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A kind of high-functionality hydroxyl-terminated polybutadiene and its preparation method

A hydroxyl-terminated polybutadiene and high-functionality technology, which is applied in the field of high-functionality hydroxyl-terminated polybutadiene and its preparation, can solve problems such as insufficient functionality, reduce molecular weight distribution, reduce production costs, and reduce reaction the effect of time

Active Publication Date: 2022-05-27
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The high-functionality hydroxyl-terminated polybutadiene of the present invention is based on the traditional anionic synthesis of hydroxyl-terminated polybutadiene, introducing a polar reaction solvent and dodecyl alcohol sodium salt as an exchange agent, while maintaining anionic synthesis of hydroxyl-terminated polybutadiene Based on the advantages of polybutadiene material with controllable molecular weight, uniform functionality, narrow molecular weight distribution, oil resistance and chemical resistance, combined with theoretical analysis and experimental discussion, using the basis of changing the polarity of the solvent and adding sodium lauryl alkoxide On the one hand, it improves the problem of insufficient functionality of the material, avoids the appearance of pseudo-gel phenomenon, and at the same time ensures the advantages of uniform molecular weight and narrow molecular weight distribution of the material

Method used

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  • A kind of high-functionality hydroxyl-terminated polybutadiene and its preparation method
  • A kind of high-functionality hydroxyl-terminated polybutadiene and its preparation method
  • A kind of high-functionality hydroxyl-terminated polybutadiene and its preparation method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] The preparation process of the high-functionality hydroxyl-terminated polybutadiene of the present embodiment is as follows:

[0049] (1) Preparation of lithium naphthalene initiator: use cyclohexane and tetrahydrofuran to cooperate as a solvent, naphthalene and lithium metal generate a lithium naphthalene initiator under the protection of an argon atmosphere under ice-water bath conditions, and the lithium naphthalene initiator is subjected to suction filtration to obtain clarification After the liquid, it reacts with isoprene to obtain short-chain active species.

[0050] The volume ratio of cyclohexane to tetrahydrofuran was 3:1. Under the protection of argon atmosphere, the 10g lithium rod was quickly peeled off the surface oxide film, and then the scissors were used to cut it into lithium scraps. Weigh the measured naphthalene in a ratio of 1, add it into the there-necked flask, add the tetrahydrofuran that is now steamed and used under the ice-water bath conditio...

Embodiment 2

[0057] The preparation process of the high-functionality hydroxyl-terminated polybutadiene of the present embodiment is as follows:

[0058] (1) Preparation of lithium naphthalene initiator: use cyclohexane and tetrahydrofuran to cooperate as a solvent, naphthalene and lithium metal generate a lithium naphthalene initiator under the protection of an argon atmosphere under ice-water bath conditions, and the lithium naphthalene initiator is subjected to suction filtration to obtain clarification After the liquid, it reacts with isoprene to obtain short-chain active species.

[0059] The volume ratio of cyclohexane to tetrahydrofuran was 3:1. Under the protection of argon atmosphere, the 10g lithium rod was quickly peeled off the surface oxide film, and then the scissors were used to cut it into lithium scraps. Weigh the measured naphthalene in a ratio of 1, add it into the there-necked flask, add the tetrahydrofuran that is now steamed and used under the ice-water bath conditio...

Embodiment 3

[0066] The preparation process of the high-functionality hydroxyl-terminated polybutadiene of the present embodiment is as follows:

[0067] (1) Preparation of lithium naphthalene initiator: use cyclohexane and tetrahydrofuran to cooperate as a solvent, naphthalene and lithium metal generate a lithium naphthalene initiator under the protection of an argon atmosphere under ice-water bath conditions, and the lithium naphthalene initiator is subjected to suction filtration to obtain clarification After the liquid, it reacts with isoprene to obtain short-chain active species.

[0068]The volume ratio of cyclohexane to tetrahydrofuran was 3:1. Under the protection of argon atmosphere, the 10g lithium rod was quickly peeled off the surface oxide film, and then the scissors were used to cut it into lithium scraps. Weigh the measured naphthalene in a ratio of 1, add it into the there-necked flask, add the tetrahydrofuran that is now steamed and used under the ice-water bath condition...

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Abstract

The invention discloses a high-functionality hydroxyl-terminated polybutadiene and a preparation method thereof. The preparation method comprises the following steps: reacting butadiene and a short-chain initiator in a polar solvent at 30-50°C for 3-5 hours, lowering the temperature to 5-10°C, and then adding sodium lauryl alkoxide solution , react for 1-1.5 hours, then add ethylene oxide and react at 0-10°C for 2-4 hours, and finally acidify to obtain hydroxyl-terminated polybutadiene, wherein the short-chain initiator is oligomerized isopentyl initiated by both ends Lithium Diene. The hydroxyl-terminated polybutadiene prepared by the invention has the advantages of uniform functionality, narrow molecular weight distribution and high functionality, wherein the molecular weight distribution is between 1.05-1.15 and the functionality is 1.9-2.0.

Description

technical field [0001] The invention relates to the field of polymer synthesis, in particular to a high-functionality hydroxyl-terminated polybutadiene and a preparation method thereof. Background technique [0002] Hydroxyl-terminated polybutadiene (HTPB) obtained by anionic polymerization can be used in many aspects. The performance of HTPB used in rocket technology has high requirements, and HTPB-type composite solid propellant not only has a wide range of combustion rate adjustment, It has the advantages of low viscosity and high solid content, and its process performance is excellent; hydroxyl terminated polybutadiene (referred to as butylated hydroxy rubber, the same below) has a wide range of applications, and has very important applications in various fields in my country, due to its excellent mechanical properties. Performance, especially with hydrolysis resistance, acid and alkali corrosion resistance, wear resistance, low temperature resistance and excellent electri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F136/06C08F4/48C08C19/00
CPCC08F136/06C08C19/00C08F4/482
Inventor 张立群程仕华秦璇赵永凯付思伟毛立新鲁建民
Owner BEIJING UNIV OF CHEM TECH