CN102627751A - Urethane resin for impregnating ultrafine fiber for improving handfeel and dyeability and preparation method thereof - Google Patents
Urethane resin for impregnating ultrafine fiber for improving handfeel and dyeability and preparation method thereof Download PDFInfo
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- CN102627751A CN102627751A CN2012100995364A CN201210099536A CN102627751A CN 102627751 A CN102627751 A CN 102627751A CN 2012100995364 A CN2012100995364 A CN 2012100995364A CN 201210099536 A CN201210099536 A CN 201210099536A CN 102627751 A CN102627751 A CN 102627751A
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Abstract
The invention discloses urethane resin for impregnating ultrafine fiber for improving handfeel and dyeability. The urethane resin is prepared from the following raw materials in percentage by mass: 8-15 percent of diphenylmethane-4,4'-diisocyanate, 8-15 percent of polyether polyol, 3-8 percent of polyester polyol, 2-5 percent of a chain extender, 65-70 percent of N,N-dimethylformamide and the balance of other aids. The invention further discloses a preparation method of the urethane resin. By controlling a formula and process conditions for synthesizing the urethane resin, urethane resin which has good handfeel and is dyed uniformly can be produced.
Description
Technical field
The present invention relates to a kind of polyurethane resin for superfine fibre soaking that improves handling property and dyeability and preparation method thereof.
Background technology
At present general superfine fibre soaking is that feel is poor with the shortcoming of resin, and it is inhomogeneous to dye.The prescription and the technology that fall behind relatively at present are following: with PTMG 2000 (PTMG-2000) (65Kg), W 166 2000 (PPG-2000) (43Kg), PTMG 1000 (PTMG-1000) (54Kg) and NSC 6366 (NPG) (32Kg) drop in the reaction kettle stirring 10min; After intensification and controlled temperature are 60 ℃, add N, dinethylformamide (DMF) (420Kg) stirs 10min; Divide three times and add ditan-4,4 '-vulcabond (MDI), add-on is respectively 50Kg, 50Kg and 3Kg, is respectively 30min, 30min and 60min pitch time; When viscosity is ten thousand/75 ℃ of 15-16; Add N, dinethylformamide (DMF) (140Kg) dilutes, when viscosity is ten thousand/70 ℃ of 5-6; Add N again; Dinethylformamide (DMF) (140Kg) continues reaction, when viscosity is ten thousand/65 ℃ of 2.5-3, add inhibitor (FA-203) (2Kg), inhibitor (FA-202) (1Kg) stirs 30-60min and promptly accomplishes.The urethane resin that this prescription and explained hereafter go out is after the coating of ultra-fine fibre base material and handling; But the product feel that obtains is relatively poor with dyeability; Given this; The present invention is through synthetic a kind of novel urethane resin, again through the processing condition of control alkali decrement method, can obtain to have excellent hand with can chromatic product.
Summary of the invention
The object of the present invention is to provide a kind of polyurethane resin for superfine fibre soaking that improves handling property and dyeability; The present invention is through control urethane resin synthetic prescription and processing condition; The good hand touch of producing; The urethane resin of even dyeing after ultra-fine fibre base material coating, again through the processing condition of control alkali decrement method, can obtain to have excellent hand with can chromatic product.
In order to reach above-mentioned purpose, solution of the present invention is:
A kind of polyurethane resin for superfine fibre soaking that improves handling property and dyeability is formed by the preparation of raw material of following mass percent:
Ditan-4,4 '-vulcabond (MDI) (4,4-Methylene Diphenyldiisocyanate): 8%-15%;
Polyether glycol 8%-15%;
Polyester polyol 3%-8%;
Chainextender 2%-5%;
N, dinethylformamide (DMF) 65%-70%;
Surplus is other auxiliary agents.
The preferred mass per-cent of said raw material is:
Ditan-4,4 '-vulcabond (MDI) (4,4-Methylene Diphenyldiisocyanate): 11%;
Polyether glycol 11%;
Polyester polyol 5%;
Chainextender 3%;
N, dinethylformamide (DMF) 68%;
Other auxiliary agents 2%.
The molecular weight of described polyether glycol is 2000, and hydroxyl value is 53-59mgKOH/g.(manufacturer: Sinopec granary branch office)
Described polyester polyol polyester DF-1, molecular weight is 2000, hydroxyl value is 53-59mgKOH/g.(manufacturer: Jinjiang moral good fortune resin ltd)
Described chainextender adopts 1, the 4-butyleneglycol.
Described other auxiliary agents adopt viscosity stabilizer, chain terminator, photostabilizer and oxidation inhibitor.
Described viscosity stabilizer adopts oxysuccinic acid, and chain terminator adopts methyl alcohol, and described viscosity stabilizer adopts oxysuccinic acid, and chain terminator adopts the methyl alcohol photostabilizer to adopt the GW-480 photostabilizer, and oxidation inhibitor adopts B215 oxidation inhibitor.(manufacturer: be the prosperous perseverance in Xiamen and become ltd).
A kind of polyurethane resin for superfine fibre soaking preparation method who improves handling property and dyeability, 1) polyether glycol and the polyester polyol with above-mentioned mass percent is dosed in the reaction kettle, drops into the DMF of chainextender and the total add-on 60% of DMF behind the heating and melting; 2) maintain the temperature at 50-70 ℃, the MDI that drops into above-mentioned mass percent 1/2nd amounts earlier carries out building-up reactions, prevents that MDI from adding the back temperature and sharply rising; 3) when synthesis reaction temperature is lower than 80 ℃, the MDI that drops into remaining 1/2nd amounts continues reaction; 4) when reaching pre-polymerization viscosity 15-16 * 10
4During cps, drop into the dilution continued reaction of the total add-on 20% of DMF, when viscosity reaches 5-6 * 10
4Drop into the DMF dilution of the total add-on 20% of DMF during cps once more; Final viscosity is controlled at 2-3 * 10
4Cps; 5) confirm that isocyanate-free base (NCO) is residual after, drop into viscosity stabilizer oxysuccinic acid stable viscosity; After building-up reactions stops, drop into chain terminator methyl alcohol, drop into photostabilizer again, oxidation inhibitor obtains urethane resin.
Beneficial effect of the present invention is: the present invention is through control urethane resin synthetic prescription and processing condition; The good hand touch of producing; The urethane resin of even dyeing is after the coating of ultra-fine fibre base material; Again through the processing condition of control alkali decrement method, can obtain to have excellent hand with can chromatic product.
Embodiment
Embodiment 1
A kind of polyurethane resin for superfine fibre soaking that improves handling property and dyeability comprises that main preparation of raw material by following mass percent forms: MDI (4,4-Methylene Diphenyl diisocyanate): 11%; Molecular weight is 2000, and hydroxyl value is the polyether glycol 11% of 53-59mgKOH/g; (manufacturer: Sinopec granary branch office); Polyester DF-1, molecular weight are 2000, and hydroxyl value is the polyester polyol 5% of 53-59mgKOH/g; (manufacturer: Jinjiang moral good fortune resin ltd); Chainextender (1, the 4-butyleneglycol): 3%; DMF:68%; Other auxiliary agents 2% comprise viscosity stabilizer, chain terminator, photostabilizer and oxidation inhibitor; Wherein viscosity stabilizer adopts oxysuccinic acid, and chain terminator adopts methyl alcohol, and photostabilizer adopts GW-480, and oxidation inhibitor adopts B215.
A kind of polyurethane resin for superfine fibre soaking preparation method who improves handling property and dyeability of present embodiment; 1) is that 11% polyether glycol and 5% polyester polyol are dosed in the reaction kettle with mass percent, drops into the DMF of 3% chainextender and the total add-on 60% of DMF behind the heating and melting; 2) maintain the temperature at 50-70 ℃, dropping into mass percent earlier is that the MDI that 1/2nd in 11% is measured carries out building-up reactions, prevents that MDI from adding the back temperature and sharply rising; 3) when synthesis reaction temperature is lower than 80 ℃, the MDI that drops into remaining 1/2nd amounts continues reaction; 4) when reaching pre-polymerization viscosity 15-16 * 10
4During cps, drop into the DMF dilution continued reaction of the total add-on 20% of DMF, when viscosity reaches 5-6 * 10
4Drop into the DMF dilution of the total add-on 20% of DMF during cps once more; Final viscosity is controlled at 2-3 * 10
4Cps; 5) confirm that isocyanate-free base (NCO) is residual after, drop into mass percent and be other auxiliary agents of 2%, comprise viscosity stabilizer oxysuccinic acid stable viscosity; After building-up reactions stops, drop into chain terminator methyl alcohol, drop into GW-480 photostabilizer (manufacturer: the prosperous perseverance in Xiamen becomes ltd) again, B215 oxidation inhibitor (manufacturer: the prosperous perseverance in Xiamen becomes ltd) obtains urethane resin.
The new polyurethane resin that makes through above-mentioned said method is 10% at naoh concentration, temperature is 90-100 ℃ and carries out alkali decrement method aftertreatment 30-50min after the coating of ultra-fine fibre base material.Dyeing temperature be 100-110 ℃ with dyeing time be under the dyeing condition of 2h, can obtain to have excellent hand with can chromatic polyurethane coating product.
Embodiment 2
A kind of polyurethane resin for superfine fibre soaking that improves handling property and dyeability comprises that main preparation of raw material by following mass percent forms: MDI (4,4-Methylene Diphenyl diisocyanate): 8%; Molecular weight is 2000, and hydroxyl value is the polyether glycol 15% of 53-59mgKOH/g; (manufacturer: Sinopec granary branch office); Polyester DF-1, molecular weight are 2000, and hydroxyl value is the polyester polyol 8% of 53-59mgKOH/g; (manufacturer: Jinjiang moral good fortune resin ltd); Chainextender (1, the 4-butyleneglycol): 2%; DMF:65%; Other auxiliary agents 2% comprise viscosity stabilizer, chain terminator, photostabilizer and oxidation inhibitor; Wherein viscosity stabilizer adopts oxysuccinic acid, and chain terminator adopts methyl alcohol, and photostabilizer adopts GW-480, and oxidation inhibitor adopts B215.
A kind of polyurethane resin for superfine fibre soaking preparation method who improves handling property and dyeability of present embodiment; 1) is that 15% polyether glycol and 8% polyester polyol are dosed in the reaction kettle with mass percent, drops into the DMF of 2% chainextender and the total add-on 60% of DMF behind the heating and melting; 2) maintain the temperature at 50-70 ℃, dropping into mass percent earlier is that the MDI that 1/2nd in 8% is measured carries out building-up reactions, prevents that MDI from adding the back temperature and sharply rising; 3) when synthesis reaction temperature is lower than 80 ℃, the MDI that drops into remaining 1/2nd amounts continues reaction; 4) when reaching pre-polymerization viscosity 15-16 * 10
4During cps, drop into the DMF dilution continued reaction of the total add-on 20% of DMF, when viscosity reaches 5-6 * 10
4Drop into the DMF dilution of the total add-on 20% of DMF during cps once more; Final viscosity is controlled at 2-3 * 10
4Cps; 5) confirm that isocyanate-free base (NCO) is residual after, drop into mass percent and be other auxiliary agents of 2%, comprise viscosity stabilizer oxysuccinic acid stable viscosity; After building-up reactions stops, drop into chain terminator methyl alcohol, drop into GW-480 photostabilizer (manufacturer: the prosperous perseverance in Xiamen becomes ltd) again, B215 oxidation inhibitor (manufacturer: the prosperous perseverance in Xiamen becomes ltd) obtains urethane resin.
The new polyurethane resin that makes through above-mentioned said method is 10% at naoh concentration, temperature is 90-100 ℃ and carries out alkali decrement method aftertreatment 30-50min after the coating of ultra-fine fibre base material.Dyeing temperature be 100-110 ℃ with dyeing time be under the dyeing condition of 2h, can obtain to have excellent hand with can chromatic polyurethane coating product.
Embodiment 3
A kind of polyurethane resin for superfine fibre soaking that improves handling property and dyeability comprises that main preparation of raw material by following mass percent forms: MDI (4,4-Methylene Diphenyl diisocyanate): 15%; Molecular weight is 2000, and hydroxyl value is the polyether glycol 8% of 53-59mgKOH/g; (manufacturer: Sinopec granary branch office); Polyester DF-1, molecular weight are 2000, and hydroxyl value is the polyester polyol 3% of 53-59mgKOH/g; (manufacturer: Jinjiang moral good fortune resin ltd); Chainextender (1, the 4-butyleneglycol): 5%; DMF:68%; Other auxiliary agents 1% comprise viscosity stabilizer, chain terminator, photostabilizer and oxidation inhibitor; Wherein viscosity stabilizer adopts oxysuccinic acid, and chain terminator adopts methyl alcohol, and photostabilizer adopts GW-480, and oxidation inhibitor adopts B215.
A kind of polyurethane resin for superfine fibre soaking preparation method who improves handling property and dyeability of present embodiment; 1) is that 8% polyether glycol and 3% polyester polyol are dosed in the reaction kettle with mass percent, drops into the DMF of 5% chainextender and the total add-on 60% of DMF behind the heating and melting; 2) maintain the temperature at 50-70 ℃, dropping into mass percent earlier is that the MDI that 1/2nd in 15% is measured carries out building-up reactions, prevents that MDI from adding the back temperature and sharply rising; 3) when synthesis reaction temperature is lower than 80 ℃, the MDI that drops into remaining 1/2nd amounts continues reaction; 4) when reaching pre-polymerization viscosity 15-16 * 10
4During cps, drop into the DMF dilution continued reaction of the total add-on 20% of DMF, when viscosity reaches 5-6 * 10
4Drop into the DMF dilution of the total add-on 20% of DMF during cps once more; Final viscosity is controlled at 2-3 * 10
4Cps; 5) confirm that isocyanate-free base (NCO) is residual after, drop into mass percent and be other auxiliary agents of 2%, comprise viscosity stabilizer oxysuccinic acid stable viscosity; After building-up reactions stops, drop into chain terminator methyl alcohol, drop into GW-480 photostabilizer (manufacturer: the prosperous perseverance in Xiamen becomes ltd) again, B215 oxidation inhibitor (manufacturer: the prosperous perseverance in Xiamen becomes ltd) obtains urethane resin.
The new polyurethane resin that makes through above-mentioned said method is 10% at naoh concentration, temperature is 90-100 ℃ and carries out alkali decrement method aftertreatment 30-50min after the coating of ultra-fine fibre base material.Dyeing temperature be 100-110 ℃ with dyeing time be under the dyeing condition of 2h, can obtain to have excellent hand with can chromatic polyurethane coating product.
Claims (8)
1. polyurethane resin for superfine fibre soaking that improves handling property and dyeability is characterized in that being formed by the preparation of raw material of following mass percent:
Ditan-4,4 '-vulcabond 8%-15%;
Polyether glycol 8%-15%;
Polyester polyol 3%-8%;
Chainextender: 2%-5%;
N, dinethylformamide: 65%-70%;
Surplus is other auxiliary agents.
2. a kind of polyurethane resin for superfine fibre soaking that improves handling property and dyeability as claimed in claim 1 is characterized in that the mass percent of said raw material is:
Ditan-4,4 '-vulcabond 11%;
Polyether glycol 11%;
Polyester polyol 5%;
Chainextender 3%;
N, dinethylformamide 68%;
Other auxiliary agents 2%.
3. according to claim 1 or claim 2 a kind of polyurethane resin for superfine fibre soaking that improves handling property and dyeability, it is characterized in that: the molecular weight of described polyether glycol is 2000, hydroxyl value is 53-59mgKOH/g.
4. according to claim 1 or claim 2 a kind of polyurethane resin for superfine fibre soaking that improves handling property and dyeability, it is characterized in that: the molecular weight of described polyester polyol is 2000, hydroxyl value is 53-59mgKOH/g.
5. according to claim 1 or claim 2 a kind of polyurethane resin for superfine fibre soaking that improves handling property and dyeability, it is characterized in that: described chainextender adopts 1, the 4-butyleneglycol.
6. according to claim 1 or claim 2 a kind of polyurethane resin for superfine fibre soaking that improves handling property and dyeability, it is characterized in that: described other auxiliary agents adopt viscosity stabilizer, chain terminator, photostabilizer and oxidation inhibitor.
7. a kind of polyurethane resin for superfine fibre soaking that improves handling property and dyeability as claimed in claim 6; It is characterized in that: described viscosity stabilizer adopts oxysuccinic acid; Chain terminator adopts the methyl alcohol photostabilizer to adopt the GW-480 photostabilizer, and oxidation inhibitor adopts B215 oxidation inhibitor.
8. the polyurethane resin for superfine fibre soaking preparation method of raising handling property as claimed in claim 1 and dyeability; It is characterized in that: 1) polyether glycol and the polyester polyol with above-mentioned mass percent is dosed in the reaction kettle; Drop into chainextender and N behind the heating and melting; The N of the total add-on 60% of dinethylformamide, dinethylformamide; 2) maintain the temperature at 50-70 ℃, drop into the ditan-4 of above-mentioned mass percent 1/2nd amounts earlier, 4 '-vulcabond carries out building-up reactions, prevents ditan-4, and 4 '-vulcabond adds the back temperature and sharply rises; 3) when synthesis reaction temperature is lower than 80 ℃, drop into the ditan-4 of remaining 1/2nd amounts, 4 '-vulcabond continues reaction; 4) when reaching pre-polymerization viscosity 15-16 * 10
4During cps, drop into N, the N of the total add-on 20% of dinethylformamide, the reaction of dinethylformamide dilution continued is when viscosity reaches 5-6 * 10
4Drop into N during cps once more, the N of the total add-on 20% of dinethylformamide, dinethylformamide dilution; Final viscosity is controlled at 2-3 * 10
4Cps; 5) confirm that the isocyanate-free base is residual after, drop into viscosity stabilizer oxysuccinic acid stable viscosity; After building-up reactions stops, drop into chain terminator methyl alcohol, drop into photostabilizer, oxidation inhibitor again, obtain urethane resin.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100995364A CN102627751A (en) | 2012-04-06 | 2012-04-06 | Urethane resin for impregnating ultrafine fiber for improving handfeel and dyeability and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012100995364A CN102627751A (en) | 2012-04-06 | 2012-04-06 | Urethane resin for impregnating ultrafine fiber for improving handfeel and dyeability and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103641978A (en) * | 2013-12-06 | 2014-03-19 | 上海华峰超纤材料股份有限公司 | Polyurethane resin slurry and industrial application thereof |
| CN105968288A (en) * | 2016-06-02 | 2016-09-28 | 台州禾欣高分子新材料有限公司 | High-modulus high-resilience polyurethane resin and preparation method and application thereof |
| CN109593455A (en) * | 2018-10-25 | 2019-04-09 | 运研材料科技（上海）有限公司 | A kind of skin hydronasty polyurethane coating and preparation method thereof |
| CN111087566A (en) * | 2019-09-29 | 2020-05-01 | 扬州工业职业技术学院 | Preparation method of polyester modified biomass hydrolysis-resistant high-peel-resistance PU wet resin |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1688447A1 (en) * | 2003-11-18 | 2006-08-09 | Sanyo Chemical Industries, Ltd. | Polyurethane resin for artificial leather and porous sheet material |
| CN101481449A (en) * | 2009-01-23 | 2009-07-15 | 合肥安利化工有限公司 | Wet impregnated polyurethane resin for high hydrolysis resistance synthetic leather and preparation thereof |
| CN102212183A (en) * | 2011-05-03 | 2011-10-12 | 烟台华大化学工业有限公司 | Polyurethane resin used for skin-imitated superfine fiber synthetic leather, and preparation method thereof |
-
2012
- 2012-04-06 CN CN2012100995364A patent/CN102627751A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1688447A1 (en) * | 2003-11-18 | 2006-08-09 | Sanyo Chemical Industries, Ltd. | Polyurethane resin for artificial leather and porous sheet material |
| CN101481449A (en) * | 2009-01-23 | 2009-07-15 | 合肥安利化工有限公司 | Wet impregnated polyurethane resin for high hydrolysis resistance synthetic leather and preparation thereof |
| CN102212183A (en) * | 2011-05-03 | 2011-10-12 | 烟台华大化学工业有限公司 | Polyurethane resin used for skin-imitated superfine fiber synthetic leather, and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103641978A (en) * | 2013-12-06 | 2014-03-19 | 上海华峰超纤材料股份有限公司 | Polyurethane resin slurry and industrial application thereof |
| CN103641978B (en) * | 2013-12-06 | 2015-10-28 | 上海华峰超纤材料股份有限公司 | A kind of Polyurethane resin slurry and industrial application thereof |
| CN105968288A (en) * | 2016-06-02 | 2016-09-28 | 台州禾欣高分子新材料有限公司 | High-modulus high-resilience polyurethane resin and preparation method and application thereof |
| CN109593455A (en) * | 2018-10-25 | 2019-04-09 | 运研材料科技（上海）有限公司 | A kind of skin hydronasty polyurethane coating and preparation method thereof |
| CN111087566A (en) * | 2019-09-29 | 2020-05-01 | 扬州工业职业技术学院 | Preparation method of polyester modified biomass hydrolysis-resistant high-peel-resistance PU wet resin |
| CN111087566B (en) * | 2019-09-29 | 2021-10-29 | 扬州工业职业技术学院 | Preparation method of polyester modified biomass hydrolysis-resistant high-peel-resistance PU wet resin |
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Application publication date: 20120808 |