polyurethane resin after modification can not be affected by the organic silicon, and the anti-sticking property, surface smoothness, wear resistance and water resistance are obviously improved simultaneously.
Description
Technical field
The present invention relates to the synthetic leather manufacture field, especially the preparation method of use for synthetic leather organic silicon modified polyurethane resin.
Background technology
When urethane resin is applied to synthetic leather dry method surface layer or face finish, can add the feel that organic silicon additive improves product usually, improve the performance such as antiseized, water-fast, wear-resisting of product.The mode of adding generally is that organosilyl auxiliary agent is added in the urethane resin by the mode of physical mixed, because the consistency between organosilicon and the urethane resin is relatively poor, the addition manner that simple physics is mixed can cause organosilicon to be separated out, cause that product surface is fuel-displaced, in addition, urethane resin and silicone resin consistency be not good also can to cause the film of resin to turn white, degradation side effect under the gloss, influence the outward appearance of product, and along with the increase of organosilicon addition, this side effect is more and more obvious.
Summary of the invention
The objective of the invention is to provide in order to solve above-mentioned the deficiencies in the prior art a kind of preparation method of use for synthetic leather organic silicon modified polyurethane resin, method by chemosynthesis is introduced organosilicon on the molecular chain of urethane, improve the consistency of organosilicon and urethane resin, make that product appearance is transparent, glossiness is high.
In order to achieve the above object, the use for synthetic leather organic silicon modified polyurethane resin that the present invention is designed, it is characterized in that its raw materials used composition and quality percentage composition are as follows: vulcabond 2%-30%, polyester or polyether alcohol 5%-40%, terminal hydroxy group organosilicon 0.5%-20%, small molecules polyvalent alcohol chainextender 0%-10%, small molecules polyamine chainextender 0%-13%, catalyzer 0.01%-1%, all the other are solvent, it is the polyether-polysiloxane copolymers of hydroxyl that described terminal hydroxy group organosilicon adopts two ends, and polyether segment is polyoxyethylene or polyoxypropylene.The present invention contains organosilyl segment by the copolymerization on the urethane segment of the chemical reaction between the hydroxyl in the terminal hydroxy group organosilicon and the NCO base, can make urethane and organosilicon reach the molecule level mixture, the glossiness of the urethane resin after the modification and transparency can not be subjected to organosilyl influence.Organic silicon modified polyurethane resin of the present invention is compared with common aliphatic polyurethane resin simultaneously, on anti-adhesion performance, surperficial smooth degree and wear-resisting, water resistance, all be significantly improved, be particularly suitable for high performance Synthetic Leather and synthetic leather face finish.Because common polysiloxane and urethane consistency is relatively poor, even be linked on the polyurethane chain by chemical process, also can cause modified polyurethane gloss poor transparency owing to the problem of consistency, even gel occurs and cause resin to use.The polyether-polysiloxane copolymers that the present invention adopts is compared common polysiloxane, because the existence of polyether segment wherein, improved the consistency of itself and urethane resin, the modified polyurethane that obtains can not occur because of the not good variety of issue that causes of consistency.Adopt method of the present invention to carry out modification to the urethane resin that comprises aliphatics, aromatic any kind of, the scope of application is very extensive.The present invention substitutes the organosilicon of terminal hydroxy group polyester or polyether glycol and the di-isocyanate reaction of part, organosilyl materials are unrestricted, even can substitute most polyester or polyether glycol use, therefore organosilicon can be accomplished very high content in the modified polyurethane that obtains, and the highlyest can reach 20%.
The preparation method of this organic silicon modified polyurethane resin is as follows:
(1) polyester or polyether alkylol cpd were carried out vacuum hydro-extraction dry 50-70 minute under 90-110 ℃;
(2) add solvent, the terminal hydroxy group organosilicon of solvent total amount 40-75% in the reactor, the vulcabond of 70%-95%, catalyzer, small molecules polyvalent alcohol chainextender fully stir, and at 60-90 ℃ of reaction 2-4h down, generate the lower performed polymer of molecular weight;
(3) add the solvent of solvent total amount 20-40% in the reactor, add vulcabond in batches and carry out chain extending reaction, the 0.5-1h at interval that at every turn feeds intake, temperature of reaction 60-90 ℃, along with the adding of vulcabond, the performed polymer molecular weight increases gradually;
(4) when system viscosity reaches 300cps/25 ℃-300000cps/25 ℃, stop chain extending reaction, cooling adds remaining solvent;
(5) cooling.
Improve and replenish as the further of said structure, the present invention also comprises the arbitrary combination of following additional technical feature or these features:
Described terminal hydroxy group organosilicon is that two ends are the polyether-polysiloxane copolymers of hydroxyl, and polyether segment can be polyoxyethylene or polyoxypropylene, its molecular structure (molecular weight is below 6000) as follows:
Or
Described diisocyanate cpd is a kind of or arbitrary combination of following compound: diphenylmethanediisocyanate, tolylene diisocyanate, isophorone diisocyanate, hexamethylene diisocyanate, two cyclohexyl methane diisocyanates.
Described small molecules polyvalent alcohol chainextender is a kind of or arbitrary combination of following compound: ethylene glycol, Diethylene Glycol, 1,2-propylene glycol, 1,4-butyleneglycol, 1,6-hexylene glycol, neopentyl glycol, trimethylolpropane tris alcohol.
Described small molecules polyamine chainextender is the mixture of different Buddhist diketone diamines or quadrol or said two devices.
Described catalyzer is organic tin catalyzer or organo-bismuth class catalyzer or the above two mixture.
Described organic tin catalyzer is stannous octoate or dibutyl tin laurate or the above two mixture.
Described solvent is a kind of or arbitrary combination of following compound: N, dinethylformamide, N,N-dimethylacetamide, butanone, acetone, toluene, dimethylbenzene, ethyl acetate, butylacetate, ethylene glycol monomethyl ether, propylene glycol monomethyl ether, methyl alcohol, ethanol, Virahol, propyl carbinol, isopropylcarbinol.
Described polyester or polyether glycol are a kind of or arbitrary combination of following compound: polyoxypropyleneglycol, polytetrahydrofuran diol, polycaprolactone glycol, polycarbonate diol, the polyethylene glycol adipate glycol, the polydiethylene glycol adipate glycol, the poly adipate succinic acid ester glycol, the polypropylene adipate (PPA) glycol, poly-hexanodioic acid hexylene glycol esterdiol, the polyneopentyl glycol adipate glycol, poly-adipate glycol-Diethylene Glycol esterdiol, polyester or the polyether Glycols of poly-adipate glycol-butanediol ester glycol and other specific types.
The polyester that the present invention uses or polyether polyols molecular weight between 400～12000g/mol, preferably between 1000～3000.The viscosity of described organic silicon modified polyurethane resin is between 300cps～300000cps.
The present invention contains organosilyl segment by the copolymerization on the urethane segment of the chemical reaction between the hydroxyl in the terminal hydroxy group organosilicon and the NCO base, can make urethane and organosilicon reach the molecule level mixture, the glossiness of the urethane resin after the modification and transparency can not be subjected to organosilyl influence.Organic silicon modified polyurethane resin of the present invention is compared with common aliphatic polyurethane resin simultaneously, on anti-adhesion performance, surperficial smooth degree and wear-resisting, water resistance, all be significantly improved, be particularly suitable for high performance Synthetic Leather and synthetic leather face finish; Improved the consistency of itself and urethane resin, the not good variety of issue that causes of consistency of common polysiloxane-modified appearance can not appear in the modified polyurethane that obtains.
Embodiment
The present invention is further described by the following embodiment.
Example one
With 139.5 parts of polycarbonate diols (molecular weight 2000), be warmed up to 100 ℃, the about 1h of vacuum hydro-extraction cools to 50 ℃, adds 400 parts of DMF, 30 parts of polyether-polysiloxanes, 7.9 part 1 in the reactor, and 4-butyleneglycol, 6.3 parts of ethylene glycol stir; Add 21.2 parts of TDI, 35 parts of MDI, 0.5 part of dibutyl tin laurate stirs, and is warmed up to 75 ℃, the reaction 3.5h; Add 250 parts of TOL in reactor, keep 75 ℃ of temperature, the MDI tackify with 9.6 parts feeds intake once every 45min, each charging capacity 0.5-3 part; After treating that viscosity reaches preset value, cool to 60 ℃, add 100 parts of butanone and stir, continue to be cooled to 30 ℃, discharging.Obtaining solid content is 25%, and viscosity is 20000cps/25 ℃, and 100% modulus is 80kgf/cm
2The organic silicon modified polyurethane resin.
Organic-silicon-modified urethane resin and similar prescription are not contrasted the variation of non-stick property, water tolerance and wear resistance respectively through the urethane resin of modification; The method of test is as follows:
Non-stick property: urethane resin is diluted to 20% solid content with DMF after, roller coat and dry-method chemical leather surface, 150 ℃ of baking 5min.Then synthetic leather is fitted face-to-face, in 100 ℃ of baking ovens, placed 1 hour under the pressure of 3kg, take out the adhesion situation that binding face is observed in the cooling back, the progression evaluation criteria is with reference to subordinate list one.
Water tolerance: urethane resin is made the film that thickness is about 1mm at the tetrafluoroethylene plate, and the deionized water of putting into 25 ℃ fully after the oven dry soaks 24h, investigates the variation of film total amount before and after soaking.
Wear resistance: after urethane resin made synthetic leather dry method sample, the number of turns that galls with the test of H22 emery wheel at TABER friction testing instrument.
The modified polyurethane resin that example one is obtained and similar prescription do not compare test through organic-silicon-modified polyether-polyurethane resin according to above-mentioned method, the result is as follows:
| ? | Anti-adhesion performance | Water resistance | Wear resisting property |
| Example one modification resin | 5 grades | 1.2% | 800 change |
| Unmodified resin | 5 grades | 2.8% | 300 change |
This example adopts polycarbonate diol to be synthetic raw material, and the synthetic urethane resin of polycarbonate diol is generally used for wear resisting property is had the occasion of requirement, and through organic-silicon-modified, the wear resisting property of urethane resin is more than doubled.
Claims (7)
1. the preparation method of use for synthetic leather organic silicon modified polyurethane resin, it is characterized in that its raw materials used composition and quality percentage composition are as follows: vulcabond 2%-30%, polyester or polyether alcohol 5%-40%, terminal hydroxy group organosilicon 0.5%-20%, small molecules polyvalent alcohol chainextender 0%-10%, small molecules polyamine chainextender 0%-13%, catalyzer 0.01%-1%, all the other are solvent, it is the polyether-polysiloxane copolymers of hydroxyl that described terminal hydroxy group organosilicon adopts two ends, and polyether segment is polyoxyethylene or polyoxypropylene; The preparation method of this organic silicon modified polyurethane resin is as follows:
(1) polyester or polyether alkylol cpd were carried out vacuum hydro-extraction dry 50-70 minute under 90-110 ℃;
(2) add solvent, the terminal hydroxy group organosilicon of solvent total amount 40-75% in the reactor, the vulcabond of 70%-95%, catalyzer, small molecules polyvalent alcohol chainextender fully stir, and at 60-90 ℃ of reaction 2-4h down, generate the lower performed polymer of molecular weight;
(3) add the solvent of solvent total amount 20-40% in the reactor, add vulcabond in batches and carry out chain extending reaction, the 0.5-1h at interval that at every turn feeds intake, temperature of reaction 60-90 ℃, along with the adding of vulcabond, the performed polymer molecular weight increases gradually;
(4) when system viscosity reaches 300cps/25 ℃-300000cps/25 ℃, stop chain extending reaction, cooling adds remaining solvent;
(5) cooling.
2. the preparation method of use for synthetic leather organic silicon modified polyurethane resin according to claim 1 is characterized in that described diisocyanate cpd is a kind of or arbitrary combination of following compound: diphenylmethanediisocyanate, tolylene diisocyanate, isophorone diisocyanate, hexamethylene diisocyanate, dicyclohexyl methane diisocyanate.
3. the preparation method of use for synthetic leather organic silicon modified polyurethane resin according to claim 1, it is characterized in that described small molecules polyvalent alcohol chainextender is a kind of or arbitrary combination of following compound: ethylene glycol, Diethylene Glycol, 1,2-propylene glycol, 1,4-butyleneglycol, 1,6-hexylene glycol, neopentyl glycol, trimethylolpropane tris alcohol.
4. the preparation method of use for synthetic leather organic silicon modified polyurethane resin according to claim 1 is characterized in that described small molecules polyamine chainextender is the mixture of different Buddhist diketone diamines or quadrol or said two devices.
5. the preparation method of use for synthetic leather organic silicon modified polyurethane resin according to claim 1 is characterized in that described catalyzer is organic tin catalyzer or organo-bismuth class catalyzer or the above two mixture.
6. the preparation method of use for synthetic leather organic silicon modified polyurethane resin according to claim 5 is characterized in that described organic tin catalyzer is stannous octoate or dibutyl tin laurate or the above two mixture.
7. the preparation method of use for synthetic leather organic silicon modified polyurethane resin according to claim 1, it is characterized in that described solvent is a kind of or arbitrary combination of following compound: N, dinethylformamide, N,N-dimethylacetamide, butanone, acetone, toluene, dimethylbenzene, ethyl acetate, butylacetate, ethylene glycol monomethyl ether, propylene glycol monomethyl ether, methyl alcohol, ethanol, Virahol, propyl carbinol, isopropylcarbinol.
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