Method for preparing liquid polyisoprene rubber with medium or low molecular weight by bulk polymerization

A polyisoprene and low-molecular-weight technology, applied in the field of low-molecular-weight liquid polyisoprene rubber, can solve problems such as difficult recycling, low production efficiency, and environmental pollution by solvents, achieve mild polymerization process, reduce production costs, The effect of improving productivity

Active Publication Date: 2012-05-16
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

WO9937694-A; EP1049727-A reported a method for preparing isoprene and polybutadiene by using the gas phase method of rare earth chloride system. This method needs to add electronic reagents, such as ethanol and phosphoric acid tris Butyl ester, etc., increase the preparation process and cost
Simultaneously, this method is gas-phase polymerization, and production efficiency is low
Patents US2008182954-A1 and JP2008163338-A report a method for preparing liquid isoprene and polybutadiene using a rare earth system, but this method needs to use methylaluminoxane (MAO) as an auxiliary agent in the catalyst preparation process. catalyst, and toluene is required as a solvent, which not only increases the cost of catalyst preparation, but also pollutes the environment and is not easy to recycle

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1 Under the protection of nitrogen, in a dry catalyst reactor, according to the molar ratio of 1:60, add 0.25mmol dodecylbenzenesulfonate neodymium and 15mmol triisobutylaluminum Al(i- Bu) 3 , and then added 1.14ml of hexane solution, and aged at 70°C for 0.5 hour to obtain a homogeneous catalyst.

[0017] The conditions for preparing medium and low molecular weight liquid polyisoprene rubber by isoprene bulk polymerization are as follows: under the protection of nitrogen, add 13.6g of isoprene monomer to an anhydrous and oxygen-free polymerization kettle, and then add 0.55ml The above-mentioned neodymium dodecylbenzenesulfonate catalyst, the molar ratio of the catalyst neodymium dodecylbenzenesulfonate to the mass g of isoprene monomer is 2.0×10 -6 , polymerized at a temperature of 20°C for 25 hours; after the reaction, terminated with an ethanol solution containing 1% (weight ratio) of 2,6-di-tert-butyl-p-cresol, and then washed and extruded, the temperature ...

Embodiment 2

[0020] Example 2 Under the protection of nitrogen, into the dry catalyst reactor, according to the molar ratio of 1:30, add 0.25mmol of neodymium dodecylbenzenesulfonate and 7.5mmol of diethylaluminum hydride AlEt 2 H, add 4.12ml of hexane solution, and age at 50°C for 5 hours to obtain a homogeneous catalyst.

[0021] The conditions for preparing medium and low molecular weight liquid polyisoprene rubber by isoprene bulk polymerization are as follows: under the protection of nitrogen, add 13.6g of isoprene monomer to an anhydrous and oxygen-free polymerization kettle, and then add 0.27ml The above-mentioned neodymium dodecylbenzenesulfonate catalyst, the mol number of the catalyst neodymium dodecylbenzenesulfonate and the mass g ratio of the isoprene monomer are 1.0×10 -6 , polymerized at a temperature of 60°C for 20 hours; after the reaction, terminated with an ethanol solution containing 1% (by weight) of 2,6-di-tert-butyl-p-cresol, and then washed and extruded, the tempera...

Embodiment 3

[0024]Example 3 Under the protection of nitrogen, into the dry catalyst reactor, according to the molar ratio of 1:30, respectively add 0.25mmol of dodecylbenzenesulfonate neodymium compound and 7.5mmol of triisobutylaluminum Al (i-Bu) 3 , and then added 3.07ml of hexane solution, aged at -20°C for 4 hours to obtain a homogeneous catalyst.

[0025] The conditions for preparing medium and low molecular weight liquid polyisoprene rubber by isoprene bulk polymerization are as follows: under the protection of nitrogen, add 13.6g of isoprene monomer to an anhydrous and oxygen-free polymerization kettle, and then add 0.14ml The above-mentioned neodymium dodecylbenzenesulfonate catalyst, the mol number of the catalyst neodymium dodecylbenzenesulfonate and the mass g ratio of the isoprene monomer are 0.5×10 -6 , polymerized at a temperature of 50°C for 24 hours; after the reaction, terminated with an ethanol solution containing 1% (weight ratio) of 2,6-di-tert-butyl-p-cresol, and the...

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Abstract

The invention belongs to a method for preparing liquid polyisoprene rubber with medium or low molecular weight by bulk polymerization. Catalyst comprises binary components: rare earth organic sulfonic acid compound taken as main catalyst and alkyl aluminium taken as catalyst promoter; wherein, the mole ratio between the catalyst promoter and the main catalyst is 20-60:1. In the preparation process of the catalysts, a third component is not added; the production efficiency is improved, and the production cost caused by recovery treatment of solvent can be reduced. In addition, the polymerization process is mild and stable, and is not needed to be added with a heat withdrawing device; therefore, after polymerization, the liquid polyisoprene rubber which has medium or low molecular weight, the monomer conversion rate of more than 90%, cis-1, 4 structural content of more than 89%, the weight-average molecular weight of 5000-20000 and the molecular weight distribution index of 3-6 can be obtained.

Description

technical field [0001] The invention belongs to a method for preparing medium and low molecular weight liquid polyisoprene rubber by bulk polymerization. Background technique [0002] Generally, liquid rubber refers to a viscous flowable liquid with a relative molecular mass of 10,000 or less. Its main advantages are: easy to operate; it can be processed by casting method and injection method, with simple equipment and convenient construction; it can produce various rubber products from rubber shoes, industrial products to tires, etc.; it is the best processing aid in the rubber industry. Such as plasticizers, vulcanization aids, modifiers, etc. It is also a toughening agent in the plastics industry, a potting agent, a coating agent in the electronics industry, and a modifier for asphalt. In addition, liquid rubber is also widely used to make various coatings, such as low-temperature coatings, anti-corrosion coatings, electrical insulation coatings, water-soluble coatings a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F136/08C08F2/02C08F4/52
Inventor 蔡洪光张旭张学全姜连升毕吉福代全权张春雨那丽华范长亮贾翔宇
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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