CN104004153A - Method for manufacturing acid and alkali resistant thermoplastic polyurethane elastomer - Google Patents
Method for manufacturing acid and alkali resistant thermoplastic polyurethane elastomer Download PDFInfo
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- CN104004153A CN104004153A CN201410264654.5A CN201410264654A CN104004153A CN 104004153 A CN104004153 A CN 104004153A CN 201410264654 A CN201410264654 A CN 201410264654A CN 104004153 A CN104004153 A CN 104004153A
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- Prior art keywords
- acid
- thermoplastic polyurethane
- polyurethane elastomer
- alkali
- silicon oil
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/67—Unsaturated compounds having active hydrogen
- C08G18/69—Polymers of conjugated dienes
- C08G18/698—Mixtures with compounds of group C08G18/40
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/61—Polysiloxanes
Abstract
The invention discloses a method for manufacturing an acid and alkali resistant thermoplastic polyurethane elastomer. The method includes the steps that (1), hydroxyl-terminated polybutadiene, polyether polyol, catalysts and a small amount of diisocyanate are added into a reaction still to be stirred evenly, amino silicon oil is added dropwise, diisocyanate is replenished after adding of the amino silicon oil is finished, the ratio of the molar content of isocyanate root ions in a system to the sum of the molar content of amidogen and the molar content of hydroxy is (2-3):1, and an amino silicon oil modified polyurethane prepolymer is obtained through warming reaction; (2), a chain extender is heated to be 50-80 DEG C to be blended with the amino silicon oil modified polyurethane prepolymer in the step (1), and a thermoplastic polyurethane elastomer is obtained through stirring; (3), the thermoplastic polyurethane elastomer obtained in the step (2) is heated and dried under the vacuum condition, and then the acid and alkali resistant thermoplastic polyurethane elastomer is obtained. The acid and alkali resistant thermoplastic polyurethane elastomer manufactured according to the method is mainly used for rubber rollers and paving materials of the papermaking industry, caulking materials and repairing materials under the bad condition, and the like.
Description
Technical field
The present invention relates to a kind of method for preparing thermoplastic polyurethane elastomer, relate in particular to a kind of acid and alkali-resistance method for preparing thermoplastic polyurethane elastomer.
Background technology
Polyurethane Thermoplastic Elastomer (being called again TPU) novel material is called as " epoch-making novel high polymer material ", is one of our times six synthetic materials greatly with development prospect.
The corrosion resistance nature of research polyurethane elastomer, the ph stability of raising polyurethane material, no matter the life-span of prolongation polyurethane material and goods is to society or polyurethane industrial, all has very important significance.
Summary of the invention
Technical problem to be solved by this invention is: provide a kind of in strong acid or highly basic strength retention high, the acid and alkali-resistance method for preparing thermoplastic polyurethane elastomer that the rate of decay is slow.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of acid and alkali-resistance method for preparing thermoplastic polyurethane elastomer, the steps include:
1) in reactor, add hydroxy-terminated polybutadienes (HTPB), polyether glycol, catalyzer and account for hydroxy-terminated polybutadienes and the vulcabond of polyether glycol total mass 0.5%-1%, under the cooling bath of 5 ± 1 ℃, stirring; Rotating speed at 600～2000rpm disperses to drip amido silicon oil under agitation condition, and 1 ± 0.5h dropwises; Then add stoichiometric vulcabond, make the ratio (NCO/ (NH of isocyanic ester radical ion molar content in system and amino and hydroxyl molar content sum
2+ OH)) be 2-3:1, be warming up to 85 ± 5 ℃ of reaction 4 ± 0.5h, make amino-modified silicone base polyurethane prepolymer for use as;
Described hydroxy-terminated polybutadienes and the mass ratio of polyether glycol are 1:4～4:1, described catalyzer account for HTPB, polyether glycol total mass 0.01%～0.5%; Described amido silicon oil account for hydroxy-terminated polybutadienes and polyether glycol total mass 0.01%～1%;
2) chainextender is heated to 50-80 ℃ with step 1) the amino-modified silicone base polyurethane prepolymer for use as of gained mixes, and with 600～2000rpm rotating speed mechanical stirring, 30～180s, obtains Polyurethane Thermoplastic Elastomer;
The consumption of described chainextender accounts for 1%～10% of amino-modified silicone base polyurethane prepolymer for use as quality;
3) by step 2) Polyurethane Thermoplastic Elastomer of gained pours the polytetrafluoroethyldisk disk of clean dried into, be placed horizontally in vacuum drying oven, keeping in vacuum drying oven temperature is that 80～150 ℃, pressure are-0.08～-0.1MPa, after dry 4～24h, take out, obtain acid and alkali-resistance Polyurethane Thermoplastic Elastomer.
Described polyether glycol is to be obtained through autohemagglutination or copolymerization by propylene oxide, tetrahydrofuran (THF); The number-average molecular weight of polyether glycol is 1000～2000.
Described catalyzer is organic tin catalyzer, is selected from the mixture of a kind of in stannous octoate, dibutyltin diacetate and dibutyl tin laurate or any two kinds.
Described vulcabond is selected from tolylene diisocyanate, isophorone diisocyanate, hexamethylene diisocyanate, to phenyl diisocyanate, hexamethylene diisocyanate, 4, the mixture of a kind of or any two kinds and above composition in 4-diphenylmethanediisocyanate.
Described chainextender is selected from a kind of in following substances: BDO, 1,3-PD, Isosorbide-5-Nitrae-hexalin, neopentyl glycol, 1,6-hexylene glycol.
The amino value of described amido silicon oil is 0.3～0.6.
The invention has the beneficial effects as follows: utilizing hydroxy-terminated polybutadienes (HTPB) and polyether glycol is the urethane that soft section and vulcabond copolymerization obtain high strength, acid-alkali-corrosive-resisting, polyolefine segment is owing to not containing ester group, the ether of polarity, do not exist easily by the group of proton, electronic attack or oxidation, alkene key has hydrophobicity simultaneously, thereby this class formation has excellent acid-proof alkaline; Polyether segment polarity is little, and ehter bond stability to hydrolysis is good, and the soft segment structure acid-proof alkaline that ehter bond concentration is large is very outstanding; Amido silicon oil is the important Synergist S-421 95 of polyurethane elastomer, has low surface energy and hydrophobic nature, with it, as properties-correcting agent, can improve to a certain extent elastomeric acid-proof alkaline.
The acid and alkali-resistance type Polyurethane Thermoplastic Elastomer strength retention in strong acid and highly basic that adopts preparation method of the present invention to make is high, and the rate of decay is slow, has splendid acid-proof alkaline.
Embodiment
Describe specific embodiment of the invention scheme below in detail.
Embodiment 1
In the encloses container with high speed dispersor, high pure nitrogen protection, thermometer, add hydroxy-terminated polybutadienes (HTPB) 700g, polytetrahydrofuran polyvalent alcohol (number-average molecular weight 1000) 300g, stannous octoate 0.5g and vulcabond 5g; under the cooling bath of 5 ℃, stir; under the condition stirring in high speed dispersion, by dropping funnel, drip amido silicon oil, approximately 0.5h dropwises.Then add stoichiometric vulcabond, make the NCO/ (NH in system
2+ OH) be 2, be warmed up to about 85 ℃ reaction 4h, make amino-modified silicone base polyurethane prepolymer for use as.
By 1,4-butyleneglycol 36g is heated to 70 ℃ to be mixed with above-mentioned mixed type polyurethane prepolymer, with 600～2000rpm rotating speed mechanical stirring, 30～180s, obtain Polyurethane Thermoplastic Elastomer, above-mentioned product is poured into the polytetrafluoroethyldisk disk of clean dried, be placed horizontally in 120 ℃ of vacuum drying ovens, keeping vacuum tightness is-0.08～-0.1MPa, after 12h, take out, obtain acid and alkali-resistance Polyurethane Thermoplastic Elastomer.
Embodiment 2
In the encloses container with high speed dispersor, high pure nitrogen protection, thermometer, add hydroxy-terminated polybutadienes (HTPB) 500g, polytetrahydrofuran polyvalent alcohol (number-average molecular weight 1000) 500g, stannous octoate 0.5g and vulcabond 7g; under the cooling bath of 5 ℃, stir; under the condition stirring in high speed dispersion, by dropping funnel, drip amido silicon oil, approximately 0.5h dropwises.Then add stoichiometric vulcabond, make the NCO/ (NH in system
2+ OH) be 2, be warmed up to about 85 ℃ reaction 4h, make amino-modified silicone base polyurethane prepolymer for use as.
By 1, ammediol 45g is heated to 75 ℃ to be mixed with above-mentioned mixed type polyurethane prepolymer, with 600～2000rpm rotating speed mechanical stirring, 30～180s, obtain Polyurethane Thermoplastic Elastomer, above-mentioned product is poured into the polytetrafluoroethyldisk disk of clean dried, be placed horizontally in 110 ℃ of vacuum drying ovens, keeping vacuum tightness is-0.08～-0.1MPa, after 20h, take out, obtain acid and alkali-resistance Polyurethane Thermoplastic Elastomer.
Embodiment 3
In the encloses container with high speed dispersor, high pure nitrogen protection, thermometer, add hydroxy-terminated polybutadienes (HTPB) 300g, polytetrahydrofuran polyvalent alcohol (number-average molecular weight 1000) 700g, stannous octoate 0.5g and vulcabond 10g; under the cooling bath of 5 ℃, stir; under the condition stirring in high speed dispersion, by dropping funnel, drip amido silicon oil, approximately 0.5h dropwises.Then add stoichiometric vulcabond, make the NCO/ (NH in system
2+ OH) be 2, be warmed up to about 85 ℃ reaction 4h, make amino-modified silicone base polyurethane prepolymer for use as.
By 1,4-hexalin 50g is heated to 65 ℃ to be mixed with above-mentioned mixed type polyurethane prepolymer, with 600～2000rpm rotating speed mechanical stirring, 30～180s, obtain Polyurethane Thermoplastic Elastomer, above-mentioned product is poured into the polytetrafluoroethyldisk disk of clean dried, be placed horizontally in 100 ℃ of vacuum drying ovens, keeping vacuum tightness is-0.08～-0.1MPa, after 15h, take out, obtain acid and alkali-resistance Polyurethane Thermoplastic Elastomer.
GB/T1690-2006 standard is pressed in acid and alkali-resistance experiment, and style is placed in respectively 50% sulfuric acid, 18% hydrochloric acid and 48% sodium hydroxide solution, takes out test test piece performance after 70 times maintenance 72h.Stretching strength determination method: ISO37-2005.
Use after HTPB, elastomeric initial strength can be influenced, but because its strength retention is high, rate of decay is slow, show excellent stability especially in strong acid, makes PU elastomerics on work-ing life, occupy greater advantage.
Claims (7)
1. an acid and alkali-resistance method for preparing thermoplastic polyurethane elastomer, the steps include:
1) in reactor, add hydroxy-terminated polybutadienes, polyether glycol, catalyzer and account for hydroxy-terminated polybutadienes and the vulcabond of polyether glycol total mass 0.5%-1%, under 5 ± 1 ℃ of conditions, stir; Rotating speed at 600～2000rpm disperses to drip amido silicon oil under agitation condition, after dropwising, add vulcabond, making the isocyanic ester radical ion molar content in system is 2-3:1 with the ratio of amino and hydroxyl molar content sum, be warming up to 85 ± 5 ℃ of reaction 4 ± 0.5h, make amino-modified silicone base polyurethane prepolymer for use as;
Described hydroxy-terminated polybutadienes and the mass ratio of polyether glycol are 1:4～4:1; Described catalyzer account for hydroxy-terminated polybutadienes and polyether glycol total mass 0.01%～0.5%; Described amido silicon oil account for hydroxy-terminated polybutadienes and polyether glycol total mass 0.01%～1%;
2) chainextender being heated to after 50-80 ℃ and step 1) the amino-modified silicone base polyurethane prepolymer for use as of gained mixes, and with 600～2000rpm rotating speed, stirs 30～180s, obtains Polyurethane Thermoplastic Elastomer;
Described chainextender accounts for 1%～10% of amino-modified silicone base polyurethane prepolymer for use as quality;
3) by step 2) Polyurethane Thermoplastic Elastomer of gained is that 80～150 ℃, pressure are under-0.08～-0.1MPa condition in temperature, dry 4～24h, obtains acid and alkali-resistance Polyurethane Thermoplastic Elastomer.
2. a kind of acid and alkali-resistance method for preparing thermoplastic polyurethane elastomer according to claim 1, is characterized in that: described polyether glycol is to be obtained through autohemagglutination or copolymerization by propylene oxide, tetrahydrofuran (THF); The number-average molecular weight of polyether glycol is 1000～2000.
3. a kind of acid and alkali-resistance method for preparing thermoplastic polyurethane elastomer according to claim 1, is characterized in that: described catalyzer is organic tin catalyzer.
4. a kind of acid and alkali-resistance method for preparing thermoplastic polyurethane elastomer according to claim 3, is characterized in that: described organic tin catalyzer is selected from the mixture of a kind of in stannous octoate, dibutyltin diacetate and dibutyl tin laurate or any two kinds.
5. a kind of acid and alkali-resistance method for preparing thermoplastic polyurethane elastomer according to claim 1, it is characterized in that: described vulcabond is selected from tolylene diisocyanate, isophorone diisocyanate, hexamethylene diisocyanate, to phenyl diisocyanate, hexamethylene diisocyanate, 4 mixture of a kind of or any two kinds and above composition in 4-diphenylmethanediisocyanate.
6. a kind of acid and alkali-resistance method for preparing thermoplastic polyurethane elastomer according to claim 1, it is characterized in that: described chainextender is selected from a kind of in following substances: BDO, 1,3-PD, 1,4-hexalin, neopentyl glycol, 1,6-hexylene glycol.
7. a kind of acid and alkali-resistance method for preparing thermoplastic polyurethane elastomer according to claim 1, is characterized in that: the amino value of described amido silicon oil is 0.3～0.6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410264654.5A CN104004153A (en) | 2014-06-13 | 2014-06-13 | Method for manufacturing acid and alkali resistant thermoplastic polyurethane elastomer |
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| CN201410264654.5A CN104004153A (en) | 2014-06-13 | 2014-06-13 | Method for manufacturing acid and alkali resistant thermoplastic polyurethane elastomer |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105238033A (en) * | 2015-10-09 | 2016-01-13 | 滁州环球聚氨酯科技有限公司 | Wear-resistant acid/alkali-resistant polyurethane elastomer |
| CN109134822A (en) * | 2018-07-24 | 2019-01-04 | 大连中海达科技有限公司 | It is a kind of can ultraviolet light cross-linking thermoplastic polyurethane elastomer synthetic method |
| CN109401713A (en) * | 2018-09-11 | 2019-03-01 | 浙江奔富新能源股份有限公司 | A kind of dual-component polyurethane adhesive and preparation method thereof of resistance to acid liquid corrosion |
| 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 |
| EP3581603A4 (en) * | 2017-02-10 | 2020-11-25 | Miracll Chemicals Co., Ltd. | Thermoplastic organosilicone-polyurethane elastomer and preparation method therefor |
| 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 |
| CN115873199A (en) * | 2022-12-07 | 2023-03-31 | 盛鼎高新材料有限公司 | Low-temperature-resistant and impact-resistant polyurethane elastomer and processing technology thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105238033A (en) * | 2015-10-09 | 2016-01-13 | 滁州环球聚氨酯科技有限公司 | Wear-resistant acid/alkali-resistant polyurethane elastomer |
| EP3581603A4 (en) * | 2017-02-10 | 2020-11-25 | Miracll Chemicals Co., Ltd. | Thermoplastic organosilicone-polyurethane elastomer and preparation method therefor |
| US11643498B2 (en) | 2017-02-10 | 2023-05-09 | Miracll Chemicals Co., Ltd. | Thermoplastic silicone-polyurethane elastomer and method for preparing the same |
| CN109134822A (en) * | 2018-07-24 | 2019-01-04 | 大连中海达科技有限公司 | It is a kind of can ultraviolet light cross-linking thermoplastic polyurethane elastomer synthetic method |
| CN109134822B (en) * | 2018-07-24 | 2021-06-25 | 大连中海达科技有限公司 | Synthesis method of thermoplastic polyurethane elastomer capable of being crosslinked by ultraviolet light |
| CN109401713A (en) * | 2018-09-11 | 2019-03-01 | 浙江奔富新能源股份有限公司 | A kind of dual-component polyurethane adhesive and preparation method thereof of resistance to acid liquid corrosion |
| 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 |
| CN115873199A (en) * | 2022-12-07 | 2023-03-31 | 盛鼎高新材料有限公司 | Low-temperature-resistant and impact-resistant polyurethane elastomer and processing technology thereof |
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Effective date of registration: 20160620 Address after: 215600, Austen, Mstar Technology Ltd, 17 Yue Yue Road, Zhangjiagang Economic Development Zone, Jiangsu, Suzhou Applicant after: SUZHOU AUSTIN NOVEL MATERIALS TECHNOLGY CO., LTD. Address before: 215600 Austen new material (Zhangjiagang) Co., Ltd., 17 Yue Yue Road, Zhangjiagang Economic Development Zone, Suzhou, Jiangsu Applicant before: Austen new material (Zhangjiagang) Co., Ltd. |
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