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Polyurethane elastomer based on high cis-terminated hydroxyl polybutadiene and preparation method thereof

A technology of hydroxyl-terminated polybutadiene and polyurethane elastomer, which is applied in the field of polyurethane elastomer based on high-cis-hydroxyl-terminated polybutadiene and its preparation, can solve the problem of uneven crosslinking network, inaccurate distribution of hydroxyl groups, and mechanical problems. Poor performance and other problems, to achieve the effect of low glass transition temperature, excellent mechanical properties, and mild reaction conditions

Active Publication Date: 2019-01-18
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the hydroxyl-terminated polybutadiene synthesized by free radical polymerization method on the market has a 1,4-content of about 77%, a glass transition temperature of about -78°C, and a wide molecular weight distribution and inaccurate distribution of hydroxyl groups.
The hydroxyl-terminated polybutadiene obtained by free radical polymerization has the disadvantages of uneven crosslinking network and poor mechanical properties as the soft segment of synthetic polyurethane elastomer. At the same time, its glass transition temperature is about -70 ° C. There is no obvious advantage over type polyurethane

Method used

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  • Polyurethane elastomer based on high cis-terminated hydroxyl polybutadiene and preparation method thereof
  • Polyurethane elastomer based on high cis-terminated hydroxyl polybutadiene and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Take 4g of high-cis-hydroxyl-terminated polybutadiene with a hydroxyl value of 0.38mmol / g, dissolve it in 30ml of anhydrous tetrahydrofuran, and add measured toluene diisocyanate to ensure that cyanate and high-cis-polybutadiene in toluene diisocyanate The molar ratio of the hydroxyl groups in the hydroxyl-terminated polybutadiene is 1.2, and 0.05% dibutyltin dilaurate (DBTDL) is added as a catalyst, under the protection of anhydrous and nitrogen, at 25°C. Reaction 1h to obtain prepolymer.

[0022] (2) The prepolymer prepared in step (1) is reacted with measured 1,4-butanediol, and the hydroxyl group in 1,4-butanediol is different from the prepolymer prepared in step (1). The molar ratio of cyanate was 0.2, and the reaction was carried out under the protection of anhydrous and nitrogen at 25°C for 1 hour.

[0023] (3) Remove the solvent tetrahydrofuran from the product prepared in step (2) and cure it at 60°C for 5 hours to finally obtain a polyurethane elastomer w...

Embodiment 2

[0026] (1) Take 4g of high cis-hydroxyl-terminated polybutadiene with a hydroxyl value of 0.7mmol / g, dissolve it in 40ml of anhydrous tetrahydrofuran, and add the measured diphenylmethane diisocyanate to ensure that the diphenylmethane diisocyanate The mol ratio of cyanate group and hydroxyl in the high cis-end hydroxyl polybutadiene is 1.4, add the dibutyltin dilaurate (DBTDL) of relative high cis-end hydroxyl polybutadiene quality 0.1% as catalyst, in anhydrous and Under nitrogen protection, react at 30°C for 1.5h to obtain a prepolymer.

[0027] (2) the prepolymer prepared in step (1) is reacted with metered ethylene glycol, and the mol ratio of isocyanate in the hydroxyl group in ethylene glycol and the prepolymer prepared in step (1) is 0.4, Under the protection of anhydrous and nitrogen, react at 30°C for 1.5h.

[0028] (3) Remove the solvent tetrahydrofuran from the product obtained in step (2) and cure it at 70°C for 6 hours to finally obtain a polyurethane elastomer ...

Embodiment 3

[0030] (1) Take 4g of high-cis-hydroxyl-terminated polybutadiene with a hydroxyl value of 0.9mmol / g, dissolve it in 50ml of anhydrous tetrahydrofuran, and add a measured amount of 1,5-naphthalene diisocyanate to ensure that 1,5-naphthalene diisocyanate The mol ratio of the cyanate group in the isocyanate and the hydroxyl group in the high-cis-end hydroxyl polybutadiene is 1.6, and the dibutyltin dilaurate (DBTDL) of 0.3% of the relative high-cis-end hydroxyl polybutadiene quality is added as a catalyst. Under the protection of water and nitrogen, react at 35°C for 2h to obtain a prepolymer.

[0031] (2) the prepolymer prepared in the step (1) is reacted with the measured propylene glycol, and the mol ratio of the isocyanate in the hydroxyl group in the propylene glycol and the prepolymer prepared in the step (1) is 0.6, in anhydrous and Under nitrogen protection, react at 35°C for 2h.

[0032] (3) Remove the solvent tetrahydrofuran from the product obtained in step (2) and cu...

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Abstract

The invention discloses a high cis terminal hydroxyl polybutadiene-based polyurethane elastomer and a preparation method therefore. The polyurethane elastomer is prepared by segmenting high cis terminal hydroxyl polybutadiene which is taken as a soft segment and diisocyanate and dihydric alcohol as a hard segment. The preparation method comprises: by taking high cis terminal hydroxyl polybutadiene and diisocyanate as raw materials, firstly preparing a pre-polymer; then carrying out a reaction on the pre-polymer and dihydric alcohol; and finally removing tetrahydrofuran and curing to obtain novel casted polyurethane elastomer. The high cis terminal hydroxyl polybutadiene-based polyurethane elastomer prepared by the preparation method has good low temperature property and elasticity, and the glass-transition temperature of the elastomer can reach -104 DEG C and the elongation at break is 500-700%. According to the high cis terminal hydroxyl polybutadiene-based polyurethane elastomer disclosed by the invention, the application range of the polyurethane elastomer is expanded, and the market of the polyurethane elastomer is expanded.

Description

technical field [0001] The invention belongs to the technical field of cast polyurethane elastomers, and relates to a polyurethane elastomer based on high cis-terminated hydroxyl polybutadiene and a preparation method thereof. Background technique [0002] Polyurethane elastomer refers to a polymer material with a glass transition temperature lower than room temperature, an elongation at break greater than 50%, good recovery after external force is removed, and a main chain containing repeatable urethane segments. Its molecular main chain is composed of a soft segment whose glass transition temperature is lower than room temperature and a hard segment block whose glass transition temperature is higher than room temperature. The soft segment occupies a large proportion in the polyurethane molecule. According to different soft segments, polyurethane elastomers can be divided into polyester type, polyether type and polyolefin type. Among the polyolefin polyurethanes, the poly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/69C08G18/65C08G18/32C08G18/10
CPCC08G18/10C08G18/3206C08G18/6588C08G18/69
Inventor 介素云李伯耿曹哲周勤灼
Owner ZHEJIANG UNIV
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