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

Slurry polymerization method for preparing bimodal distribution star-branched butyl rubber by using imino-terminated functionalized macromolecular branching agent

A technology with terminal imino function and bimodal distribution, applied in the field of butyl rubber preparation, can solve the problems of unsuitability for industrial application and high gel content, and achieve fast stress relaxation, low solution viscosity, and good carbon black compatibility. Effect

Active Publication Date: 2020-02-28
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
View PDF5 Cites 11 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The system using divinylbenzene as a branching agent is easy to synthesize star-branched structure butyl rubber, which can be used to explore the synthesis rules and structural characterization methods of star-branched structures. The glue content is very high, according to the current research results, it is not suitable for industrial application

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
  • Slurry polymerization method for preparing bimodal distribution star-branched butyl rubber by using imino-terminated functionalized macromolecular branching agent
  • Slurry polymerization method for preparing bimodal distribution star-branched butyl rubber by using imino-terminated functionalized macromolecular branching agent
  • Slurry polymerization method for preparing bimodal distribution star-branched butyl rubber by using imino-terminated functionalized macromolecular branching agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Under anhydrous and oxygen-free conditions, add 250 mL of cyclohexane, 16 mL of styrene, 1 mL of tetramethylethylenediamine (TMEDA) and 0.7 mL of n-butyllithium (0.9 M hexane solution) into the polymerization bottle, Shake well and seal, react at 50°C for 5 hours, then add 12mL of isoprene, react at 50°C for 6 hours, add 2mL of p-N,N-dimethylaminobenzoic acid aniline (0.1M, cyclohexyl alkane solution), react at 60°C for 30min, add cyclohexane and methanol to repeatedly flocculate and dissolve the product, wash off unreacted p-N,N-dimethylaminobenzoic acid aniline, and dry in a vacuum oven at 30°C Spare, number SI-1.

[0045] (2) Dissolve the branching agent sample of 0.2% of the total monomer weight in 40mL of dichloromethane, add it to a 4L polymerization kettle with a total volume, add 1296mL of methyl chloride, 536mL of isobutylene, 29mL of isoprene, and the rotation speed of the stirring paddle is 190r / min, the temperature drops below -85°C, take 2.65mL of dic...

Embodiment 2

[0049] (1) Under anhydrous and oxygen-free conditions, add 250 mL of cyclohexane, 16 mL of styrene, 1 mL of tetramethylethylenediamine (TMEDA) and 0.7 mL of n-butyllithium (0.9 M hexane solution) into the polymerization bottle, Shake well and seal, react at 50°C for 5 hours, then add 12mL of isoprene, react at 50°C for 6 hours, add 2mL of p-N,N-dimethylaminobenzoic acid aniline (0.1M, cyclohexyl alkane solution), react at 60°C for 30min, add cyclohexane and methanol to repeatedly flocculate and dissolve the product, wash off unreacted p-N,N-dimethylaminobenzoic acid aniline, and dry in a vacuum oven at 30°C Spare, number SI-1.

[0050] (2) Dissolve the 0.5% branching agent sample of the total monomer weight in 40mL of dichloromethane, add it to a total volume of 4L polymerization kettle, add 1296mL of methyl chloride, 536mL of isobutylene, 29mL of isoprene, and the stirring speed of the impeller is 190r / min, the temperature was lowered to below -85°C, 2.65mL of saturated dic...

Embodiment 3

[0052] (1) Under anhydrous and oxygen-free conditions, add 250 mL of cyclohexane, 16 mL of styrene, 1 mL of tetramethylethylenediamine (TMEDA) and 0.7 mL of n-butyllithium (0.9 M hexane solution) into the polymerization bottle, Shake well and seal, react at 50°C for 5 hours, then add 12mL of isoprene, react at 50°C for 6 hours, add 2mL of p-N,N-dimethylaminobenzoic acid aniline (0.1M, cyclohexyl alkane solution), react at 60°C for 30min, add cyclohexane and methanol to repeatedly flocculate and dissolve the product, wash off unreacted p-N,N-dimethylaminobenzoic acid aniline, and dry in a vacuum oven at 30°C Spare, number SI-1.

[0053] (2) Dissolve the 1.0% branching agent sample of the total monomer weight in 40mL of dichloromethane, add it to a 4L polymerization kettle with a total volume, add 1296mL of methyl chloride, 536mL of isobutylene, 29mL of isoprene, and the stirring speed is 190r / min, the temperature was lowered to below -85°C, 2.65mL of saturated dichloromethane...

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

No PUM Login to View More

Abstract

The invention belongs to the technical field of butyl rubber preparation, and relates to a slurry polymerization method for preparing bimodal distribution star-shaped branched butyl rubber by using animino-terminated functionalized macromolecular branching agent. The slurry polymerization method comprises two steps of synthesizing the imino-terminated functionalized macromolecular branching agentand synthesizing the star-branched butyl rubber with amino; a copolymer of styrene and derivatives of styrene, and isoprene is prepared by adopting active anionic polymerization technology, and the imino-containing branching agent macromolecules are obtained by using Schiff base for end capping. The preparation method comprises the following steps: dissolving the branching agent into chloromethane, adding an obtained mixture into a butyl rubber slurry polymerization kettle, and preparing the star-shaped branched butyl rubber with bimodal distribution by taking the branching agent as a cationic polymerization grafting agent and a slurry stabilizer. Lower Mooney stress relaxation and intrinsic viscosity are achieved, and better processability is achieved; the imino groups introduced duringend capping can increase the polarity of the branching agent, so that the dispersion of carbon black in a butyl rubber matrix is facilitated, the compatibility of butyl rubber and carbon black is improved, and the system energy is reduced.

Description

technical field [0001] The invention belongs to the technical field of butyl rubber preparation, and in particular relates to a slurry polymerization method for preparing bimodal star-shaped branched butyl rubber with an imino-terminated functionalized macromolecular branching agent; A method for preparing bimodal star-branched butyl rubber with imino-functional macromolecules as branching agents; that is, a diblock-terminated imino copolymer of styrene and its derivatives and isoprene as branch A preparation method for synthesizing star-branched butyl rubber with chemical agent and slurry stabilizer. Background technique [0002] Butyl rubber is polymerized from isobutylene and a small amount of isoprene, and is currently the only industrialized product of cationic polymerization. The molecular chain unsaturation of butyl rubber is extremely low, about 0.5% to 3.3% (mol), which is far lower than that of natural rubber, but it is enough to form a cross-linked network struct...

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
Patent Type & Authority Applications(China)
IPC IPC(8): C08F210/12C08F236/08C08F212/08C08F8/32
CPCC08F210/12C08F212/08C08F8/32C08F236/08
Inventor 伍一波黄珊商育伟李树新郭文莉
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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