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Resource-saving preparation method of isoolefine and conjugated diene copolymer

A conjugated diene and resource-saving technology is applied in the field of resource-saving preparation of isoolefin and conjugated diene copolymers, and can solve the problems of easy scaling, inability to provide low-temperature reaction solvents, and difficulty in promotion and development.

Inactive Publication Date: 2010-09-29
江苏圣杰实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (2) The equipment investment for industrial production of butyl rubber is very high. In addition to the cost of circulating cooling equipment accounting for 35% of the total investment, the reactor itself is also very expensive
[0005] (3) In the production of butyl rubber, the glue coating of the polymer will increase the temperature in the reactor, and it is difficult to ensure stable quality
First, the discharge screw is a single-screw extruder, which is prone to fouling and therefore cannot be operated continuously for long periods of time
Second, the liquid reaction solvent is forced back to the reactor by gravity rather than being removed from the material stream first, thereby not providing an opportunity to purify the liquid reaction solvent, or to interfere with polymerization if the reaction solvent is returned directly to the reactor process, it does not provide the opportunity to use the low temperature reaction solvent for other cooling purposes
[0010] However, this solution polymerization reactor is only suitable for operation under lower viscosity conditions, thus limiting the single-pass conversion rate of isobutylene monomer and the increase of glue concentration. The conversion rate is only 20-30%, and the monomer concentration is only 10%. %, so the energy and raw materials consumed per unit product are very high, and the production efficiency of the device is low, which makes it difficult to promote and develop this method so far

Method used

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  • Resource-saving preparation method of isoolefine and conjugated diene copolymer
  • Resource-saving preparation method of isoolefine and conjugated diene copolymer
  • Resource-saving preparation method of isoolefine and conjugated diene copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] 50% by mass of mixed monomer [containing 98.3% by mass of isobutylene and 1.7% by mass of isoprene] and 50% by mass of solvent (containing a mixed solvent of n-hexane and dichloromethane with a mass ratio of 70:30) were injected into the single The body is configured in the kettle 5, and the temperature is lowered to the polymerization temperature of -50°C by circulating a low-temperature (-70°C) cold medium. Then it is continuously transported to reactor 1 in sections through lines 5a, 5b and 5c. After a stable circulation flow is established at each section, the mass ratio of the mixed monomer solution added to the three sections is 1:1:1. Threaded elements ensure that individual streams can be separated.

[0064] Use 10 per mole (mixed) monomer -6 moles of diethylaluminum chloride (catalyst), 5×10 -7 moles of tert-butyl chloride (initiator), 10 -6 Moles of triethylamine (electron donor) and 1 liter of mixed solvent containing n-hexane and dichloromethane with a ma...

Embodiment 2

[0068] The present embodiment is the same as the preparation process and conditions of Example 1, and the difference is that the ingredients are formulated according to the following formula,

[0069] Inject 20% by mass of mixed monomer (containing 90% by mass of isobutylene and 10% by mass of isoprene) and 80% of solvent (containing a mixed solvent of butane and methyl chloride with a mass ratio of 80:20) into the monomer configuration Kettle 5 is fed into reactor 1 continuously at 3 points via lines 5a, 5b and 5c.

[0070] 10 per mole of monomer -7 moles of aluminum trichloride as catalyst, 10 -8 molar water as initiator, 10 -6 Moles of N, N-dimethylaniline as the electron donor and 1 liter of mixed solvent containing butane and methyl chloride with a mass ratio of 80:20 are continuously fed into the reactor 1 through the line 4a as the catalyst solution. The copolymerization reaction temperature is -100°C. The molecular weight (Mn) of the copolymer was 1.196 million / mol...

Embodiment 3

[0072] The present embodiment is the same as the preparation process and conditions of Example 1, and the difference is that the ingredients are formulated according to the following formula,

[0073] 40% by mass of mixed monomer (isoprene containing 98% of isobutylene and 2% by mass of mixed monomer) and 60% of solvent (containing a mixed solvent of n-hexane and dichloromethane with a mass ratio of 60:40) At the same time, it is continuously conveyed to reactor 1 via lines 5a, 5b and 5c.

[0074] 3×10 per mole of monomer -5 mol of dichloroethylaluminum catalyst, 2×10 -6 moles of tert-butyl acetate as initiator, 6×10 -5 Moles of 2,6-di-tert-butylpyridine as the electron donor and 1 liter of mixed solvent containing n-hexane and dichloromethane with a mass ratio of 60:40 as the catalyst solution were continuously fed into the reactor 1 through the line 4a.

[0075] The copolymerization reaction temperature was -60°C. The molecular weight (Mn) of the copolymer was 308,000 / mo...

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Abstract

The invention relates to a resource-saving method for preparing an isoolefine and conjugated diene copolymer. The method comprises the steps as follows: an isoolefine monomer and a conjugated diene monomer, a solvent, a catalyzer and an accessory ingredient are put in an extrusion reactor, an unloading extruder and a postprocessing extruder system which are connected in three stages in series forcontinuous solution polymerization, termination, wash, devolatilization and post processing. The process units involved in the method are advanced; the process flow is short; the resource-saving method is very controllable; the resource-saving method significantly saves resources and investment compared with the traditional art; the total energy consumed is reduced by more than 50 percent; the product quality is stable; the production cycle is short; the environment is not polluted.

Description

technical field [0001] The invention relates to the field of preparing polymers, in particular to a resource-saving method for preparing isoolefin and conjugated diene copolymers. Background technique [0002] The main species of isoolefin and conjugated diene copolymer is isobutylene and isoprene copolymer (referred to as butyl rubber). Since the advent of butyl rubber, because of its low air permeability, good air tightness, heat aging resistance, deep Widely concerned by countries all over the world. Early butyl rubber production usually uses Friedel-Craft cationic catalysts, and industrial production is carried out in the polymerization solvent methyl chloride at a very low polymerization temperature (-100 ° C). Since butyl rubber is insoluble in methyl chloride, it forms a polymerization There are some disadvantages in this slurry production process, [0003] (1) The energy consumption in the manufacturing process is very large, mainly due to the huge energy consumpti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F210/12C08F2/01C08F2/06C08F6/06
Inventor 刘祖安王志鸿葛瑞思兰茜
Owner 江苏圣杰实业有限公司
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