CN102040719A - Organosilicon modified water-based polyurethane resin and washing treating agent for synthetic leather - Google Patents
Organosilicon modified water-based polyurethane resin and washing treating agent for synthetic leather Download PDFInfo
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- CN102040719A CN102040719A CN 201010554508 CN201010554508A CN102040719A CN 102040719 A CN102040719 A CN 102040719A CN 201010554508 CN201010554508 CN 201010554508 CN 201010554508 A CN201010554508 A CN 201010554508A CN 102040719 A CN102040719 A CN 102040719A
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Abstract
The invention discloses an organosilicon modified water-based polyurethane resin and a washing treating agent for synthetic leather. The water-based polyurethane resin is formed by the copolymerization of ternary block co-modified siloxane, isocyanate, polyester dihydric alcohol, a chain extender, a neutralizer, a catalyst, a solvent and water; and based on the total weight of the washing treating agent, the washing treating agent is formed by mixing 30-50 parts of water-based polyurethane resin, 3-5 parts of extinction powder, 15-20 parts of polyvinyl alcohol, 1-5 parts of organosilicon leveling wetting agent, 1-3 parts of firmness enhancer, 0.1-0.5 part of defoaming agent and 20-40 parts of water. In the invention, the synthesized organosilicon modified water-based polyurethane resin is taken as a base material and other auxiliary materials are added to prepare the washing treating agent; and the washing treating agent is used for washing and treating polyurethane synthetic leather to ensure that the product has good high and low temperature resisting performance, smooth hand feel, abrasion resistance and antique style.
Description
Technical field
The present invention relates to urethane resin and washing treatment agent, particularly a kind of organosilicon modified aqueous polyurethane resin and the washing treatment agent that is used for synthetic leather.
Background technology
The washing Synthetic Leather, finished leather has style modelled after an antique, represents an important development direction of following synthetic leather industry; But aqueous treatment agent in today of countries in the world pay attention to day by day environmental protection, enjoys the concern of synthetic leather research and production department in the solvent-free discharging of production process.
Summary of the invention
The objective of the invention is: a kind of organosilicon modified aqueous polyurethane resin and the washing treatment agent that is used for synthetic leather are provided, by the organosilicon modified aqueous polyurethane resin that synthesizes is base-material, add other auxiliary material and make the washing treatment agent, the Synthetic Leather finished product high and low temperature resistance that the washing treatment agent is handled is good, feel is sliding glutinous, characteristics such as wear-resisting, and style modelled after an antique is arranged.
Technical solution of the present invention is: this organosilicon modified aqueous polyurethane resin is total to modified siloxane by the ternary block and isocyanic ester, polyester diol, chainextender, neutralizing agent, catalyzer, solvent and water are polymerized jointly; By weight, the isocyanic ester of 50-60 part, the polyester diol of 200-300 part, the ternary block of 10-20 part is modified siloxane altogether, the dibasic alcohol chainextender of 10-15 part, the amine chain extender of 1-1.5 part, 0.5 part catalyzer, 10 parts neutralizing agent, the solvent of 30-50 part, 400 parts water; Concrete steps are: with the ternary block of pure and mild 10-20 part of polyester binary of the isocyanic ester of 50-60 part, 200-300 part altogether the catalyzer of modified siloxane and 0.5 part add in the reactor, 60-90 ℃ of reaction 1-3 hour down, make base polyurethane prepolymer for use as; Then system temperature is controlled at 40 ℃ and adds solvent 30-50 part, the dibasic alcohol chainextender that in system, adds 10-15 part simultaneously, heat up and remain on 70-90 ℃ and reacted 3-4 hour, after reaction is finished, be cooled to 40 ℃ and in system, add 10 parts neutralizing agent and keep this temperature to carry out neutralization reaction 30 minutes; Again under agitation, add 400 parts water, the amine chain extender that adds 1-1.5 part after high speed dispersion was reacted 3-4 hour, desolvated and low-boiling-point substance by the decompression extrct at last, got waterborne polyurethane resin.
Wherein, the molecular structural formula of the common modified siloxane of described ternary block is:
H (OC
2H
4)
a(C
3H
6O)
bOC
3H
6[(CH
3)
2SiO]
mC
3H
6O (C
3H
6O)
b(C
2H
4O)
aR (OC
3H
6)
b(C
2H
4O)
aO-C
3H
6[(CH
3)
2SiO]
mC
3H
6O (C
3H
6O)
b(C
2H
4O)
aH; Wherein: a, b, m are positive integers, a=6～12; B=0～5; M=5～10; R is the TDI(tolylene diisocyanate), MDI(ditan-4,4, vulcabond) in a kind of; By the 1:1 reaction in molar ratio of the end capped polysiloxane of hydroxy polyethers and alkyl or aryl vulcabond and get; The end capped polysiloxane of described hydroxy polyethers is buied from marketing, the L-587 of the modest company of DS, BYK-9565; Described alkyl or aryl vulcabond is a commodity TDI(tolylene diisocyanate) or MDI(ditan-4,4, vulcabond), they are buied from market.
Wherein, described isocyanic ester is that different Fo Er vulcabond (IPDI), 1 is arranged, and 6-is a kind of in based isocyanate (HDI), two cyclohexyl methane diisocyanates (H12MDI), the tolylene diisocyanate (DTI).
Wherein, described polyester diol is to be the polyester diol of 1500-2000 with the number-average molecular weight of isocyanate reaction.
Wherein, described dibasic alcohol chainextender is 1, a kind of in 4-butyleneglycol, ethylene glycol, the propylene glycol; Described amine chain extender is a kind of in quadrol, the triethylene tetramine.
Wherein, described neutralizing agent is a kind of in triethylamine or the ammoniacal liquor.
Wherein, described catalyzer is a kind of in stannous octoate, the dibutyl tin dilaurate.
Wherein, described solvent agent is a kind of in acetone, the butanone.
A kind of washing treatment agent that is used for synthetic leather, gross weight with treatment agent is a benchmark, and the washing treatment agent is mixed by waterborne polyurethane resin 30-50 part, flatting silica 3-5 part, polyvinyl alcohol 15-20 part, organosilicon levelling wetting agent 1-5 part, fastness elevator 1-3 part, defoamer 0.1-0.5 part, water 20-40 part; Concrete steps are: in the waterborne polyurethane resin adding equipment with 30-50 part, under high-speed stirring, add the organosilicon levelling wetting agent of 1-5 part, the flatting silica of 3-5 part, the fastness elevator of 1-3 part, the polyvinyl alcohol of 15-20 part, the water of 20-40 part, the defoamer of 0.1-0.5 part, stir, making viscosity is the washing treatment agent of 6000-15000CPS.
Wherein, described organosilicon levelling wetting agent is the KY-204SE of our company or the DC-5211 of DOW CORNING; Described flatting silica specific surface area is at 200m
2More than/the g, tap density 40g/l; The polymerization degree of described polyvinyl alcohol is at 1500-2000, alcoholysis degree 80-90mol%; The deblocking temperature of described fastness elevator is more than or equal to 120 ℃, and the deblocking time was smaller or equal to 60 seconds fully.
The present invention is total to the synthetic waterborne polyurethane resin of modified siloxane with the ternary block, be that base-material makes use for synthetic leather washing treatment agent with this resin again, it is good that the Synthetic Leather finished product of handling with this treatment agent has a high and low temperature resistance, and the feel cunning is glutinous, characteristics such as wear-resisting, and style modelled after an antique is arranged.
Embodiment
Further specify technical solution of the present invention below in conjunction with specific embodiment, these embodiment can not be interpreted as it is restriction to technical scheme.Wherein embodiment 1-2 is the preparation of modified siloxane altogether of ternary block, and embodiment 3-7 is the preparation of waterborne polyurethane resin, and embodiment 8-10 is the preparation of washing treatment agent.
Embodiment 1:
In being equipped with the there-necked flask of thermometer, reflux condensing tube, agitator, 1000ml adds tolylene diisocyanate (TDI) 87g, the end capped polysiloxane of hydroxy polyethers (L-587) 770g, catalyzer (stannous octoate) 0.8g, reacted 5 hours down at 80 ℃, remove low-boiling-point substance by the decompression extracting then, obtain ternary block modified siloxane altogether.
Embodiment 2:
Be equipped with at 1000ml and add MDI(ditan-4 in the there-necked flask of thermometer, reflux condensing tube, agitator, 4, vulcabond) 125g, the end capped polysiloxane of hydroxy polyethers (BYK9565) 800g, catalyzer (stannous octoate) 0.8g, reacted 5 hours down at 80 ℃, remove low-boiling-point substance by the decompression extracting then, obtain ternary block modified siloxane altogether.
Embodiment 3:
In being equipped with the four-hole boiling flask of thermometer, reflux condensing tube, agitator, 1000ml adds tolylene diisocyanate (TDI) 50g, the ternary block of embodiment 1 is modified siloxane 20g altogether, poly-adipic acid ester hexylene glycol (Mn2000) 300g, catalyzer (dibutyl tin dilaurate) 0.5g reacted 3 hours down at 60 ℃; Temperature is controlled at 40 ℃ adds acetone 30g, add ethylene glycol 10g, reacted 4 hours down, temperature is controlled at 40 ℃ again, in system, add 10g ammoniacal liquor and carried out neutralization reaction 30 minutes at 70 ℃; Adding the 400g deionized water under the high-speed stirring in neutral performed polymer carries out emulsification and disperses, and-when nco value drops to mass content 0.8%, add the 1.5g quadrol and carry out the secondary chain extension reaction, desolvate and low-boiling-point substance by the decompression extrct at last, obtain the waterborne polyurethane resin of solid content about 48%.
Embodiment 4:
Be equipped with at 1000ml and add two cyclohexyl methane diisocyanate (H12MDI) 55g in the four-hole boiling flask of thermometer, reflux condensing tube, agitator, the ternary block of embodiment 2 is modified siloxane 10g altogether, poly-adipic acid ester ethylene glycol (Mn1500) 200g, catalyzer (stannous octoate) 0.5g reacted 2 hours down at 75 ℃; Temperature is controlled at 40 ℃ adds acetone 40g, add 1,4-butyleneglycol 12.5g reacted 3.5 hours down at 80 ℃, temperature was controlled at 40 ℃ again, adds the 10g triethylamine and carried out neutralization reaction 30 minutes in system; Adding the 400g deionized water under the high-speed stirring in neutral performed polymer carries out emulsification and disperses, and-when nco value drops to mass content 0.8%, add the 1.0g quadrol and carry out the secondary chain extension reaction, desolvate and low-boiling-point substance by the decompression extrct at last, obtain the waterborne polyurethane resin of solid content about 41%.
Embodiment 5:
Be equipped with at 1000ml and add two cyclohexyl methane diisocyanate (HDI) 60g in the four-hole boiling flask of thermometer, reflux condensing tube, agitator, the ternary block of embodiment 1 is modified siloxane 15g altogether, poly-adipic acid ester ethylene glycol (Mn1600) 250g, catalyzer (stannous octoate) 0.5g reacted 1 hour down at 90 ℃; Temperature is controlled at 40 ℃ adds butanone 40g, add propylene glycol 12.5g, reacted 3 hours down, temperature is controlled at 40 ℃ again, in system, add the 10g triethylamine and carried out neutralization reaction 30 minutes at 90 ℃; Adding the 400g deionized water under the high-speed stirring in neutral performed polymer carries out emulsification and disperses, and-when nco value drops to mass content 0.8%, add the 1.25g quadrol and carry out the secondary chain extension reaction, desolvate and low-boiling-point substance by the decompression extrct at last, obtain the waterborne polyurethane resin of the present invention of solid content about 46%.
Embodiment 6:
Be equipped with at 1000ml and add two cyclohexyl methane diisocyanate (IPDI) 50g in the four-hole boiling flask of thermometer, reflux condensing tube, agitator, the ternary block of embodiment 2 is modified siloxane 15g altogether, poly-adipic acid ester ethylene glycol (Mn1500) 200g, catalyzer (dibutyl tin dilaurate) 0.5g reacted 2.5 hours down at 70 ℃; Temperature is controlled at 40 ℃ adds acetone 50g, add 1,4-butyleneglycol 15g reacted 3.5 hours down at 80 ℃, temperature was controlled at 40 ℃ again, adds 10g ammoniacal liquor and carried out neutralization reaction 30 minutes in system; Adding the 400g deionized water under the high-speed stirring in neutral performed polymer carries out emulsification and disperses, and-when nco value drops to mass content 0.8%, add the 1.25g triethylene tetramine and carry out the secondary chain extension reaction, desolvate and low-boiling-point substance by the decompression extrct at last, obtain the waterborne polyurethane resin of the present invention of solid content 43%.
Embodiment 7:
Be equipped with at 1000ml and add two cyclohexyl methane diisocyanate (H12MDI) 60g in the four-hole boiling flask of thermometer, reflux condensing tube, agitator, the ternary block of embodiment 1 is modified siloxane 10g altogether, poly-adipic acid ester ethylene glycol (Mn1500) 250g, catalyzer (stannous octoate) 0.5g reacted 2 hours down at 80 ℃; Temperature is controlled at 40 ℃ adds butanone 30g, add ethylene glycol 12.5g, reacted 3 hours down, temperature is controlled at 40 ℃ again, in system, add the 10g triethylamine and carried out neutralization reaction 30 minutes at 90 ℃; Adding the 400g deionized water under the high-speed stirring in neutral performed polymer carries out emulsification and disperses, and-when nco value drops to mass content 0.8%, add the 1.5g triethylene tetramine and carry out the secondary chain extension reaction, desolvate and low-boiling-point substance by the decompression extrct at last, obtain the waterborne polyurethane resin of the present invention of solid content about 45%.
Embodiment 8:
Waterborne polyurethane resin with embodiment 4
50In the kg adding equipment, add the levelling wetting agent (KY-204SE) of 1kg, the flatting silica of 3kg, the fastness elevator of 1kg, the polyvinyl alcohol of 20kg, the deionized water of 30kg, the defoamer of 0.5kg under high-speed stirring, stir, getting viscosity is 15000CPS
AboutWashing treatment agent A.
Embodiment 9:
Waterborne polyurethane resin with embodiment 5
40In the kg adding equipment, under high-speed stirring, add the levelling wetting agent (KY-204SE) of 2.5kg, the flatting silica of 4kg, the fastness elevator of 2kg, the polyvinyl alcohol of 17.5kg, the deionized water of 20kg, 0.25 part defoamer, stir, getting viscosity is 12000CPS
AboutWashing treatment agent B.
Embodiment 10:
Waterborne polyurethane resin with embodiment 6
30In the kg adding equipment, the levelling wetting agent of adding 5kg under high-speed stirring (
DC-5211), the flatting silica of 5kg, the fastness elevator of 3kg, the polyvinyl alcohol of 15kg, the deionized water of 40kg, 0.1 part defoamer, stir, viscosity be 6000CPS
AboutWashing treatment agent C.
Comparative example:
Distinguish the bass surface of roller coating with commercially available excellent Nike UNKPU – 620 washing treatment agents and water conditioner of the present invention at the synthetic leather of embossing, add " 503 " aqueous black paste 20% that the dark blue company in Hangzhou produces during use in proportion, all resin solid contents transfer to 30%, 120～150 ℃ of oven dry, washing is handled on rinsing machine, and oven dry back effect is as follows:
Claims (10)
1. organosilicon modified aqueous polyurethane resin is characterized in that: modified siloxane and isocyanic ester, polyester diol, chainextender, neutralizing agent, catalyzer, solvent and water are polymerized this waterborne polyurethane resin jointly altogether by the ternary block; By weight, the isocyanic ester of 50-60 part, the polyester diol of 200-300 part, the ternary block of 10-20 part is modified siloxane altogether, the dibasic alcohol chainextender of 10-15 part, the amine chain extender of 1-1.5 part, 0.5 part catalyzer, 10 parts neutralizing agent, the solvent of 30-50 part, 400 parts water; Concrete steps are: the isocyanic ester of 50-60 part, the polyester diol of 200-300 part, the common modified siloxane of ternary block of 10-20 part and 0.5 part catalyzer are added in the reactor, reacted 1-3 hour down at 60-90 ℃, make base polyurethane prepolymer for use as; Then system temperature is controlled at 40 ℃ and adds solvent 30-50 part, the dibasic alcohol chainextender that in system, adds 10-15 part simultaneously, heat up and remain on 70-90 ℃ and reacted 3-4 hour, after reaction is finished, be cooled to 40 ℃ and in system, add 10 parts neutralizing agent and keep this temperature to carry out neutralization reaction 30 minutes; Again under agitation, add 400 parts water, the amine chain extender that adds 1-1.5 part after high speed dispersion was reacted 3-4 hour, desolvated and low-boiling-point substance by the decompression extrct at last, got waterborne polyurethane resin.
2. a kind of organosilicon modified aqueous polyurethane resin according to claim 1 is characterized in that: the described ternary block molecular structural formula of modified siloxane altogether is:
H (OC
2H
4)
a(C
3H
6O)
bOC
3H
6[(CH
3)
2SiO]
mC
3H
6O (C
3H
6O)
b(C
2H
4O)
aR (OC
3H
6)
b(C
2H
4O)
aO-C
3H
6[(CH
3)
2SiO]
mC
3H
6O (C
3H
6O)
b(C
2H
4O)
aH; Wherein: a, b, m are positive integers, a=6～12; B=0～5; M=5～15; R is the TDI(tolylene diisocyanate) or MDI(ditan-4,4, vulcabond) in a kind of; Described ternary block altogether modified siloxane be by the end capped polysiloxane of hydroxy polyethers and vulcabond in molar ratio 1:1 react and get; The end capped polysiloxane of described hydroxy polyethers is buied from marketing, the L-587 of the modest company of DS, BYK-9565; Described vulcabond is a commodity TDI(tolylene diisocyanate), MDI(ditan-4,4, vulcabond) in a kind of, they are buied from market.
3. a kind of organosilicon modified aqueous polyurethane resin according to claim 1, it is characterized in that: isocyanic ester is that different Fo Er vulcabond (IPDI), 1 is arranged, and 6-is a kind of in based isocyanate (HDI), two cyclohexyl methane diisocyanates (H12MDI), the tolylene diisocyanate (TDI).
4. a kind of organosilicon modified aqueous polyurethane resin according to claim 1 is characterized in that: described polyester diol is to be the polyester diol of 1500-2000 with the number-average molecular weight of isocyanate reaction.
5. a kind of organosilicon modified aqueous polyurethane resin according to claim 1 is characterized in that: described dibasic alcohol chainextender is 1, a kind of in 4-butyleneglycol, ethylene glycol, the propylene glycol; Described amine chain extender is a kind of in quadrol, the triethylene tetramine.
6. a kind of organosilicon modified aqueous polyurethane resin according to claim 1 is characterized in that: described neutralizing agent is a kind of in triethylamine or the ammoniacal liquor.
7. a kind of organosilicon modified aqueous polyurethane resin according to claim 1 is characterized in that: described catalyzer is a kind of in stannous octoate, the dibutyl tin dilaurate.
8. a kind of organosilicon modified aqueous polyurethane resin according to claim 1 is characterized in that: described solvent agent is a kind of in acetone, the butanone.
9. washing treatment agent that is used for synthetic leather, it is characterized in that: the gross weight with treatment agent is a benchmark, and the washing treatment agent is mixed by waterborne polyurethane resin 30-50 part, flatting silica 3-5 part, polyvinyl alcohol 15-20 part, organosilicon levelling wetting agent 1-5 part, fastness elevator 1-3 part, defoamer 0.1-0.5 part, water 20-40 part; Concrete steps are: in the waterborne polyurethane resin adding equipment with 30-50 part, under high-speed stirring, add the organosilicon levelling wetting agent of 1-5 part, the flatting silica of 3-5 part, the fastness elevator of 1-3 part, the polyvinyl alcohol of 15-20 part, the water of 20-40 part, the defoamer of 0.1-0.5 part, stir, making viscosity is the washing treatment agent of 6000-15000CPS.
10. a kind of washing treatment agent that is used for synthetic leather according to claim 9 is characterized in that: described organosilicon levelling wetting agent is the KY-204SE of our company or the DC-5211 of DOW CORNING; Described flatting silica specific surface area is at 200m
2More than/the g, tap density 40g/l; The polymerization degree of described polyvinyl alcohol is at 1500-2000, alcoholysis degree 80-90mol%; The deblocking temperature of described fastness elevator is more than or equal to 120 ℃, and the deblocking time was smaller or equal to 60 seconds fully.
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| CN102953270A (en) * | 2012-11-05 | 2013-03-06 | 淮安凯悦科技开发有限公司 | Convex pattern liquid crystal surface synthetic leather manufacturing method |
| CN103205894A (en) * | 2013-04-02 | 2013-07-17 | 嘉兴禾大科技化学有限公司 | Finished and brightened polyurethane leather surface treatment agent with real-feather feel and preparation method thereof |
| CN103306138A (en) * | 2013-06-26 | 2013-09-18 | 江苏宝泽高分子材料股份有限公司 | Water-kneading pressure change resin for synthetic leather and preparing method of resin |
| CN104131466A (en) * | 2014-07-22 | 2014-11-05 | 嘉兴禾大科技化学有限公司 | Velvet feeling polyurethane leather surface conditioning agent and preparation method thereof |
| CN104726021A (en) * | 2013-12-22 | 2015-06-24 | 瓦克化学（中国）有限公司 | Modified resin water-based dispersion liquid |
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| CN104131466A (en) * | 2014-07-22 | 2014-11-05 | 嘉兴禾大科技化学有限公司 | Velvet feeling polyurethane leather surface conditioning agent and preparation method thereof |
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Application publication date: 20110504 |