CN101735597A - Resin for polyurethane shoe with extremely-low density and high hardness and preparation method thereof - Google Patents
Resin for polyurethane shoe with extremely-low density and high hardness and preparation method thereof Download PDFInfo
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- CN101735597A CN101735597A CN200910232336A CN200910232336A CN101735597A CN 101735597 A CN101735597 A CN 101735597A CN 200910232336 A CN200910232336 A CN 200910232336A CN 200910232336 A CN200910232336 A CN 200910232336A CN 101735597 A CN101735597 A CN 101735597A
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Abstract
The invention relates to resin for a polyurethane shoe with extremely-low density and high hardness and a preparation method thereof, belonging to the chemical field. The resin is prepared by foaming a component A and a component B at a certain condition through a polyurethane foaming machine and injecting the mixture into a shoe mold. The component A is formed by mixing polyalcohol A1, polymer of polyester polyol A2, a cross-linking agent, a polyesterdiol chain extender, a catalyst, an organic silicon foam stabilizer, a water foaming agent and the like; and the component B is a prepolymer prepared by reacting polyisocyanates, polyester polyol B1 and polyether polyol B2. The invention has the advantages of maintaining higher hardness of products at lower density and greatly reducing the productions cost of production manufacturers of the polyster type polyurethane shoe. In addition, the invention has easily-obtained raw material, favorable repeatability of products and capability of realizing batch production.
Description
Technical field
The present invention relates to a kind of resin for polyurethane shoe with extremely-low density and high hardness and preparation method, belong to chemical field.
Background technology
Owing to have light wear-resisting, good springiness, the constantly end, characteristics such as anti-skidding, grease proofing, comfortable and easy to wear, more and more be subjected to the human consumer and welcome at the bottom of the polyurethane shoe.There is in the world maximum shoemaking industry in China, produces 7,000,000,000 pairs of footwear altogether in 2003, accounts for the output in the whole world 50%, and China's footwear in 2006 already export and just reach 7,800,000,000 pairs, estimates will produce 9,000,000,000 pairs of footwear in 2010.Material for shoes mainly contains leather, rubber, polyvinyl chloride (PVC), ethylene vinyl acetate (EVA), styrene butadiene styrene (SBS) and Polyurethane Thermoplastic Elastomer (TPU) etc. at present.China's polyurethane stock solution market is subjected to the influence to Chinese footwear Antidumping incident of cost of material and European Union in recent years, slowed down rate of growth, proportion is less than 6% at the bottom of the present polyurethane shoe, and account for the market share more than 50% at the bottom of developed country's polyurethane shoe, therefore the market space at the bottom of China's polyurethane shoe is still very big, the polyurethane shoe material accounts for 80% based on polyester polyol on the market.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of resin for polyurethane shoe with extremely-low density and high hardness and preparation method are provided, solve the polyurethane polyester sole and under low density situation, still can keep the very technical barrier of high rigidity.
According to technical scheme provided by the invention, described resin for polyurethane shoe with extremely-low density and high hardness comprises A component and B component, it is characterized in that:
The A component comprises: 20～80% polyester polyol A1,20～80% polymer polyester polyol A2, and unit is a weight percentage; Also comprise 0.1～0.8% linking agent, 5～40% dibasic alcohol chainextender, 1～3% catalyzer, 0.3～1.2% organosilicon foam stabilizer, 1～2% water, unit is the weight percentage that accounts for polyester polyol A1 and polymer polyester polyol A2 throwing amount always;
Described polyester polyol A1 is that one or more materials of ethylene glycol, Diethylene Glycol, 1,4 butyleneglycol, 1,3 butyleneglycol, 1,3 propylene glycol and trihydroxy methyl propane and molecular weight that hexanodioic acid makes by transesterification reaction are 1500～1850 polyester polyol;
To be one or more materials in vinylbenzene, vinyl cyanide, the methyl methacrylate and polyester polyol A1 make by radical polymerization described polymer polyester polyol A2 is that 1000～5000mpas, solid content are 20～40% polymer polyester polyol 40 ℃ of following viscosity;
The B component comprises: 50～80% polyisocyanates, 15～40% polyester polyols ester B1,1～20% polyether glycol B2; Unit is a weight percentage.
Described dibasic alcohol chainextender is one or more materials in ethylene glycol, Diethylene Glycol, 1,4 butyleneglycol, 1,3 propylene glycol.
Described linking agent is one or more materials in TriMethylolPropane(TMP), glycerol, diethanolamine, the trolamine.
Described catalyzer is a tertiary amine catalyst; Described organosilicon foam stabilizer is the organic silicon modified by polyether tensio-active agent.
Described polyisocyanates is 4,4 '-diphenylmethanediisocyanate, tolylene diisocyanate, carbodiimide modification 4,4 '-one or more materials in the diphenylmethanediisocyanate.
Described polyester polyol B1 is that molecular weight that one or more materials in ethylene glycol, Diethylene Glycol, 1,4 butyleneglycol, 1,3 propylene glycol and hexanodioic acid make by transesterification reaction is 2000～2500 polyester polyol.
Described polyether glycol B2 is that functionality is 2～3, and molecular weight is 3000～5000 polyether glycol.
The method for preparing resin for polyurethane shoe with extremely-low density and high hardness:
A component preparation: at normal temperatures nitrogen is fed in the reactor, add polyester polyol A1, polymer polyester polyol A2, dibasic alcohol chainextender, linking agent, organosilicon foam stabilizer, catalyzer and water in the reactor successively, keeping temperature of reaction kettle is 50～65 ℃, stir discharging behind 3～5 hours thorough mixing, sealing is preserved, and makes the A component;
B component preparation: in 50～60 ℃ reactor, feed nitrogen, earlier polyisocyanates is dropped in the reactor, again polyester polyol B1, polyether glycol B2 are divided in 3～4 adding reactors, keeping temperature of reaction kettle is 65～75 ℃, reacts 3～5 hours, after the sampling detection is qualified, be cooled to 40～50 ℃, discharging feeds nitrogen-sealed and preserves, and makes the B component.
The method of utilizing resin for polyurethane shoe with extremely-low density and high hardness to make sole is: A component and B component are foamed on polyurethane foaming machine, inject the footwear mould, the demoulding makes polyurethane product after 3～5 minutes, and footwear mould temperature is 50～60 ℃, and the temperature of A component, B component is 40～42 ℃.
The compact density of described polyurethane resin for shoes is 0.20～0.38g/cm
3, hardness is Shao Shi A 55～97.
The invention has the advantages that product greatly reduces the production cost of PAUR shoe sole production producer than keeping higher hardness under the low density.Raw material is easy to get, technology simple, good repetitiveness, can realize producing in batches.
Embodiment
The invention will be further described below in conjunction with specific embodiment.
It is the polyether glycol of TED28 that polyether glycol B2 selects the trade mark of Tianjin three petrochemical iy produced for use.
The A33 that catalyzer selects for use U.S.'s gas companies to produce.
The Niax*L-1505 that the organosilicon foam stabilizer selects for use U.S. Mai Tu company to produce.
Table 1 is the consumption of each component among embodiment 1～embodiment 7:
Table 1
Example 1: a kind of resin for polyurethane shoe with extremely-low density and high hardness and preparation method
A component preparation: at normal temperatures nitrogen is fed in the reactor, add polyester polyol A1, polymer polyester polyol A2, dibasic alcohol chainextender, linking agent, organosilicon foam stabilizer, catalyzer, water in the reactor successively, keeping temperature of reaction kettle is 50 ℃, stir discharging behind 5 hours thorough mixing, sealing is preserved, and makes the A component;
B component preparation: in 50 ℃ reactor, feed nitrogen, earlier polyisocyanates is dropped in the reactor, again polyester polyol B1, polyether glycol B2 are divided in 3 adding reactors, keeping temperature of reaction kettle is 65 ℃, reacts 5 hours, after the sampling detection is qualified, be cooled to 50 ℃, discharging feeds nitrogen-sealed and preserves, and makes the B component.
A component and B component are foamed on polyurethane foaming machine, inject the footwear mould, the demoulding makes polyurethane product after 3 minutes, and footwear mould temperature is 50 ℃, and the temperature of A component, B component is 40 ℃.The polyurethane resin for shoes compact density is 0.316g/cm
3, hardness is Shao Shi A60, shrinkage strain does not appear in flat appearance, but material flowability is poor, easily causes the goods part not in place.
Example 2: a kind of resin for polyurethane shoe with extremely-low density and high hardness and preparation method
A component preparation: at normal temperatures nitrogen is fed in the reactor, add polyester polyol A1, polymer polyester polyol A2, dibasic alcohol chainextender, linking agent, organosilicon foam stabilizer, catalyzer, water in the reactor successively, keeping temperature of reaction kettle is 65 ℃, stir discharging behind 3 hours thorough mixing, sealing is preserved, and makes the A component;
B component preparation: in 60 ℃ reactor, feed nitrogen, earlier polyisocyanates is dropped in the reactor, again polyester polyol B1, polyether glycol B2 are divided in 4 adding reactors, keeping temperature of reaction kettle is 75 ℃, reacts 3 hours, after the sampling detection is qualified, be cooled to 50 ℃, discharging feeds nitrogen-sealed and preserves, and makes the B component.
A component and B component are foamed on polyurethane foaming machine, inject the footwear mould, the demoulding makes polyurethane product after 5 minutes, and footwear mould temperature is 60 ℃, and the temperature of A component, B component is 42 ℃.The polyurethane resin for shoes compact density is 0.303g/cm
3, hardness is Shao Shi A63, shrinkage strain does not appear in flat appearance.
Example 3: a kind of resin for polyurethane shoe with extremely-low density and high hardness and preparation method
A component preparation: at normal temperatures nitrogen is fed in the reactor, add polyester polyol A1, polymer polyester polyol A2, dibasic alcohol chainextender, linking agent, organosilicon foam stabilizer, catalyzer, water in the reactor successively, keeping temperature of reaction kettle is 60 ℃, stir discharging behind 4 hours thorough mixing, sealing is preserved, and makes the A component;
B component preparation: in 55 ℃ reactor, feed nitrogen, earlier polyisocyanates is dropped in the reactor, again polyester polyol B1, polyether glycol B2 are divided in 3 adding reactors, keeping temperature of reaction kettle is 70 ℃, reacts 4 hours, after the sampling detection is qualified, be cooled to 45 ℃, discharging feeds nitrogen-sealed and preserves, and makes the B component.
A component and B component are foamed on polyurethane foaming machine, inject the footwear mould, the demoulding makes polyurethane product after 4 minutes, and footwear mould temperature is 55 ℃, and the temperature of A component, B component is 41 ℃.The polyurethane resin for shoes compact density is 0.299g/cm
3, hardness is Shao Shi A72, shrinkage strain does not appear in flat appearance.
Example 4: a kind of resin for polyurethane shoe with extremely-low density and high hardness and preparation method
Processing condition are with embodiment 1, and the polyurethane resin for shoes compact density is 0.294g/cm
3, hardness is Shao Shi A78, shrinkage strain does not appear in flat appearance.
Example 5: a kind of resin for polyurethane shoe with extremely-low density and high hardness and preparation method
Processing condition are with embodiment 2, and the polyurethane resin for shoes compact density is 0.286g/cm
3, hardness is Shao Shi A85, shrinkage strain does not appear in flat appearance.
Example 6: a kind of resin for polyurethane shoe with extremely-low density and high hardness and preparation method
Processing condition are with embodiment 3, and the polyurethane resin for shoes compact density is 0.278g/cm
3, hardness is Shao Shi A92, shrinkage strain does not appear in flat appearance.
Example 7: a kind of resin for polyurethane shoe with extremely-low density and high hardness and preparation method
Processing condition are with embodiment 3, and the polyurethane resin for shoes compact density is 0.256g/cm
3, hardness is Shao Shi A97, shrinkage strain does not appear in flat appearance.
Claims (10)
1. a resin for polyurethane shoe with extremely-low density and high hardness comprises A component and B component, it is characterized in that:
The A component comprises: 20～80% polyester polyol A1,20～80% polymer polyester polyol A2, and unit is a weight percentage; Also comprise 0.1～0.8% linking agent, 5～40% dibasic alcohol chainextender, 1～3% catalyzer, 0.3～1.2% organosilicon foam stabilizer, 1～2% water, unit is the weight percentage that accounts for polyester polyol A1 and polymer polyester polyol A2 throwing amount always;
Described polyester polyol A1 is that one or more materials of ethylene glycol, Diethylene Glycol, 1,4 butyleneglycol, 1,3 butyleneglycol, 1,3 propylene glycol and trihydroxy methyl propane and molecular weight that hexanodioic acid makes by transesterification reaction are 1500～1850 polyester polyol;
To be one or more materials in vinylbenzene, vinyl cyanide, the methyl methacrylate and polyester polyol A1 make by radical polymerization described polymer polyester polyol A2 is that 1000～5000mpas, solid content are 20～40% polymer polyester polyol 40 ℃ of following viscosity;
The B component comprises: 50～80% polyisocyanates, 15～40% polyester polyols ester B1,1～20% polyether glycol B2; Unit is a weight percentage.
2. resin for polyurethane shoe with extremely-low density and high hardness as claimed in claim 1 is characterized in that, described dibasic alcohol chainextender is one or more materials in ethylene glycol, Diethylene Glycol, 1,4 butyleneglycol, 1,3 propylene glycol.
3. resin for polyurethane shoe with extremely-low density and high hardness as claimed in claim 1 is characterized in that, described linking agent is one or more materials in TriMethylolPropane(TMP), glycerol, diethanolamine, the trolamine.
4. resin for polyurethane shoe with extremely-low density and high hardness as claimed in claim 1 is characterized in that, described catalyzer is a tertiary amine catalyst; Described organosilicon foam stabilizer is the organic silicon modified by polyether tensio-active agent.
5. resin for polyurethane shoe with extremely-low density and high hardness as claimed in claim 1, it is characterized in that, described polyisocyanates is 4,4 '-diphenylmethanediisocyanate, tolylene diisocyanate, carbodiimide modification 4,4 '-one or more materials in the diphenylmethanediisocyanate.
6. resin for polyurethane shoe with extremely-low density and high hardness as claimed in claim 1, it is characterized in that, described polyester polyol B1 is ethylene glycol, Diethylene Glycol, 1, the molecular weight that one or more materials in 4 butyleneglycols, 1,3 propylene glycol and hexanodioic acid make by transesterification reaction is 2000～2500 polyester polyol.
7. resin for polyurethane shoe with extremely-low density and high hardness as claimed in claim 1 is characterized in that, described polyether glycol B2 is that functionality is 2～3, and molecular weight is 3000～5000 polyether glycol.
8. prepare the method for the described resin for polyurethane shoe with extremely-low density and high hardness of claim 1, it is characterized in that:
A component preparation: at normal temperatures nitrogen is fed in the reactor, add polyester polyol A1, polymer polyester polyol A2, dibasic alcohol chainextender, linking agent, organosilicon foam stabilizer, catalyzer and water in the reactor successively, keeping temperature of reaction kettle is 50～65 ℃, stir discharging behind 3～5 hours thorough mixing, sealing is preserved, and makes the A component;
B component preparation: in 50～60 ℃ reactor, feed nitrogen, earlier polyisocyanates is dropped in the reactor, again polyester polyol B1, polyether glycol B2 are divided in 3～4 adding reactors, keeping temperature of reaction kettle is 65～75 ℃, reacts 3～5 hours, after the sampling detection is qualified, be cooled to 40～50 ℃, discharging feeds nitrogen-sealed and preserves, and makes the B component.
9. the method for utilizing the described resin for polyurethane shoe with extremely-low density and high hardness of claim 1 to make sole, it is characterized in that: A component and B component are foamed on polyurethane foaming machine, inject the footwear mould, the demoulding makes polyurethane product after 3～5 minutes, footwear mould temperature is 50～60 ℃, and the temperature of A component, B component is 40～42 ℃.
10. method as claimed in claim 9 is characterized in that: the compact density of described polyurethane resin for shoes is 0.20～0.38g/cm
3, hardness is Shao Shi A 55～97.
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| CN200910232336A CN101735597A (en) | 2009-12-07 | 2009-12-07 | Resin for polyurethane shoe with extremely-low density and high hardness and preparation method thereof |
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| CN102492286A (en) * | 2011-12-09 | 2012-06-13 | 方夺棉 | Wood chip-containing polyurethane shoe material and preparation method thereof |
| CN102504181A (en) * | 2011-09-30 | 2012-06-20 | 无锡双象化学工业有限公司 | Resin used for polyurethane cold-resistant flexible middle/low-density shoes and preparation method thereof |
| CN102898608A (en) * | 2012-09-24 | 2013-01-30 | 吴江市信许塑料鞋用配套有限公司 | Preparation method of ultra-light foamed sole material |
| CN104262584A (en) * | 2014-09-22 | 2015-01-07 | 东莞市吉鑫高分子科技有限公司 | Thermoplastic polyurethane elastomer for shoe printing material and preparation method of thermoplastic polyurethane elastomer |
| CN104479091A (en) * | 2014-11-19 | 2015-04-01 | 嘉兴禾欣化学工业有限公司 | Low-density high-hardness polyurethane sole material and preparation method thereof |
| CN104497254A (en) * | 2014-12-25 | 2015-04-08 | 合肥华凌股份有限公司 | Composition, hard polyurethane foam material and refrigerating equipment |
| WO2015062960A1 (en) * | 2013-10-28 | 2015-05-07 | Basf Se | Low density polyurethane microcellular elastomer |
| CN105111405A (en) * | 2015-07-27 | 2015-12-02 | 江苏欣润塑胶有限公司 | Cold-resistant soft middle/low density polyurethane resin |
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| CN106188469A (en) * | 2016-07-21 | 2016-12-07 | 山东诺威聚氨酯股份有限公司 | With polyurethane shoe-sole and preparation method thereof at the bottom of Low-density environmentally-friefloor type foot-high shoes |
| CN106263270A (en) * | 2016-08-22 | 2017-01-04 | 温州盈泰鞋业股份有限公司 | The formula of a kind of polyethers perforate Novel shoe pad and processing technology thereof |
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| CN112029220A (en) * | 2020-08-18 | 2020-12-04 | 温州金鸿远鞋业有限公司 | Wear-resistant women's shoes and preparation method thereof |
| CN115477737A (en) * | 2022-11-02 | 2022-12-16 | 山东一诺威聚氨酯股份有限公司 | Hydrolysis-resistant and flex-resistant polyurethane sole resin composition and preparation and application thereof |
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2009
- 2009-12-07 CN CN200910232336A patent/CN101735597A/en active Pending
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| CN102492286A (en) * | 2011-12-09 | 2012-06-13 | 方夺棉 | Wood chip-containing polyurethane shoe material and preparation method thereof |
| CN102898608A (en) * | 2012-09-24 | 2013-01-30 | 吴江市信许塑料鞋用配套有限公司 | Preparation method of ultra-light foamed sole material |
| KR102262243B1 (en) | 2013-10-28 | 2021-06-09 | 바스프 에스이 | Low density polyurethane microcellular elastomer |
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| CN105683236A (en) * | 2013-10-28 | 2016-06-15 | 巴斯夫欧洲公司 | Low density polyurethane microcellular elastomer |
| KR20160079842A (en) * | 2013-10-28 | 2016-07-06 | 바스프 에스이 | Low density polyurethane microcellular elastomer |
| EP3063201B1 (en) | 2013-10-28 | 2017-12-13 | Basf Se | Low density polyurethane microcellular elastomer |
| CN104262584A (en) * | 2014-09-22 | 2015-01-07 | 东莞市吉鑫高分子科技有限公司 | Thermoplastic polyurethane elastomer for shoe printing material and preparation method of thermoplastic polyurethane elastomer |
| CN104479091A (en) * | 2014-11-19 | 2015-04-01 | 嘉兴禾欣化学工业有限公司 | Low-density high-hardness polyurethane sole material and preparation method thereof |
| CN104497254B (en) * | 2014-12-25 | 2017-07-18 | 合肥华凌股份有限公司 | Composition, rigid polyurethane foam and refrigeration plant |
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| CN105111405A (en) * | 2015-07-27 | 2015-12-02 | 江苏欣润塑胶有限公司 | Cold-resistant soft middle/low density polyurethane resin |
| CN105747358A (en) * | 2016-04-26 | 2016-07-13 | 彭伟成 | Safety shoe |
| CN106188469B (en) * | 2016-07-21 | 2019-06-18 | 山东一诺威聚氨酯股份有限公司 | Low-density environmentally-friefloor type foot-high shoes bottom polyurethane shoe-sole and preparation method thereof |
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| CN106263270A (en) * | 2016-08-22 | 2017-01-04 | 温州盈泰鞋业股份有限公司 | The formula of a kind of polyethers perforate Novel shoe pad and processing technology thereof |
| CN108409934A (en) * | 2018-03-09 | 2018-08-17 | 旭川化学（昆山）有限公司 | Height rebound Low temperature-resistanpolyurethane polyurethane sole raw material and preparation method thereof |
| CN109730394A (en) * | 2019-01-29 | 2019-05-10 | 佛山市南海起弘新材料科技有限公司 | A kind of shoes and its preparation process with integral type waterproof layer |
| CN110144111A (en) * | 2019-04-15 | 2019-08-20 | 泉州邦尼生物科技有限公司 | A kind of lightweight adds numb polyurethane shoe-sole and preparation method thereof |
| CN110643014A (en) * | 2019-06-04 | 2020-01-03 | 福建小爱科技有限公司 | Production and manufacturing process method of polyurethane insole |
| CN111138624A (en) * | 2019-12-16 | 2020-05-12 | 旭川化学（苏州）有限公司 | Polyurethane resin for high-physical-property breathable insole and preparation method thereof |
| CN112029220A (en) * | 2020-08-18 | 2020-12-04 | 温州金鸿远鞋业有限公司 | Wear-resistant women's shoes and preparation method thereof |
| CN115477737A (en) * | 2022-11-02 | 2022-12-16 | 山东一诺威聚氨酯股份有限公司 | Hydrolysis-resistant and flex-resistant polyurethane sole resin composition and preparation and application thereof |
| CN117106154A (en) * | 2023-10-25 | 2023-11-24 | 山东一诺威聚氨酯股份有限公司 | Low-temperature-resistant and dirt-resistant polyurethane sole resin and preparation method and application thereof |
| CN117106154B (en) * | 2023-10-25 | 2024-03-08 | 山东一诺威聚氨酯股份有限公司 | Low-temperature-resistant and dirt-resistant polyurethane sole resin and preparation method and application thereof |
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Application publication date: 20100616 |