Chlorinated butyl rubber synthesizing process

A chlorinated butyl rubber and synthesis process technology, which is applied in the field of chemical synthesis, can solve problems such as high energy consumption, difficult product quality, and product processability decline, and achieve low energy consumption, simple equipment, and reduced occurrence of transposition side reactions The effect of the probability

Active Publication Date: 2012-11-14
ZHEJIANG CENWAY MATERIALS CO LTD +1
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  • Abstract
  • Description
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Problems solved by technology

[0003] The route of the chlorination reaction of butyl rubber is very short and the mechanism is not complicated. However, due to the high viscosity of the reaction system and the existence of rapid series side reactions, it is still very difficult to accurately control the reaction process and obtain high-quality products.
Specifically, the product chlorinated butyl rubber is prone to the conversion of substituted chlorine from the secondary position to the primary position in the presence of chlorine and hydrogen chloride. If this process cannot be blocked in time, the processability of the product will decline rapidly.
At present, the synthesis of chlorobutyl rubber is mainly carried out in strongly stirred tank reactors. On the one hand, this technology brings high energy consumption to the production process, and on the other hand, it is difficult to To ensure product quality without adding additives, this has also led to no major breakthroughs in the synthesis of chlorobutyl rubber in my country for decades

Method used

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  • Chlorinated butyl rubber synthesizing process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] according to figure 1 The flow chart of the butyl rubber n-hexane solution with a concentration of 25wt% and a concentration of 10wt% Cl 2 The normal hexane solution and lye are 10wt% sodium hydroxide aqueous solution as raw materials; wherein the unsaturation of butyl rubber is 1.9%, Cl 2 Cl in n-hexane solution 2 The molar ratio to the double bond in butyl rubber is 0.7, NaOH and Cl 2 The molar ratio is 1:1. The temperature of each feed is 30oC; The flow velocity in the follow-up pipeline of the first pipeline reactor is 0.3m / s, and the residence time is 60 seconds; The flow velocity in the follow-up pipeline of the second pipeline reactor is 0.3m / s, and the residence time is 300 seconds. The product chlorinated butyl rubber has a chlorination degree of 2%, a secondary chlorine content of 70%, an unsaturation of 0.5%, a rubber number average molecular weight of 180,000 Daltons, and a molecular weight distribution PDI of 2.5.

Embodiment 2

[0020] according to figure 1 The flow chart of the butyl rubber n-heptane solution with a concentration of 5wt% and a concentration of 8wt% Cl 2 The n-heptane solution and the 2wt% sodium hydroxide aqueous solution as the lye are raw materials. Butyl rubber has an unsaturation of 1.2%. Cl 2 Cl in n-heptane solution 2 The molar ratio to the double bond in butyl rubber is 1.1, NaOH and Cl 2 The molar ratio is 2:1. The temperature of each feed is 20oC; the flow velocity in the follow-up pipeline of the first pipeline reactor is 1m / s, and the residence time is 10 seconds; the flow velocity in the follow-up pipeline of the second pipeline reactor is 1m / s, and the residence time is 60 seconds . The product chlorinated butyl rubber has a chlorination degree of 0.8%, a secondary chlorine content of 99%, a degree of unsaturation of 0.5%, a rubber number average molecular weight of 230,000 Daltons, and a molecular weight distribution PDI of 1.9.

Embodiment 3

[0022] according to figure 1 The flow chart of the butyl rubber n-octane solution with a concentration of 5wt% and a concentration of 2wt% Cl 2 The n-octane solution and the 0.1wt% sodium hydroxide aqueous solution as the lye are raw materials. Butyl rubber has an unsaturation of 3.0%. Cl 2 Cl in n-octane solution 2 The molar ratio of the double bonds in the raw material butyl rubber is 2.0, NaOH and Cl 2 The molar ratio is 1.5:1. The temperature of each feed is 50oC; the flow velocity in the follow-up pipeline of the first pipeline reactor is 2m / s, and the residence time is 6 seconds; the flow velocity in the follow-up pipeline of the second pipeline reactor is 2m / s, and the residence time is 20 seconds . The product chlorinated butyl rubber has a chlorination degree of 1.2%, a secondary chlorine content of 99%, a degree of unsaturation of 1.2%, a rubber number average molecular weight of 220,000 Daltons, and a molecular weight distribution PDI of 2.3.

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Abstract

The invention discloses a chlorinated butyl rubber synthesizing process and belongs to the technical field of chemical synthesis. The chlorinated butyl rubber synthesizing process includes two series processes, namely butyl rubber chlorination and neutralization of chlorinated mixed liquid. The process utilizes a pipeline type reactor to enable a C12 alkane solution and a butyl rubber alkane solution to be mixed and perform the chlorination, then utilizes the other pipeline type reactor and introduces alkali liquor into the reactor to start neutralization reaction after the solution stays for 6-60 seconds in a follow-up pipeline, and finishes the reaction after reaction solution stays for 20-300 seconds in the follow-up pipeline. The process has the advantages that the reaction speed is quick, the reaction time is short and can be accurately controlled, the conversion from a main product replaced by meso-position chlorine to a by-product replaced by primary-position chlorine is inhibited, and indexes of an obtained product are excellent.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a synthesis process of chlorinated butyl rubber. Background technique [0002] Chlorinated butyl rubber is obtained by chlorination of butyl rubber. Chlorination occurs in the isoprene part of butyl rubber, requiring most of the substitution reaction of chlorine, so that the double bond of butyl rubber is better preserved. , which can be used for further rubber processing. The majority of chlorobutyl rubber is a saturated butyl skeleton, which has many characteristics of butyl molecules, especially low air and moisture permeability, good shock absorption, good aging resistance and weather resistance in atmospheric environment, etc. In addition, chlorobutyl rubber also has a series of advantages such as fast vulcanization speed, co-vulcanization with other rubbers, more heat resistance, and small compression deformation. Therefore, it has a wide range of u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F210/12C08F8/22
Inventor 骆广生任纪文吕阳成代俊明王凯
Owner ZHEJIANG CENWAY MATERIALS CO LTD
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