CN101117374A - Preparation method of urethane elastomer - Google Patents
Preparation method of urethane elastomer Download PDFInfo
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- CN101117374A CN101117374A CNA2007100618273A CN200710061827A CN101117374A CN 101117374 A CN101117374 A CN 101117374A CN A2007100618273 A CNA2007100618273 A CN A2007100618273A CN 200710061827 A CN200710061827 A CN 200710061827A CN 101117374 A CN101117374 A CN 101117374A
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Abstract
A method of producing polyurethane elastomer is to dehydrate hydroxy-terminated polybutadiene and tetrahydrofuran in vacuum, which are then cooled to 20 to 50 DEG C and added to the melting dimethyl-methane isocyanate (MDI) according to the mole ratio of hydroxyl to isocyanates being 1:1-2. The reaction lasts for one to five hours under 80 to 120 DEG C and a prepolymer is obtained. While beating up, the temperature is heated up to 90 to 120 DEG C, 1, 4-Butanediol is added to the prepolymer under fast mixing for one or three minutes, and poured into warm-up flat mould coated with demolding agent and become hard set, 1-10MPa is added for solidification and demolding, and then polyurethane can be obtained from sulfuration under 110-140 DEG C for 18 to 24 hours. The polyurethane elastomer of the present invention has the advantages of good anti-corrosion, abrasion resistance and good mechanical performance.
Description
Technical field
The present invention relates to a kind of synthetic method for preparing polyurethane elastomer, be specifically related to hydroxy-terminated polybutadienes (HTPB), polytetrahydrofuran (PTMG), '-diphenylmethane diisocyanate (MDI) and 1, the method for 4-butyleneglycol (BDO) prepared in reaction polyurethane elastomer.
Technical background
General polyurethane series is reacted by polynary organic isocyanate and polyol compound and makes.From structure, the polyurethane macromolecular main chain is to be formed by the rigid chain segment block that subambient soft segment of second-order transition temperature and second-order transition temperature are higher than room temperature.Can synthesize the different polyurethane elastomer of composition, structure and performance according to the different of raw materials used kind and ratio.Hydroxy-terminated polybutadienes is a kind of new type functional polymkeric substance that grows up the nineties in 20th century, the polyurethane elastomer that is made by HTPB is with the tensile strength height, wear resistance is good, the bonding strength height, charge capacity is big, and is corrosion-resistant, performances such as anti-ozone and be widely used in elastomerics, the aspects such as material, electrical device pouring sealant that discharge water, but its mechanical property is not as good as the polyether-type and the PAUR elastomerics of equal hard segment content.
Summary of the invention
The purpose of this invention is to provide a kind of mechanical property good usefulness hydroxy-terminated polybutadienes (HTPB), polytetrahydrofuran (PTMG), '-diphenylmethane diisocyanate (MDI) and 1, the method for 4-butyleneglycol (BDO) prepared in reaction polyurethane elastomer.
Is 1 by hydroxy-terminated polybutadienes (HTPB) with polytetrahydrofuran (PTMG) mass ratio: 0.01-100, be preferably 1: 0.1-10, with hydroxy-terminated polybutadienes (HTPB) and polytetrahydrofuran (PTMG) at 100 ℃ of-120 ℃ of following vacuum hydro-extraction 1-3h, be cooled to 20-50 ℃ of temperature then, the mol ratio of pressing hydroxyl and isocyanic ester 1: 1-2 adds the '-diphenylmethane diisocyanate of fusing, insulation reaction 1-5h under 80 ℃ of-120 ℃ of temperature obtains performed polymer.
Press the isocyanic ester and 1 of performed polymer, the molar ratio of the hydroxyl of 4-butyleneglycol (BDO) is 1: 1-5, heat temperature raising to 90 while stirring ℃-120 ℃, with 1,4-butyleneglycol (BDO) joins in the performed polymer under stirring fast, stirs rapidly 1-3 minute, is poured into preheating and scribbles in the flat plate mold of remover to reach when solidifying, pressurization 1-10MPa curing and demolding promptly gets polyurethane elastomer at 110-140 ℃ of sulfuration 18-24h.
The present invention has following advantage compared with the prior art:
The polyurethane elastomer of gained is existing good corrosion-resistant, and performance such as wear-resisting has the good mechanical performance again.
Embodiment
Embodiment 1
With mass ratio is that 1: 0.1 HTPB and PTMG add in the four-hole boiling flask, at 100 ℃ of following vacuum hydro-extraction 3h, be cooled to 50 ℃ then, the '-diphenylmethane diisocyanate of fusing is added rapidly under stirring fast, the hydroxyl in the system and the mol ratio of isocyanic ester are 1: 1.2,80 ℃ of following insulation reaction 5h, sampling analysis NCO content, airtight preservation is stand-by.
Take by weighing a certain amount of performed polymer, heat temperature raising to 90 ℃ temperature while stirring, molar ratio by the hydroxyl of the isocyanic ester of performed polymer and BDO is 1: 1, BDO is added in the performed polymer under stirring fast, stir rapidly 1min, be poured into preheating and scribble in the flat plate mold of remover, wait to reach when solidifying, pressurization 10MPa curing and demolding, and 110 ℃ of sulfuration 24h promptly get required elastomerics test piece in loft drier.The tensile strength of gained test piece is 30MPa, and tensile yield is 450%, and tear strength is 70KNm
-1
Embodiment 2
With mass ratio is that 1: 1 HTPB and PTMG add in the four-hole boiling flask, at 110 ℃ of following vacuum hydro-extraction 2h, be cooled to 30 ℃ then, the '-diphenylmethane diisocyanate of fusing is added rapidly under stirring fast, the hydroxyl in the system and the mol ratio of isocyanic ester are 1: 1.5,100 ℃ of following insulation reaction 3h, sampling analysis NCO content, airtight preservation is stand-by.
Take by weighing a certain amount of performed polymer, heat temperature raising is to certain temperature while stirring, heat temperature raising to 105 ℃ temperature while stirring, molar ratio by the hydroxyl of the isocyanic ester of performed polymer and BDO is 1: 1.5, and BDO is added in the performed polymer under stirring fast, stirs 2min rapidly, be poured into preheating and scribble in the flat plate mold of remover, wait to reach when solidifying, pressurization 5MPa curing and demolding, and 130 ℃ of sulfuration 20h promptly get required elastomerics test piece in loft drier.The tensile strength of gained test piece is 23MPa, and tensile yield is 380%, and tear strength is 60KNm
-1
Embodiment 3
With mass ratio is that 1: 10 HTPB and PTMG add in the four-hole boiling flask, at 120 ℃ of following vacuum hydro-extraction 1h, be cooled to 20 ℃ then, the '-diphenylmethane diisocyanate of fusing is added rapidly under stirring fast, the hydroxyl in the system and the mol ratio of isocyanic ester are 1: 2,120 ℃ of following insulation reaction 1h, sampling analysis NCO content, airtight preservation is stand-by.
Take by weighing a certain amount of performed polymer, heat temperature raising to 120 ℃ temperature while stirring, molar ratio by the hydroxyl of the isocyanic ester of performed polymer and BDO is 1: 2, BDO is added in the performed polymer under stirring fast, stir rapidly 3min, be poured into preheating and scribble in the flat plate mold of remover, wait to reach when solidifying, pressurization 1MPa curing and demolding, and 140 ℃ of sulfuration 18h promptly get required elastomerics test piece in loft drier.The tensile strength of gained test piece is 20MPa, and tensile yield is 200%, and tear strength is 30KNm
-1
Embodiment 4
With mass ratio is that 1: 100 HTPB and PTMG add in the four-hole boiling flask, at 115 ℃ of following vacuum hydro-extraction 1.5h, be cooled to 35 ℃ then, the '-diphenylmethane diisocyanate of fusing is added rapidly under stirring fast, the hydroxyl in the system and the mol ratio of isocyanic ester are 1: 1.5,115 ℃ of following insulation reaction 1.5h, sampling analysis NCO content, airtight preservation is stand-by.
Take by weighing a certain amount of performed polymer, heat temperature raising to 120 ℃ temperature while stirring, molar ratio by the hydroxyl of the isocyanic ester of performed polymer and BDO is 1: 2, BDO is added in the performed polymer under stirring fast, stir rapidly 3min, be poured into preheating and scribble in the flat plate mold of remover, wait to reach when solidifying, pressurization 1MPa curing and demolding, and 140 ℃ of sulfuration 18h promptly get required elastomerics test piece in loft drier.The tensile strength of gained test piece is 25MPa, and tensile yield is 300%, and tear strength is 40KNm
-1
Claims (2)
1. a method for preparing polyurethane elastic body is characterized in that comprising the steps:
By hydroxy-terminated polybutadienes and polytetrahydrofuran mass ratio is 1: 0.01-100, be preferably 1: 0.1-10, with hydroxy-terminated polybutadienes and polytetrahydrofuran at 100 ℃ of-120 ℃ of following vacuum hydro-extraction 1-3h, be cooled to 20-50 ℃ of temperature then, the mol ratio of pressing hydroxyl and isocyanic ester 1: 1-2 adds the '-diphenylmethane diisocyanate of fusing, insulation reaction 1-5h under 80 ℃ of-120 ℃ of temperature obtains performed polymer.
Press the isocyanic ester and 1 of performed polymer, the molar ratio of the hydroxyl of 4-butyleneglycol is 1: 1-5, heat temperature raising to 90 while stirring ℃-120 ℃, with 1, the 4-butyleneglycol joins in the performed polymer under stirring fast, stirs rapidly 1-3 minute, is poured into preheating and scribbles in the flat plate mold of remover to reach when solidifying, pressurization 1-10MPa curing and demolding promptly gets polyurethane elastomer at 110-140 ℃ of sulfuration 18-24h.
2. a kind of method for preparing polyurethane elastic body as claimed in claim 1 is characterized in that described hydroxy-terminated polybutadienes and polytetrahydrofuran mass ratio are 1: 0.1-10.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100618273A CN101117374A (en) | 2007-04-30 | 2007-04-30 | Preparation method of urethane elastomer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100618273A CN101117374A (en) | 2007-04-30 | 2007-04-30 | Preparation method of urethane elastomer |
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| CN101117374A true CN101117374A (en) | 2008-02-06 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101480582B (en) * | 2008-12-25 | 2012-06-13 | 浙江大学 | Method for preparing polyurethane film based on hydroxy-terminated polybutadiene |
| CN103665303A (en) * | 2013-11-30 | 2014-03-26 | 山东永泰化工有限公司 | Preparation method of waterproof cellular polyurethane elastomer |
| CN105837781A (en) * | 2016-04-19 | 2016-08-10 | 滁州环球聚氨酯科技有限公司 | High-strength polyurethane composite material |
| CN107446342A (en) * | 2017-06-30 | 2017-12-08 | 苏州奥斯汀新材料科技有限公司 | A kind of preparation method of low temperature-resistant thermoplastic polyurethane elastomer film |
| CN108893096A (en) * | 2018-06-12 | 2018-11-27 | 陕西纤润调温材料研究开发有限公司 | A kind of hairless protein microcapsules of storing energy through phase change slurry and the preparation method and application thereof |
| CN111057208A (en) * | 2019-12-17 | 2020-04-24 | 上海汇得科技股份有限公司 | Polyolefin polyol modified thermoplastic polyurethane elastomer and preparation method thereof |
| CN112126034A (en) * | 2019-06-24 | 2020-12-25 | 北京化工大学 | Mixed soft segment type polyurethane damping material and preparation method thereof |
| CN115124678A (en) * | 2022-07-03 | 2022-09-30 | 郑州大学 | High-strength polyurethane elastomer and preparation method thereof |
| CN117542641A (en) * | 2023-11-08 | 2024-02-09 | 江苏普隆磁电有限公司 | Preparation method of heat-resistant NdFeB magnet |
-
2007
- 2007-04-30 CN CNA2007100618273A patent/CN101117374A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101480582B (en) * | 2008-12-25 | 2012-06-13 | 浙江大学 | Method for preparing polyurethane film based on hydroxy-terminated polybutadiene |
| CN103665303A (en) * | 2013-11-30 | 2014-03-26 | 山东永泰化工有限公司 | Preparation method of waterproof cellular polyurethane elastomer |
| CN105837781A (en) * | 2016-04-19 | 2016-08-10 | 滁州环球聚氨酯科技有限公司 | High-strength polyurethane composite material |
| CN107446342A (en) * | 2017-06-30 | 2017-12-08 | 苏州奥斯汀新材料科技有限公司 | A kind of preparation method of low temperature-resistant thermoplastic polyurethane elastomer film |
| CN108893096A (en) * | 2018-06-12 | 2018-11-27 | 陕西纤润调温材料研究开发有限公司 | A kind of hairless protein microcapsules of storing energy through phase change slurry and the preparation method and application thereof |
| CN112126034A (en) * | 2019-06-24 | 2020-12-25 | 北京化工大学 | Mixed soft segment type polyurethane damping material and preparation method thereof |
| CN112126034B (en) * | 2019-06-24 | 2022-05-17 | 北京化工大学 | Mixed soft segment type polyurethane damping material and preparation method thereof |
| CN111057208A (en) * | 2019-12-17 | 2020-04-24 | 上海汇得科技股份有限公司 | Polyolefin polyol modified thermoplastic polyurethane elastomer and preparation method thereof |
| CN115124678A (en) * | 2022-07-03 | 2022-09-30 | 郑州大学 | High-strength polyurethane elastomer and preparation method thereof |
| CN117542641A (en) * | 2023-11-08 | 2024-02-09 | 江苏普隆磁电有限公司 | Preparation method of heat-resistant NdFeB magnet |
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