Method for preparing thermo-plastically reprocessed cross-linked halogenated butyl rubber

A technology of halogenated butyl rubber and cross-linked rubber, used in the preparation of carboxylate, organic chemistry, etc.

Inactive Publication Date: 2011-01-26
BEIJING UNIV OF CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Replacing the traditional cross-linking agent (vulcanizing agent) with a thermally reversible cross-linking agent to carry out covalent cross-linking of rubber, while ensuring that the cross-linked rubber has certain physical a

Method used

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  • Method for preparing thermo-plastically reprocessed cross-linked halogenated butyl rubber
  • Method for preparing thermo-plastically reprocessed cross-linked halogenated butyl rubber
  • Method for preparing thermo-plastically reprocessed cross-linked halogenated butyl rubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] 100g deionized water, 0.83g sodium dodecyl sulfate (SDS), 0.27g NaHCO 3 Add it into the reactor and heat until completely dissolved, then add 5g of octyl acrylate (OA) to pre-emulsify for 20 minutes to obtain a pre-emulsion. After the temperature rises to 75°C, add 20 mL of an aqueous solution containing 0.05 g of potassium persulfate (KPS), and add dropwise 20 mL of an aqueous solution containing 0.15 g of KPS, 10.51 g of 4-vinylpyridine, and 9.74 g of octyl acrylate. The monomer mixture composed of 2.56 g of butyl acrylate was controlled to add the monomer for 3 hours. After the monomer was added, the reaction was continued for 8 hours, and the mixture was cooled and discharged to obtain a milky white emulsion. The solid content of the emulsion is 20%, and the monomer conversion rate is about 90%.

[0075] The resulting emulsion was demulsified with a 2% NaCl solution to obtain a polymer containing pyridine side groups. The polymer was soaked in an aqueous NaOH solut...

Embodiment 2

[0077] With 500g deionized water, 5.36g sodium dodecylsulfonate (SDS), 0.54gNaHCO 3 Add it into the reactor until it completely dissolves. After the temperature is raised to 70°C and stabilizes, add 6.00 g of a mixture of styrene and divinylbenzene (DVB) (99% styrene, 1% DVB) for pre-emulsification for 20 minutes to obtain a pre-emulsion. Add 25mL of aqueous solution containing 0.54g of ammonium persulfate (APS) was pre-polymerized, and after the blue light appeared in the system, 34.00g of mixed monomers of styrene and divinylbenzene (styrene 99%, DVB1%) were added dropwise, and the dropping time was 4h . After adding the mixed monomers of styrene and divinylbenzene, react for 6 hours, then add 13.60 g of mixed monomers of styrene and 4-vinylpyridine (4-VP15%, styrene 85%) dropwise, and continue the reaction After 16 hours, a translucent white emulsion with blue light was obtained. The solid content of the emulsion is 10%, and the monomer conversion rate is 96%.

[0078] A...

Embodiment 3

[0080] Add 27.78g of sodium sand into 442.52g of anhydrous tetrahydrofuran, and gradually add 59.57g of cyclopentadiene (CPD) under the conditions of ice-water bath cooling and magnetic stirring, and react for 24h. The obtained cyclopentadiene sodium solution was mixed with excess dry ice, reacted for 6 hours to obtain dicyclopentadiene sodium dicarboxylate slurry, and then the solvent was removed by suction filtration and dried under reduced pressure at 60°C to constant weight to obtain dicyclopentadiene dicarboxylate slurry. Sodium formate crosslinker [DCPD(COONa) 2 ] 85.78 g.

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Abstract

The invention relates to a method for preparing a thermo-plastically reprocessed cross-linked halogenated butyl rubber. A rubber is cross-linked by blending a polymer containing a pyridine side group or dicyclopentadiene formate thermally-reversible cross-linking agent and a halogenated butyl rubber and performing quaternization or esterification on the mixture under a thermo-compression condition. The cross-linked rubber sample is subjected to reverse quaternization or reverse Diels-Alder reaction of dicyclopentadiene cross-linking bridge bonds under the thermo-compression condition at a high temperature to perform decrosslinking, so the cross-linked rubber has thermoplastic processability. The rubber sample cross-linked by the thermally-reversible cross-linking agent has the performance of a vulcanized rubber and thermoplastic processability, so that rubber scraps and waste or old rubber products are conveniently reprocessed and utilized.

Description

technical field [0001] The present invention relates to a thermally reversible cross-linking technology of halogen functionalized rubber, in particular to a cross-linking technology of halogenated butyl rubber and tertiary amine-containing polymer or dicyclopentadiene dicarboxylate cross-linking agent and cross-linked rubber performance. Background technique [0002] Halogenated butyl rubber not only has excellent air tightness, excellent heat resistance, aging resistance and ozone resistance, but also has the advantages of fast vulcanization speed, good compatibility with other rubbers, good mutual adhesion, and small compression deformation. It has a wide range of applications in medical sealing products, tire inner tubes or tire linings, protective clothing and other fields. [0003] As we all know, raw rubber has a chemical crosslinking network after being vulcanized and crosslinked by various vulcanizing agents, so it has certain physical and mechanical properties and ...

Claims

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Application Information

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IPC IPC(8): C08J3/24C08L23/28C08L33/08C08L25/08C08K13/02C08K5/098C08F220/18C08F226/06C08F212/08C07C61/29C07C51/41
Inventor 陈晓农申凤山张立毅谢映雪苏志强石淑先张立群马东风王备战
Owner BEIJING UNIV OF CHEM TECH
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