CN104650577A - High-frequency-attached high-water-pressure-resistance polyurethane resin for leather and method for producing high-frequency-attached high-water-pressure-resistance polyurethane resin for leather - Google Patents
High-frequency-attached high-water-pressure-resistance polyurethane resin for leather and method for producing high-frequency-attached high-water-pressure-resistance polyurethane resin for leather Download PDFInfo
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- CN104650577A CN104650577A CN201510058801.8A CN201510058801A CN104650577A CN 104650577 A CN104650577 A CN 104650577A CN 201510058801 A CN201510058801 A CN 201510058801A CN 104650577 A CN104650577 A CN 104650577A
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Abstract
The invention relates to a high-frequency-attached high-water-pressure-resistance polyurethane resin for leather and a method for producing the high-frequency-attached high-water-pressure-resistance polyurethane resin for the leather. The method for producing the high-frequency-attached high-water-pressure-resistance polyurethane resin for the leather have the characteristics of heating a polyol compound in a drying chamber or an oven into liquid with the moisture content of smaller than 0.03%; sequentially adding 15-20% of a solvent, 10-15% of polyol compound, 1-5% of a diol chain extender and 0.01-1.0% of a catalyst in a reaction kettle and fully mixing by controlling the temperature of 30-60 DEG C; reacting for 1-2 hours by controlling the temperature of the reaction system of 70-80 DEG C and the viscosity of 100000-200000 cps/25 DEG C after 3-7% of isocyanate is added in the reaction kettle; carrying out heat preservation for 1-2 hours by controlling the temperature of the reaction system of 70-80 DEG C; and finally adjusting the viscosity by adding the remaining isocyanate, the remaining solvent and 0.0-2.0% of additive to 50000-200000 cps/25 DEG C. The high-frequency-attached high-water-pressure-resistance polyurethane resin for leather and the method for producing the high-frequency-attached high-water-pressure-resistance polyurethane resin for the leather have the advantages of meeting the standards of export to European Union, greatly reducing the output power, attachment temperature, attachment pressure and attachment time of high frequency attachment and meeting the requirements for water pressure resistance.
Description
Technical field
The present invention relates to a kind of clothing leather, protection rain coat, tent etc. of being applied to and need to carry out seamless applying leather products, particularly relate to a kind of leather high frequency and to fit high water pressure resistance urethane resin and production method thereof.
Background technology
At present, leather in order to improve crystallinity and the intensity of resin, employs the water-resisting agent of fluorine element with high water pressure resistance urethane; But while raising Resin crystallization, also improve softening temperature and the resistance toheat of resin.Therefore, when carrying out high frequency laminating, needing higher output rating, binding temperature, laminate pressure and laminating time, reducing production efficiency, increasing energy consumption.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art and provide a kind of while raising water pressure resistance function and strength, also can at lower high frequency, temperature, pressure, carry out high frequency laminating under the laminating time, the leather high frequency making leather have Waterproof Breathable function is fitted high water pressure resistance urethane resin and production method thereof.
In order to achieve the above object, leather high frequency of the present invention high water pressure resistance urethane resin of fitting realizes like this, it is characterized in that comprising the isocyanic ester of 6-11%, the polyol compound of 10-15%, the molecular weight of 2.0-11% be less than 150 glycol chain extender, the catalyzer of 0.0-1.0%, the solvent of 62-80% and 0.0-2.0% auxiliary agent, they are weight percentage.
Described isocyanic ester is tolylene diisocyanate or 4,4 '-diphenylmethanediisocyanate or liquefied mdi.
Described polyol compound is one or both mixture of polyester polyol or polyether glycol; Described polyester polyol is one or more the mixture in polycaprolactone polyol or poly-hexanodioic acid polyvalent alcohol, and number-average molecular weight is 1000-3000g/mol; Described polyether glycol is polyoxypropyleneglycol or polyoxyethylene glycol or polytetramethylene ether dibasic alcohol, and number-average molecular weight is 500-3000g/mol.
Described molecular weight be less than 150 glycol chain extender be one or more mixture in ethylene glycol or propylene glycol or BDO or 1,6-hexylene glycol or neopentyl glycol or dimethylol propionic acid or TriMethylolPropane(TMP).
Described solvent is one or more the mixture in dimethyl formamide or butanone or toluene or vinyl acetic monomer.
Described auxiliary agent comprise the oxidation inhibitor of 8-18%, the flow agent of 25-30%, the defoamer of 25-40% and 25-40% without fluoro water proofing agent; Described oxidation inhibitor comprises Hinered phenols and the 30-70% phosphite ester kind antioxidant of 30-70%; Described flow agent, defoamer are organic silicon modified by polyether, and they are weight percentage.
In order to achieve the above object, the fit production method of high water pressure resistance urethane resin of a kind of leather high frequency of the present invention is achieved in that and it is characterized in that comprising the steps preparation:
A, polyol compound put into drying room or baking oven for heating becomes liquid, and use water removal device to carry out drying to dewater, make its water ratio be less than 0.03%;
B, to be added by the catalyzer of the polyol compound of the solvent of 15-20%, 10-15%, the glycol chain extender of 1-5% and 0.0-1.0% in reactor and fully stir successively, the temperature controlled during stirring is 30-60 DEG C;
C, add in the reactor of step b by the isocyanic ester of 3-7%, the temperature controlling reaction system is 70-80 DEG C, and the reaction times is 1-2 hour, controls viscosity 100000-200000cps/25 DEG C;
D, add the remaining glycol chain extender of part and the solvent of 15-20%, stir, and cool to 50-60 DEG C;
E, add the isocyanic ester of 3-4%, control temperature of reaction system at 70-80 DEG C, insulation 1-2 hour;
F, according to system viscosity height situation, add the auxiliary agent adjusting viscosity of remaining isocyanic ester, remaining solvent and 0.0-2.0%, and the most at last viscosity controller at 50000-200000cps/25 DEG C.
The present invention's advantage is compared with prior art: meet European Union's export standard, greatly reduce the output rating of high frequency laminating, binding temperature, laminate pressure and laminating time, its water pressure resistance can reach requirement, make the performance of leather products obtain very large breakthrough, improve leather finish production efficiency, reduce production power consumption, ensure production safety.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is described further.It should be noted that at this, the explanation for these embodiments understands the present invention for helping, but does not form limitation of the invention.In addition, if below in described each embodiment of the present invention involved technical characteristic do not form conflict each other and just can be combined with each other.
embodiment one
It is that a kind of leather high frequency is fitted high water pressure resistance urethane resin, comprise the isocyanic ester of 11%, the polyol compound of 10%, the molecular weight of 6% be less than 150 glycol chain extender, the catalyzer of 1.0%, the solvent of 70% and 2.0% auxiliary agent, they are weight percentage.
Its production method comprises the steps preparation:
A, polyol compound put into drying room or baking oven for heating becomes liquid, and use water removal device to carry out drying to dewater, make its water ratio be less than 0.03%;
B, successively by the solvent of 15%, 10% polyol compound (polyol compound that water ratio is less than 0.03%), the glycol chain extender of 5% and the catalyzer of 1.0% to add in reactor and fully to stir, the temperature controlled during stirring is 30 DEG C;
C, add in the reactor of step b by the isocyanic ester of 4%, the temperature controlling reaction system is 75 DEG C, and the reaction times is 1.5 hours, controls viscosity 100000cps/25 DEG C;
D, the glycol chain extender of 1% adding remaining part and the solvent of 15%, stir, and cool to 50 DEG C;
E, add 6% isocyanic ester, control temperature of reaction system at 75 DEG C, be incubated 1.5 hours;
F, according to system viscosity height situation, add the remaining isocyanic ester of 1%, the solvent of remaining 30% and 2.0% auxiliary agent adjusting viscosity, and the most at last viscosity controller at 100000cps/25 DEG C.
In the present embodiment, described isocyanic ester is tolylene diisocyanate, and described polyol compound is the mixture of polycaprolactone polyol and poly-hexanodioic acid polyvalent alcohol, and number-average molecular weight is 2000g/mol; Described glycol chain extender is ethylene glycol; Described catalyzer is organic bismuth catalyst; Described solvent is dimethyl formamide; Described every part of auxiliary agent comprise 10% oxidation inhibitor, the flow agent of 25%, the defoamer of 40% and 25% without fluoro water proofing agent; Described every part of oxidation inhibitor comprises Hinered phenols and 70% phosphite ester kind antioxidant of 30%; Described flow agent, defoamer are organic silicon modified by polyether.
embodiment two
It is that a kind of leather high frequency is fitted high water pressure resistance urethane resin, comprise the isocyanic ester of 8%, the polyol compound of 15%, the molecular weight of 2% be less than 150 glycol chain extender, the catalyzer of 0.5%, the solvent of 74% and 0.5% auxiliary agent, they are weight percentage.
Its production method comprises the steps preparation:
A, polyol compound put into drying room or baking oven for heating becomes liquid, and use water removal device to carry out drying to dewater, make its water ratio be less than 0.03%;
B, successively by the solvent of 20%, 15% polyol compound (polyol compound that water ratio is less than 0.03%), the glycol chain extender of 1.5% and the catalyzer of 0.5% to add in reactor and fully to stir, the temperature controlled during stirring is 45 DEG C;
C, add in the reactor of step b by the isocyanic ester of 3%, the temperature controlling reaction system is 70 DEG C, and the reaction times is 2 hours, controls viscosity 150000cps/25 DEG C;
D, the glycol chain extender of 0.5% adding remaining part and the solvent of 20%, stir, and cool to 55 DEG C;
E, add 4% isocyanic ester, control temperature of reaction system at 70 DEG C, be incubated 2 hours;
F, according to system viscosity height situation, add the remaining isocyanic ester of 1%, the solvent of remaining 34% and 0.5% auxiliary agent adjusting viscosity, and the most at last viscosity controller at 50000cps/25 DEG C.
In the present embodiment, described isocyanic ester is 4,4 '-diphenylmethanediisocyanate; Described polyol compound is polyoxypropyleneglycol, and number-average molecular weight is 3000g/mol; Described glycol chain extender is the mixture of propylene glycol and BDO; Described catalyzer is organic bismuth catalyst; Described solvent is the mixture of butanone and toluene; Described every part of auxiliary agent comprise 18% oxidation inhibitor, the flow agent of 30%, the defoamer of 25% and 27% without fluoro water proofing agent; Described every part of oxidation inhibitor comprises Hinered phenols and 30% phosphite ester kind antioxidant of 70%; Described flow agent, defoamer are organic silicon modified by polyether.
embodiment three
It is that a kind of leather high frequency is fitted high water pressure resistance urethane resin, and comprise the isocyanic ester of 6%, the polyol compound of 12%, the molecular weight of 11% be the glycol chain extender of less than 150 and the solvent of 71%, they are weight percentage.
Its production method comprises the steps preparation:
A, polyol compound put into drying room or baking oven for heating becomes liquid, and use water removal device to carry out drying to dewater, make its water ratio be less than 0.03%;
B, the solvent of 16%, the polyol compound (polyol compound that water ratio is less than 0.03%) of 12% and the glycol chain extender of 9% to be added in reactor and fully stir successively, the temperature controlled during stirring is 60 DEG C;
C, add in the reactor of step b by the isocyanic ester of 2%, the temperature controlling reaction system is 80 DEG C, and the reaction times is 1 hour, controls viscosity 200000cps/25 DEG C;
D, the glycol chain extender of 2% adding remaining part and the solvent of 18%, stir, and cool to 60 DEG C;
E, add 3% isocyanic ester, control temperature of reaction system at 80 DEG C, be incubated 1 hour;
F, according to system viscosity height situation, add the remaining isocyanic ester of 1% and the solvent adjustment viscosity of remaining 37%, and the most at last viscosity controller at 200000cps/25 DEG C.
In the present embodiment, described isocyanic ester is liquefied mdi; Described polyol compound is the mixture of poly-hexanodioic acid polyvalent alcohol and polyoxyethylene glycol, and number-average molecular weight is 1000g/mol; Described glycol chain extender is neopentyl glycol; Described solvent is vinyl acetic monomer; Described every part of auxiliary agent comprise 13% oxidation inhibitor, the flow agent of 27%, the defoamer of 30% and 30% without fluoro water proofing agent; Described every part of oxidation inhibitor comprises Hinered phenols and 50% phosphite ester kind antioxidant of 50%; Described flow agent, defoamer are organic silicon modified by polyether.
embodiment four
It is that a kind of leather high frequency is fitted high water pressure resistance urethane resin, comprise the isocyanic ester of 9%, the polyol compound of 13%, the molecular weight of 7% be the glycol chain extender of less than 150, the catalyzer of 1% and 70% solvent, they are weight percentage.
Its production method comprises the steps preparation:
A, polyol compound put into drying room or baking oven for heating becomes liquid, and use water removal device to carry out drying to dewater, make its water ratio be less than 0.03%;
B, successively by the solvent of 18%, 13% polyol compound (polyol compound that water ratio is less than 0.03%), the glycol chain extender of 5% and the catalyzer of 1% to add in reactor and fully to stir, the temperature controlled during stirring is 45 DEG C;
C, add in the reactor of step b by the isocyanic ester of 4%, the temperature controlling reaction system is 65 DEG C, and the reaction times is 2 hours, controls viscosity 200000cps/25 DEG C;
D, the glycol chain extender of 2% adding remaining part and the solvent of 20%, stir, and cool to 60 DEG C;
E, add 3% isocyanic ester, control temperature of reaction system at 70 DEG C, be incubated 2 hours;
F, according to system viscosity height situation, add the remaining isocyanic ester of 2% and the solvent adjustment viscosity of remaining 32%, and the most at last viscosity controller at 200000cps/25 DEG C.
In the present embodiment, described isocyanic ester is tolylene diisocyanate; Described polyol compound is the mixture of polycaprolactone polyol and polytetramethylene ether dibasic alcohol, and number-average molecular weight is 2000g/mol; The mixture of described dimethylol propionic acid or TriMethylolPropane(TMP); Described catalyzer is organic bismuth catalyst; Described solvent is the mixture of toluene or vinyl acetic monomer; Described every part of auxiliary agent comprise 13% oxidation inhibitor, the flow agent of 25%, the defoamer of 32% and 32% without fluoro water proofing agent; Described every part of oxidation inhibitor comprises Hinered phenols and 40% phosphite ester kind antioxidant of 60%; Described flow agent, defoamer are organic silicon modified by polyether.
embodiment five
It is that a kind of leather high frequency is fitted high water pressure resistance urethane resin, comprise the isocyanic ester of 10%, the polyol compound of 12%, the molecular weight of 5% be the glycol chain extender of less than 150, the solvent of 72% and 1% auxiliary agent, they are weight percentage.
Its production method comprises the steps preparation:
A, polyol compound put into drying room or baking oven for heating becomes liquid, and use water removal device to carry out drying to dewater, make its water ratio be less than 0.03%;
B, the solvent of 20%, the polyol compound (polyol compound that water ratio is less than 0.03%) of 12% and the glycol chain extender of 4% to be added in reactor and fully stir successively, the temperature controlled during stirring is 50 DEG C;
C, add in the reactor of step b by the isocyanic ester of 7%, the temperature controlling reaction system is 80 DEG C, and the reaction times is 1 hour, controls viscosity 150000cps/25 DEG C;
D, the glycol chain extender of 1% adding remaining part and the solvent of 20%, stir, and cool to 60 DEG C;
E, add 2% isocyanic ester, control temperature of reaction system at 70 DEG C, be incubated 2 hours;
F, according to system viscosity height situation, add the remaining isocyanic ester of 1%, the solvent of remaining 32% and 1% auxiliary agent adjusting viscosity, and the most at last viscosity controller at 50000cps/25 DEG C.
In the present embodiment, described isocyanic ester is 4,4 '-diphenylmethanediisocyanate; Described polyol compound is polyoxypropyleneglycol, and number-average molecular weight is 3000g/mol; Described glycol chain extender is the mixture of propylene glycol and BDO; Described catalyzer is organic bismuth catalyst; Described solvent is the mixture of butanone and toluene; Described every part of auxiliary agent comprise 18% oxidation inhibitor, the flow agent of 30%, the defoamer of 25% and 27% without fluoro water proofing agent; Described every part of oxidation inhibitor comprises Hinered phenols and 30% phosphite ester kind antioxidant of 70%; Described flow agent, defoamer are organic silicon modified by polyether.
In the technical scheme of above-described embodiment, described polyol compound is one or both mixture of polyester polyol or polyether glycol; Described polyester polyol is one or more the mixture in polycaprolactone polyol or poly-hexanodioic acid polyvalent alcohol, and number-average molecular weight is 1000 ~ 3000g/mol; Described polyether glycol is polyoxypropyleneglycol or polyoxyethylene glycol or polytetramethylene ether dibasic alcohol, and number-average molecular weight is 500 ~ 3000g/mol.Described molecular weight be less than 150 glycol chain extender be one or more mixture in ethylene glycol or propylene glycol or BDO or 1,6-hexylene glycol or neopentyl glycol or dimethylol propionic acid or TriMethylolPropane(TMP).Described solvent is one or more the mixture in dimethyl formamide or butanone or toluene or vinyl acetic monomer.Described auxiliary agent comprise the oxidation inhibitor of 8-18%, the flow agent of 25-30%, the defoamer of 25-40% and 25-40% without fluoro water proofing agent; Described oxidation inhibitor comprises Hinered phenols and the 30-70% phosphite ester kind antioxidant of 30-70%; Described flow agent, defoamer are organic silicon modified by polyether.
Below detailed description is made to embodiments of the present invention, but the present invention is not limited to described embodiment in conjunction with the embodiments.For the ordinary skill in the art, carry out multiple change, amendment, replacement and distortion when not departing from principle of the present invention and aim to these embodiments still to fall within protection scope of the present invention.
Claims (7)
1. a leather high frequency is fitted high water pressure resistance urethane resin, it is characterized in that comprising the isocyanic ester of 6-11%, the polyol compound of 10-15%, the molecular weight of 2.0-11% be less than 150 glycol chain extender, the catalyzer of 0.0-1.0%, the solvent of 62-80% and 0.0-2.0% auxiliary agent, they are weight percentage.
2. leather high frequency according to claim 1 is fitted high water pressure resistance urethane resin, it is characterized in that described isocyanic ester is tolylene diisocyanate or 4,4 '-diphenylmethanediisocyanate or liquefied mdi.
3. leather high frequency according to claim 1 is fitted high water pressure resistance urethane resin, it is characterized in that described polyol compound is one or both mixture of polyester polyol or polyether glycol; Described polyester polyol is one or more the mixture in polycaprolactone polyol or poly-hexanodioic acid polyvalent alcohol, and number-average molecular weight is 1000-3000g/mol; Described polyether glycol is polyoxypropyleneglycol or polyoxyethylene glycol or polytetramethylene ether dibasic alcohol, and number-average molecular weight is 500-3000g/mol.
4. leather high frequency according to claim 1 is fitted high water pressure resistance urethane resin, it is characterized in that described molecular weight be less than 150 glycol chain extender be ethylene glycol or propylene glycol or 1, one or more mixture in 4-butyleneglycol or 1,6-hexylene glycol or neopentyl glycol or dimethylol propionic acid or TriMethylolPropane(TMP).
5. leather high frequency according to claim 1 is fitted high water pressure resistance urethane resin, it is characterized in that described solvent is one or more the mixture in dimethyl formamide or butanone or toluene or vinyl acetic monomer.
6. leather high frequency according to claim 1 is fitted high water pressure resistance urethane resin, it is characterized in that described auxiliary agent comprise the oxidation inhibitor of 8-18%, the flow agent of 25-30%, the defoamer of 25-40% and 25-40% without fluoro water proofing agent; Described oxidation inhibitor comprises Hinered phenols and the 30-70% phosphite ester kind antioxidant of 30-70%; Described flow agent, defoamer are organic silicon modified by polyether, and they are weight percentage.
7. leather high frequency is fitted a production method for high water pressure resistance urethane resin, it is characterized in that comprising the steps preparation:
A, polyol compound put into drying room or baking oven for heating becomes liquid, and use water removal device to carry out drying to dewater, make its water ratio be less than 0.03%;
B, to be added by the catalyzer of the polyol compound of the solvent of 15-20%, 10-15%, the glycol chain extender of 1-5% and 0.0-1.0% in reactor and fully stir successively, the temperature controlled during stirring is 30-60 DEG C;
C, add in the reactor of step b by the isocyanic ester of 3-7%, the temperature controlling reaction system is 70-80 DEG C, and the reaction times is 1-2 hour, controls viscosity 100000-200000cps/25 DEG C;
D, add the remaining glycol chain extender of part and the solvent of 15-20%, stir, and cool to 50-60 DEG C;
E, add the isocyanic ester of 3-4%, control temperature of reaction system at 70-80 DEG C, insulation 1-2 hour;
F, according to system viscosity height situation, add the auxiliary agent adjusting viscosity of remaining isocyanic ester, remaining solvent and 0.0-2.0%, and the most at last viscosity controller at 50000-200000cps/25 DEG C.
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| CN201510058801.8A CN104650577A (en) | 2015-02-05 | 2015-02-05 | High-frequency-attached high-water-pressure-resistance polyurethane resin for leather and method for producing high-frequency-attached high-water-pressure-resistance polyurethane resin for leather |
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| CN201510058801.8A CN104650577A (en) | 2015-02-05 | 2015-02-05 | High-frequency-attached high-water-pressure-resistance polyurethane resin for leather and method for producing high-frequency-attached high-water-pressure-resistance polyurethane resin for leather |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105348475A (en) * | 2015-10-16 | 2016-02-24 | 广东大盈化工有限公司 | High-frequency laminating yellowing-free polyurethane fabric resin for white clothing leather and preparation method thereof |
| CN110951033A (en) * | 2019-12-19 | 2020-04-03 | 超然(福建)新材料科技有限公司 | Hydrolysis-resistant polyurethane resin and preparation method thereof |
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| CN103304770A (en) * | 2013-06-06 | 2013-09-18 | 广东伊诗德新材料科技有限公司 | High-temperature-resistant polyurethane resin for synthetic leather and preparation method thereof |
| CN103304769A (en) * | 2013-06-06 | 2013-09-18 | 广东伊诗德新材料科技有限公司 | High-wear-resistant polyurethane resin for synthetic leather and preparation method thereof |
| CN104004159A (en) * | 2014-06-16 | 2014-08-27 | 旭川化学（苏州）有限公司 | Polyurethane resin and preparation method and application thereof |
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2015
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| CN103304770A (en) * | 2013-06-06 | 2013-09-18 | 广东伊诗德新材料科技有限公司 | High-temperature-resistant polyurethane resin for synthetic leather and preparation method thereof |
| CN103304769A (en) * | 2013-06-06 | 2013-09-18 | 广东伊诗德新材料科技有限公司 | High-wear-resistant polyurethane resin for synthetic leather and preparation method thereof |
| CN104004159A (en) * | 2014-06-16 | 2014-08-27 | 旭川化学（苏州）有限公司 | Polyurethane resin and preparation method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105348475A (en) * | 2015-10-16 | 2016-02-24 | 广东大盈化工有限公司 | High-frequency laminating yellowing-free polyurethane fabric resin for white clothing leather and preparation method thereof |
| CN110951033A (en) * | 2019-12-19 | 2020-04-03 | 超然(福建)新材料科技有限公司 | Hydrolysis-resistant polyurethane resin and preparation method thereof |
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Application publication date: 20150527 |