Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of conjugated diene and polar monomer segmented copolymer with low molecular weight

A technology of block copolymers and polar monomers, which is applied in the field of preparation of block copolymers of conjugated dienes and polar monomers, can solve the problems of high preparation costs and high molecular weight of copolymers, and achieve low molecular weight and high molecular weight. Narrow distribution and high catalytic activity

Active Publication Date: 2013-02-06
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
View PDF5 Cites 6 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the problem of high molecular weight and high preparation cost of existing copolymers of conjugated dienes and polar monomers, and to provide a low molecular weight conjugated diene and polar monomer block copolymerization method of preparation

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of conjugated diene and polar monomer segmented copolymer with low molecular weight
  • Preparation method of conjugated diene and polar monomer segmented copolymer with low molecular weight
  • Preparation method of conjugated diene and polar monomer segmented copolymer with low molecular weight

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0028] The present invention provides a kind of preparation method of low molecular weight conjugated diene and polar monomer block copolymer, comprising the following steps:

[0029] Step 1: adding the reaction monomer and the catalyst into an alkane solvent in a molar ratio of 100 to 2000:1 to obtain a solution a;

[0030] Step 2: adding the polar monomer to the solution a obtained in step 1 to obtain solution b; the molar ratio of the polar monomer to the catalyst is 10-800:1;

[0031] Step 3: adding ethanol solution to the solution b obtained in step 2 to condense a block copolymer of conjugated diene and polar monomer;

[0032] The reaction monomer is isoprene or butadiene;

[0033] The polar monomer is ε-caprolactone, butyrolactone, valerolactone or lactide;

[0034] The preparation method of the catalyst is as follows: alkoxy rare earth compound, hydrogen alkyl aluminum compound, chloride and conjugated diene are mixed and then reacted to obtain the catalyst.

[0035...

Embodiment 1

[0046] In the 10mL catalyst reaction bottle filled with nitrogen after vacuum baking, add neodymium isopropoxide (Nd), diisobutylaluminum hydride (Al), dichlorodimethylsilane (Cl) and isoprene Alkene (IP) was reacted in a constant temperature water bath at 20°C for 60 minutes to obtain a homogeneous rare earth catalyst. The molar ratio of [Nd] / [Al] / [Cl] / [IP] in this catalyst was 1 / 10 / 4 / 3 ;

[0047] Add toluene, isoprene and the above-mentioned homogeneous rare earth catalyst in turn to the 40mL ampoule bottle after vacuum drying and filling with nitrogen. The concentration of isoprene is 1mol / L, and the catalyst dosage is [IP] The / [Nd] molar ratio is 100 / 1, and the polymerization is carried out in a constant temperature water bath at 50°C. After 4 hours of polymerization, ε-caprolactone (ε-CL) monomer, ε-caprolactone and neodymium in a rare earth catalyst are added The molar ratio of the compound is [ε-CL] / [Nd]= 10 / 1, and after the polymerization reaction is carried out at 5...

Embodiment 2

[0050] The preparation method is the same as in Example 1, except that the molar ratio of isoprene to the neodymium compound in the rare earth catalyst is [IP] / [Nd]=200 / 1, and the ratio of ε-caprolactone to the neodymium compound in the rare earth catalyst is The molar ratio is [ε-CL] / [Nd]= 50 / 1, the yield of the obtained block copolymer of conjugated diene and polar monomer is 98%, and the polyisoprene segment in the copolymer The number average molecular weight is M n = 2.16×10 3 , the molecular weight distribution is M w / M n =1.20, 1,4-structure content is 91.7%, 3,4-structure content is 8.3%, the number average molecular weight of the copolymer is M n =2.52×10 3 , the molecular weight distribution index is M w / M n =1.23. pass 1 According to H-NMR calculation, the molar ratio of polyisoprene segment to polycaprolactone segment in the copolymer is 3.8 / 1. The glass transition temperature (T) of the copolymer was measured by DSC g ) is -67.2℃, melting point (T ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
Glass transition temperatureaaaaaaaaaa
Glass transition temperatureaaaaaaaaaa
Melting pointaaaaaaaaaa
Login to View More

Abstract

A preparation method of a conjugated diene and polar monomer segmented copolymer with low molecular weight belongs to the field of copolymer synthesis. The method can solve the problem that the existing conjugated diene and polar monomer copolymer is high in molecular weight and preparation cost. The method comprises the steps of adding a reaction monomer and a catalyst to an alkane solvent according to the molar ratio of (100-2000):1 for reaction to obtain a solution a, adding the polar monomer to the obtained solution a to obtain a solution b, adding alcohol solution to the obtained solution b with the molar ratio of the polar monomer to the catalyst of (10-800):1, and condensing the conjugated diene and polar monomer segmented copolymer. For the synthesized conjugated diene and polar monomer segmented copolymer, the number-average molecular weight is 1.2*10<3>-25.0*10<3>, and the molecular weight distribution is 1.20-1.50.

Description

technical field [0001] The invention belongs to the field of copolymer synthesis, and in particular relates to a preparation method of a low molecular weight conjugated diene and polar monomer block copolymer. Background technique [0002] Conjugated diene polymer is one of the main varieties of high-performance synthetic rubber. Introducing polar groups or polar polymer chains into conjugated diene polymers can improve its surface wettability, coloring properties, adhesion, solvent resistance, etc., and most importantly, it can improve its compatibility with other polymer materials. compatibility. At present, the method of introducing polar groups in rubber mainly focuses on the introduction of polar groups at the end or side chain of liquid rubber. This method improves the wettability, coloring, adhesion and compatibility of rubber to a certain extent. The compatibility of other polymer materials, etc., and the introduction of polar polymer segments (and block copolymers...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C08F297/06C08F236/04C08F236/06C08F236/08C08F4/54C07C67/465
Inventor 张学全王凤张春雨白晨曦毕吉福代全权那丽华于琦周
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com