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Method of controlling halogen substitution site in halogenated butyl rubber

A technology of halogenated butyl rubber and butyl rubber, applied in the field of chemical industry, can solve the problems of poor quality of halogenated butyl rubber, and achieve the effect of excellent indicators

Active Publication Date: 2013-12-25
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the current production process of halogenated butyl rubber, there is no effective means to suppress the transformation of halogen substituents, resulting in poor quality of the final halogenated butyl rubber

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Use butyl rubber with a degree of unsaturation of 1.9% to configure a butyl rubber n-hexane solution with a concentration of 3.2wt%, add water to it to a content of 1.1wt%, and obtain a uniform emulsion after fully stirring; pass chlorine gas into the emulsion Chlorination reaction, Cl 2 The molar ratio to the double bond in butyl rubber is 0.8:1, the reaction time is 0.2 minutes, and the temperature is 15°C; then add sodium hydroxide aqueous solution rapidly to the reaction system to control the concentration of sodium hydroxide and Cl 2 The molar ratio of the amount added is 2.3:1, the reaction temperature is 15°C, stirred, and left to stand; the alkane solution of the upper layer of chlorinated butyl rubber is taken out, washed, added with a stabilizer, and the substitution of chlorine is measured by NMR after drying. The results showed that the chlorination degree (mass fraction of chlorine in rubber) of the product was 1.09%, the mole fraction of secondary chlorine...

Embodiment 2

[0022] Use butyl rubber with a degree of unsaturation of 1.9% to configure a butyl rubber n-hexane solution with a concentration of 3.2wt%, add water to it to a content of 5wt%, and obtain a uniform emulsion after fully stirring; add a concentration of 16wt% to the emulsion % Cl 2 The n-hexane solution of the chlorination reaction, wherein the Cl 2 The molar ratio to the double bond in butyl rubber is 0.81:1, the reaction time is 2 minutes, and the temperature is 25°C; after that, potassium hydroxide aqueous solution is quickly added to the reaction system to control the relationship between potassium hydroxide and Cl 2 The molar ratio of the amount added is 2.2:1, the reaction temperature is 25°C, stirred, and left to stand; the alkane solution of the upper layer of chlorinated butyl rubber is taken out, washed, added with a stabilizer, and the substitution of chlorine is measured by NMR after drying. The results showed that the chlorination degree of the product was 1.17%, ...

Embodiment 3

[0024] Use butyl rubber with an unsaturation degree of 1.9% to configure a butyl rubber n-hexane solution with a concentration of 20wt%, add water to it to a content of 2wt%, and obtain a uniform emulsion after fully stirring; add a concentration of 5.0wt% to the emulsion %Br 2 The n-hexane solution carries out the bromination reaction, wherein the Br 2 The molar ratio to the double bond in butyl rubber is 1.1:1, the reaction time is 1 minute, and the temperature is 25°C; then quickly add sodium hydroxide aqueous solution to the reaction system to control the relationship between sodium hydroxide and Br 2 The molar ratio of the amount added is 2.3:1, the reaction temperature is 25°C, stirred, and allowed to stand; the alkane solution of the upper layer of bromobutyl rubber is taken out, washed, added with a stabilizer, and the substitution of bromine is measured by NMR after drying. The results show that the degree of bromination (mass fraction of bromine in the rubber) of th...

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Abstract

The invention discloses a method of controlling a halogen substitution site in halogenated butyl rubber, belonging to the technical field of chemistry and chemical engineering. The method comprises the following steps of: firstly, adding a certain amount of water into alkane liquor of butyl rubber, uniformly mixing to form emulsion; then, mixing the emulsion with a halogen to carry out halogenation reaction, in-situ extracting and halogenating haloid acid generated in the halogenation reaction process by utilizing water in the system to achieve the effect of lowering acid concentration in an organic phase to inhibit halogen substitution site transformation (transforming a secondary site into a primary site); and finally, ending the reaction process by using alkaline liquor to neutralize reaction liquid. The process is characterized in that a substitution site transformation phenomenon is effectively inhibited by introducing an appropriate amount of water (mass fraction of water being controlled to 0.5%-5.0%) into the reaction liquid, primary-site halogen mole fraction in a product is greater than 98%, halogenation degree (halogen mass fraction) can be regulated and controlled, degree of unsaturation and Mooney viscosity indexes are excellent, and conditions are provided for producing high-quality halogenated butyl rubber.

Description

technical field [0001] The invention belongs to the technical field of chemistry and chemical engineering, in particular, the invention relates to the halogenation technology and method of butyl rubber. Background technique [0002] With the development of science and technology, chemical engineering technology is constantly developing in the direction of high efficiency, energy saving and safety. In order to achieve the goal of sustainable development and comprehensive utilization of resources and energy, many new requirements are put forward for the chemical production process. In 1937, Exxon Company prepared butyl rubber. In 1953, people developed the halogenation method of butyl rubber. Compared with traditional butyl rubber, halogenated butyl rubber has better heat resistance, acid and alkali resistance, vulcanization activity, and co-existence with other rubbers. It has obvious advantages in mixing and regeneration performance, and is the main raw material for high-gra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F210/12C08F8/22
Inventor 骆广生王凯吕阳成
Owner TSINGHUA UNIV
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