CN103467696A - Preparation method of soft high-elasticity embossed sofa leather wet-method polyurethane resin - Google Patents
Preparation method of soft high-elasticity embossed sofa leather wet-method polyurethane resin Download PDFInfo
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- CN103467696A CN103467696A CN201310356394XA CN201310356394A CN103467696A CN 103467696 A CN103467696 A CN 103467696A CN 201310356394X A CN201310356394X A CN 201310356394XA CN 201310356394 A CN201310356394 A CN 201310356394A CN 103467696 A CN103467696 A CN 103467696A
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Abstract
The invention discloses a preparation method of a soft high-elasticity embossed sofa leather wet-method polyurethane resin. The preparation method comprises the steps: carrying out an appropriate prepolymerization reaction of polyols and a mixture of the polyols, and during prepolymerization, adding quantitative diisocyanate to carry out a reaction for a certain time to control the prepolymerization reaction; after finishing prepolymerization, again adding small-molecule diol and diamine for mixing, and then carrying out a chain extension reaction; finally again adding a resin modifier and an auxiliary agent; and controlling a final resin viscosity in a standard range, and ending the reaction. The soft high-elasticity embossed sofa leather wet-method polyurethane resin solves defects existing in hand feeling elasticity and hand feeling changes before and after embossing in a conventional ordinary soft low-modulus wet-method polyurethane resin after finishing leather. Synthetic leather prepared by the polyurethane resin has soft hand feeling, fullness and good elasticity, also can satisfy embossing properties, has clear and full embossed patterns, and can keep the hand feeling changed little before and after embossing.
Description
Technical field
The present invention relates to a kind of preparation method of soft snappiness embossing sofa artificial leather wet polyurethane resin, belong to technical field of polymer materials.
Background technology
Because the natural resources of corium product is limited, price is high, can't meet the growing market requirement.And Synthetic Leather products material wide material sources, low price, good processability, more and more level off to the characteristic of natural leather, meets people's life seek fully.The application of urethane resin aspect synthetic leather is mainly reflected in a plurality of fields such as clothes, case and bag, footwear, furniture, automobile, leather is more and more faster with the tempo of urethane resin in recent years, in the face of the increasing gradually of the market requirement, leather is proposed to higher requirement with urethane resin.For example, sofa artificial leather, clothing leather, glove leather etc. not only require soft, plentiful, good springiness, also want to meet embossability, and the embossing decorative pattern is clear full, before and after embossing, can keep feel to change little.At present, occur many soft low modulus Wet-type polyurethane resins on market, but, in feel elasticity, also there is a certain distance in the aspects such as embossability and the feel variation of embossing front and back, thereby make the leather goods of producing be difficult to meet the growing market requirement.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of soft snappiness embossing sofa artificial leather wet polyurethane resin, to solve after ordinary soft low modulus wet polyurethane resin finished leather in feel elasticity, the defect that before and after embossability and embossing, the aspect such as feel variation exists.
Reaction mechanism of the present invention is: in the urethane resin building-up process, select the polyester polyol that flexibility is better, contain ehter bond for soft section, guarantee the soft of resin, embossability is preferably arranged simultaneously; Add appropriate high polarity amine chain extender in hard section, the rigidity of the polarity of raising resin, elasticity and hard section, the pass anchorage force while improving the resin finished leather, guarantee that embossing front and back feel changes less; Finally add again modifier and auxiliary agent, send out permeability energy and fullness ratio while improving the resin finished leather.Thereby this resin not only has soft, plentiful, good springiness; Can also meet embossability, the embossing decorative pattern is clear full, before and after embossing, can keep feel to change the characteristics such as little.
For achieving the above object, the technological method that the present invention adopts is as follows:
A kind of preparation method of soft snappiness embossing sofa artificial leather wet polyurethane resin comprises the following steps:
(1) in reactor, various polyester polyols of input and composition thereof, oxidation inhibitor I-1010, partial solvent DMF are mixed, stir and drop into again quantitative di-isocyanate reaction after 10-15 minute, now 90% of the quantitative reasonable stoichiometric of vulcabond, during pre-polymerization, solid content should be controlled at 50-60%, the still temperature control is at 70-80 ℃, and the reaction times is controlled at 60-80 minute;
(2) add again afterwards small molecules dibasic alcohol that molecular weight is 62-200g/mol and diamine mixed chain extender, under the condition that adds catalyzer to exist, with vulcabond generation chain extending reaction, continuous increase along with system viscosity, progressively add remaining solvent DMF, final viscosity is controlled at 120-220PaS/25 ℃;
(3) reaction adds terminator methyl alcohol after finishing, and finally adds modifier and auxiliary agent again, to improve the wet type processing characteristics of resin;
(4) cool to being rushed down material, metering packing below 60 ℃.
Described polyester polyol and composition thereof composed as follows: poly-hexanodioic acid glycol ether BDO esterdiol: number-average molecular weight is 3000 ± 300g/mol, accounts for the 70-100wt% of polyol blends; Poly-adipate glycol glycol ether esterdiol: number-average molecular weight is 2000 ± 200g/mol, accounts for the 30-0wt% of polyol blends; Described polyester polyol and composition thereof and small molecules dibasic alcohol and diamine mixed chain extender mol ratio 1:1.5-2.5.
The 0.1-0.2% that the consumption of described oxidation inhibitor I-1010 is the system gross weight; The 69-71% that the consumption of described solvent DMF is the system gross weight.
Described vulcabond is 4,4 '-diphenylmethanediisocyanate.
The small molecules dibasic alcohol that described molecular weight is 62-200g/mol and diamine mixed chain extender are ethylene glycol, BDO, 1, one or both in 6-hexylene glycol, diphenylmethanediamiand; Wherein when dibasic alcohol, with diamine, mix while using, its molar ratio is 7-12:1; The consumption of described dibasic alcohol and diamine mixed chain extender accounts for the 1-2% of system gross weight.
Described catalyzer is organo-bismuth class catalyzer MB20, the 0.1-1 ‰ that consumption is polyester polyol and compound weight thereof; Described modifier is the acetic acid butyl cellulose, the 1-1.5% that consumption is the system gross weight; Described auxiliary agent is one or both the mixture in softening agent, flow agent, the 2-3% that consumption is the system gross weight.
Described polyester polyol and composition thereof, vulcabond, small molecules dibasic alcohol and diamine mixed chain extender, solvent DMF all require water ratio to be less than 500ppm.
Beneficial effect of the present invention:
The soft snappiness embossing sofa artificial leather Wet-type polyurethane resin that the present invention makes, solved after existing ordinary soft low modulus wet polyurethane resin finished leather in feel elasticity, the defect that before and after embossability and embossing, the aspect such as feel variation exists.Use not only soft, plentiful, good springiness of synthetic leather that soft snappiness embossing sofa artificial leather Wet-type polyurethane resin of the present invention makes, also want to meet embossability, the embossing decorative pattern is clear full, before and after embossing, can keep feel to change little.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach purpose and effect is easy to understand, below in conjunction with embodiment, further set forth the present invention.
embodiment 1:
Material name weight (unit K g)
Poly-hexanodioic acid glycol ether BDO esterdiol 650
Poly-adipate glycol glycol ether esterdiol 200
Ethylene glycol 34
4,4-diphenylmethanediamiand 12
4,4-diphenylmethanediisocyanate 232
Oxidation inhibitor I-1010 7.0
Catalyzer MB20 0.3
Softening agent 120
Acetic acid butyl cellulose 50
DMF 3050
Wherein, poly-hexanodioic acid glycol ether BDO esterdiol is: the polyester polyol of number-average molecular weight 3000 ± 300g/mol,
Poly-adipate glycol glycol ether esterdiol is: the polyester polyol of number-average molecular weight 2000 ± 200g/mol.
Be prepared according to the following steps:
(1) in reactor, the various polyester polyols alcohol mixtures of input, oxidation inhibitor I-1010, part DMF are mixed, stir after 10-15 minute and drop into again quantitative MDI reaction, now 90% of the quantitative reasonable stoichiometric of MDI, during pre-polymerization, solid content should be controlled at 50-60%, the still temperature control, at 70-80 ℃, is reacted about 60-80 minute;
(2) and then add DMF to stir 10 minutes, rear input ethylene glycol (EG) and 4,4-diphenylmethanediamiand (MDA), stir and within 20 minutes, drop into the MDI reaction again, reacts after 30 minutes and add catalyzer MB20 to continue reaction again;
(3) progressively add MDI midway and continue reaction, and, along with the continuous increase of system viscosity, progressively add required solvent DMF.Final viscosity is controlled at 120-220PaS/25 ℃, and the still temperature control is between 70-80 ℃;
(4) reaction adds terminator methyl alcohol after finishing, and finally adds softening agent, modifier again;
(5) cool to being rushed down material, metering packing below 60 ℃.
embodiment 2:
Material name weight (unit K g)
Poly-hexanodioic acid glycol ether BDO esterdiol 750
Poly-adipate glycol glycol ether esterdiol 100
Ethylene glycol 35
4,4-diphenylmethanediamiand 10
4,4-diphenylmethanediisocyanate 229
Oxidation inhibitor I-1010 7.0
Catalyzer MB20 0.3
Softening agent 120
Acetic acid butyl cellulose 50
DMF 3040
Wherein, poly-hexanodioic acid glycol ether BDO esterdiol is: the polyester polyol of number-average molecular weight 3000 ± 300g/mol,
Poly-adipate glycol glycol ether esterdiol is: the polyester polyol of number-average molecular weight 2000 ± 200g/mol.
Be prepared according to the following steps:
(1) in reactor, the various polyester polyols alcohol mixtures of input, oxidation inhibitor I-1010, part DMF are mixed, stir after 10-15 minute and drop into again quantitative MDI reaction, now 90% of the quantitative reasonable stoichiometric of MDI, during pre-polymerization, solid content should be controlled at 50-60%, the still temperature control, at 70-80 ℃, is reacted about 60-80 minute;
(2) and then add DMF to stir 10 minutes, rear input ethylene glycol (EG) and 4,4-diphenylmethanediamiand (MDA), stir and within 20 minutes, drop into the MDI reaction again, reacts after 30 minutes and add catalyzer MB20 to continue reaction again;
(3) progressively add MDI midway and continue reaction, and, along with the continuous increase of system viscosity, progressively add required solvent DMF.Final viscosity is controlled at 120-220PaS/25 ℃, and the still temperature control is between 70-80 ℃.
(4) reaction adds terminator methyl alcohol after finishing, and finally adds softening agent, modifier again;
(5) cool to being rushed down material, metering packing below 60 ℃.
embodiment 3:
Material name weight (unit K g)
Poly-hexanodioic acid glycol ether BDO esterdiol 800
Poly-adipate glycol glycol ether esterdiol 50
BDO 48
4,4-diphenylmethanediamiand 14
4,4-diphenylmethanediisocyanate 224
Oxidation inhibitor I-1010 7.0
Catalyzer MB20 0.3
Softening agent 120
Acetic acid butyl cellulose 50
DMF 3065
Wherein, poly-hexanodioic acid glycol ether BDO esterdiol is: the polyester polyol of number-average molecular weight 3000 ± 300g/mol,
Poly-adipate glycol glycol ether esterdiol is: the polyester polyol of number-average molecular weight 2000 ± 200g/mol.
Be prepared according to the following steps:
(1) in reactor, the various polyester polyols alcohol mixtures of input, oxidation inhibitor I-1010, part DMF are mixed, stir after 10-15 minute and drop into again quantitative MDI reaction, now 90% of the quantitative reasonable stoichiometric of MDI, during pre-polymerization, solid content should be controlled at 50-60%, the still temperature control, at 70-80 ℃, is reacted about 60-80 minute;
(2) and then add DMF to stir 10 minutes, rear input BDO (BG) and 4,4-diphenylmethanediamiand (MDA), stir and within 20 minutes, drop into the MDI reaction again, reacts after 30 minutes and add catalyzer MB20 to continue reaction again;
(3) progressively add MDI midway and continue reaction, and, along with the continuous increase of system viscosity, progressively add required solvent DMF.Final viscosity is controlled at 120-220PaS/25 ℃, and the still temperature control is between 70 ~ 80 ℃;
(4) reaction adds terminator methyl alcohol after finishing, and finally adds softening agent, modifier again;
(5) cool to being rushed down material, metering packing below 60 ℃.
In order to verify not only soft, plentiful, good springiness of synthetic leather that soft snappiness embossing sofa artificial leather Wet-type polyurethane resin of the present invention makes, can also meet embossability, the embossing decorative pattern is clear full, before and after embossing, can keep feel to change the advantages such as little.Resin prepared in above-mentioned embodiment and the contrast of ordinary soft low modulus Wet-type polyurethane resin, according to the known method of synthetic leather industry, draw a design.Through examination, survey, with the made wet method crust leather of resin of above-mentioned embodiment 1,2,3 preparations, soft plentiful, good springiness; And the wet method crust leather that ordinary soft low modulus Wet-type polyurethane resin is made is soft, but fullness ratio and elasticity are all general.Equally, with the made wet method crust leather of resin of above-mentioned embodiment 1,2,3 preparations, easily embossing, decorative pattern is clear full, and before and after embossing, feel changes little; And the wet method crust leather that ordinary soft low modulus Wet-type polyurethane resin is made, the energy embossing, but decorative pattern is clear not full, and before and after embossing, feel changes greatly.
The so-called system of the present invention, refer to whole reaction system, is exactly the total amount of all substances.The present invention is not subject to the restriction of above-mentioned case study on implementation, that in above-mentioned embodiment and specification sheets, describes just illustrates principle of the present invention, the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, within these changes and improvements all belong to context of the present invention.
Claims (7)
1. the preparation method of a soft snappiness embossing sofa artificial leather wet polyurethane resin, is characterized in that, comprises the following steps:
(1) in reactor, various polyester polyols of input and composition thereof, oxidation inhibitor I-1010, partial solvent DMF are mixed, stir and drop into again quantitative di-isocyanate reaction after 10-15 minute, now 90% of the quantitative reasonable stoichiometric of vulcabond, during pre-polymerization, solid content should be controlled at 50-60%, the still temperature control is at 70-80 ℃, and the reaction times is controlled at 60-80 minute;
(2) add again afterwards small molecules dibasic alcohol that molecular weight is 62-200g/mol and diamine mixed chain extender, under the condition that adds catalyzer to exist, with vulcabond generation chain extending reaction, continuous increase along with system viscosity, progressively add remaining solvent DMF, final viscosity is controlled at 120-220PaS/25 ℃;
(3) reaction adds terminator methyl alcohol after finishing, and finally adds modifier and auxiliary agent again, to improve the wet type processing characteristics of resin;
(4) cool to being rushed down material, metering packing below 60 ℃.
2. the preparation method of a kind of soft snappiness embossing sofa artificial leather wet polyurethane resin according to claim 1, it is characterized in that, described polyester polyol and composition thereof composed as follows: poly-hexanodioic acid glycol ether 1,4-butanediol ester glycol: number-average molecular weight is 3000 ± 300g/mol, accounts for the 70-100wt% of polyol blends; Poly-adipate glycol glycol ether esterdiol: number-average molecular weight is 2000 ± 200g/mol, accounts for the 30-0wt% of polyol blends; Described polyester polyol and composition thereof and small molecules dibasic alcohol and diamine mixed chain extender mol ratio 1:1.5-2.5.
3. the preparation method of a kind of soft snappiness embossing sofa artificial leather wet polyurethane resin according to claim 1, is characterized in that the 0.1-0.2% that the consumption of described oxidation inhibitor I-1010 is the system gross weight; The 69-71% that the consumption of described solvent DMF is the system gross weight.
4. the preparation method of a kind of soft snappiness embossing sofa artificial leather wet polyurethane resin according to claim 1, is characterized in that, described vulcabond is 4,4 '-diphenylmethanediisocyanate.
5. the preparation method of a kind of soft snappiness embossing sofa artificial leather wet polyurethane resin according to claim 1, it is characterized in that, the small molecules dibasic alcohol that described molecular weight is 62-200g/mol and diamine mixed chain extender are ethylene glycol, 1,4-butyleneglycol, 1, one or both in 6-hexylene glycol, diphenylmethanediamiand; Wherein when dibasic alcohol, with diamine, mix while using, its molar ratio is 7-12:1; The consumption of described dibasic alcohol and diamine mixed chain extender accounts for the 1-2% of system gross weight.
6. the preparation method of a kind of soft snappiness embossing sofa artificial leather wet polyurethane resin according to claim 1, is characterized in that, described catalyzer is organo-bismuth class catalyzer MB20, the 0.1-1 ‰ that consumption is polyester polyol and compound weight thereof; Described modifier is the acetic acid butyl cellulose, the 1-1.5% that consumption is the system gross weight; Described auxiliary agent is one or both the mixture in softening agent, flow agent, the 2-3% that consumption is the system gross weight.
7. the preparation method of a kind of soft snappiness embossing sofa artificial leather wet polyurethane resin according to claim 1, it is characterized in that, described polyester polyol and composition thereof, vulcabond, small molecules dibasic alcohol and diamine mixed chain extender, solvent DMF all require water ratio to be less than 500ppm.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103804627A (en) * | 2014-02-19 | 2014-05-21 | 合肥安利聚氨酯新材料有限公司 | Wet high-stripping polyurethane resin and preparation method thereof |
| CN105111406A (en) * | 2015-09-14 | 2015-12-02 | 合肥安利聚氨酯新材料有限公司 | High-plasticity wet process polyurethane resin for hydrolysis-resistant sofa leather and preparation method thereof |
| CN105153399A (en) * | 2015-09-29 | 2015-12-16 | 合肥安利聚氨酯新材料有限公司 | Hydrolysis-resistant super-soft wet-wax-feeling dry-method surface layer resin and preparation method thereof |
| CN105199078A (en) * | 2015-10-08 | 2015-12-30 | 合肥安利聚氨酯新材料有限公司 | Medium-soft luggage leather embossing resin for elastic fabrics and preparation method thereof |
| CN106397716A (en) * | 2016-09-06 | 2017-02-15 | 上海华峰超纤材料股份有限公司 | Moisture absorption dyeable polyurethane resin and preparation method thereof |
| CN106883371A (en) * | 2017-03-23 | 2017-06-23 | 苏州富仁化工有限公司 | A kind of modified polyurethane resin and preparation method thereof |
| CN108894007A (en) * | 2018-06-15 | 2018-11-27 | 合肥安利聚氨酯新材料有限公司 | Sofa furniture class use for synthetic leather polyurethane cover resin |
| CN109666114A (en) * | 2018-12-11 | 2019-04-23 | 无锡双象超纤材料股份有限公司 | A kind of preparation method of Cambodia's sense woven fabric sofa artificial leather wet polyurethane resin |
| CN109853254A (en) * | 2019-02-28 | 2019-06-07 | 扬州工业职业技术学院 | A kind of middle hard mirror surface polyurethane wet bass and preparation method thereof |
| CN110437410A (en) * | 2019-08-08 | 2019-11-12 | 合肥安利聚氨酯新材料有限公司 | A kind of soft easy embossing wet polyurethane resin of polyether-type and preparation method thereof |
| CN115260440A (en) * | 2022-08-16 | 2022-11-01 | 江苏华大新材料有限公司 | Polyurethane resin for wet-process embossing synthetic leather and preparation method thereof |
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| CN103804627A (en) * | 2014-02-19 | 2014-05-21 | 合肥安利聚氨酯新材料有限公司 | Wet high-stripping polyurethane resin and preparation method thereof |
| CN105111406A (en) * | 2015-09-14 | 2015-12-02 | 合肥安利聚氨酯新材料有限公司 | High-plasticity wet process polyurethane resin for hydrolysis-resistant sofa leather and preparation method thereof |
| CN105153399B (en) * | 2015-09-29 | 2018-04-10 | 合肥安利聚氨酯新材料有限公司 | A kind of wet wax sense dry method surface layer resin of hydrolysis ultra-soft matter and preparation method thereof |
| CN105153399A (en) * | 2015-09-29 | 2015-12-16 | 合肥安利聚氨酯新材料有限公司 | Hydrolysis-resistant super-soft wet-wax-feeling dry-method surface layer resin and preparation method thereof |
| CN105199078A (en) * | 2015-10-08 | 2015-12-30 | 合肥安利聚氨酯新材料有限公司 | Medium-soft luggage leather embossing resin for elastic fabrics and preparation method thereof |
| CN106397716A (en) * | 2016-09-06 | 2017-02-15 | 上海华峰超纤材料股份有限公司 | Moisture absorption dyeable polyurethane resin and preparation method thereof |
| CN106883371A (en) * | 2017-03-23 | 2017-06-23 | 苏州富仁化工有限公司 | A kind of modified polyurethane resin and preparation method thereof |
| CN108894007A (en) * | 2018-06-15 | 2018-11-27 | 合肥安利聚氨酯新材料有限公司 | Sofa furniture class use for synthetic leather polyurethane cover resin |
| CN109666114A (en) * | 2018-12-11 | 2019-04-23 | 无锡双象超纤材料股份有限公司 | A kind of preparation method of Cambodia's sense woven fabric sofa artificial leather wet polyurethane resin |
| CN109853254A (en) * | 2019-02-28 | 2019-06-07 | 扬州工业职业技术学院 | A kind of middle hard mirror surface polyurethane wet bass and preparation method thereof |
| CN109853254B (en) * | 2019-02-28 | 2021-08-03 | 扬州工业职业技术学院 | Medium-hard mirror polyurethane wet base and preparation method thereof |
| CN110437410A (en) * | 2019-08-08 | 2019-11-12 | 合肥安利聚氨酯新材料有限公司 | A kind of soft easy embossing wet polyurethane resin of polyether-type and preparation method thereof |
| CN115260440A (en) * | 2022-08-16 | 2022-11-01 | 江苏华大新材料有限公司 | Polyurethane resin for wet-process embossing synthetic leather and preparation method thereof |
| CN115260440B (en) * | 2022-08-16 | 2023-09-12 | 江苏华大新材料有限公司 | Polyurethane resin for wet embossing synthetic leather and preparation method thereof |
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