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Preparation method of halogenated butyl rubber

A technology of halogenated butyl rubber and butyl rubber, applied in the field of preparation of halogenated butyl rubber, can solve the problems of difficult co-vulcanization of butyl rubber, poor bonding performance, low degree of unsaturation, etc.

Active Publication Date: 2016-06-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to its low unsaturation and slow vulcanization speed, butyl rubber is difficult to co-vulcanize with other general-purpose high-unsaturation rubbers; in addition, butyl rubber has poor bonding performance with other general-purpose high-unsaturation rubbers and metals. These disadvantages limit the application of butyl rubber

Method used

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  • Preparation method of halogenated butyl rubber
  • Preparation method of halogenated butyl rubber

Examples

Experimental program
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Effect test

Embodiment

[0048] In the following examples and comparative examples, the analysis of stearic acid and calcium stearate in halogenated butyl rubber was carried out by the coating method for infrared spectrum analysis and testing, and the instrument was a Nicolet 560 Fourier transform infrared spectrometer. Choose carbon disulfide as the solvent, prepare the sample into a concentrated solution of 45-55 mg / ml, and then directly coat the solution on the potassium bromide wafer, let it stand for 4 minutes, let the solvent evaporate, and then conduct infrared spectrum testing. Scan 32 times with a resolution of 4cm -1 .

[0049] The structural characterization of halogenated butyl rubber was carried out using an AVANCE 400MHz NMR spectrometer from Bruker, Switzerland, with a magnetic field strength of 9.40 Tesla and a sample tube diameter of 5 mm. The sample was dissolved in deuterated chloroform at room temperature to prepare a solution with a mass content of 2%, with TMS as the internal sta...

Embodiment 2

[0055] Put 400 g of butyl rubber solution in a 1 L three-necked flask, add 4 g of water and 0.168 g of sodium bicarbonate and stir evenly. After heating the obtained solution to 30°C, add 1.6g of bromine under the condition of avoiding light, stir rapidly for 300s, add 50ml of 0.2mol / L NaOH aqueous solution, continue to stir for 5min, remove most of the solvent by steam, and then pass it through an open mill Remove moisture and residual solvent to obtain bromobutyl rubber product. The resulting product structure and calcium stearate and stearic acid content results are shown in Table 1.

Embodiment 3-11

[0057] Repeat embodiment 2, just change the add-on of sodium bicarbonate and water. The product structure of each bromobutyl rubber obtained and the results of calcium stearate and stearic acid content are shown in Table 1.

[0058] Table 1

[0059]

[0060] Each symbol "n.d" in the table means not detected.

[0061] From the results of Comparative Example 1 in Table 1, when sodium bicarbonate was not introduced into the bromination reaction system, the presence of calcium stearate could not be detected in the brominated butyl rubber product obtained after the bromination reaction was completed. In contrast, 0.22% by weight of stearic acid was detected in the resulting product. This content is equivalent to the calcium stearate content added in the butyl rubber solution, that is to say, the calcium stearate has been completely converted into stearic acid. Comparative Example 1 also shows that stearic acid is difficult to be neutralized by NaOH aqueous solution, and unneu...

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Abstract

The invention relates to a preparation method of halogenated butyl rubber. The preparation method comprises following steps: a) a solution containing butyl rubber is reacted with a halogenating reagent so as to obtain a halogenated butyl rubber solution; and b) the halogenated butyl rubber solution is subjected to post-processing so as to recycle halogenated butyl rubber. In the step of a), halogenation reaction is carried out in the presence of water and a weak alkaline substance which is taken as an acid scavenger, and water amount accounts for 0.05 to 5.0wt% of the weight amount of the solution containing butyl rubber. The preparation method is used for preparing halogenated butyl rubber from butyl rubber, so that stearate dispersing agents contained by butyl rubber are basically not converted into stearic acids after halogenation, and it is ensured that normal halogenation reaction of butyl rubber is not influenced.

Description

technical field [0001] The invention relates to a preparation method of halogenated butyl rubber. The preparation of the halogenated butyl rubber by this method can prevent the stearate dispersant contained in the butyl rubber from being substantially converted into stearic acid after halogenation, while ensuring that the normal halogenation reaction of the butyl rubber is not affected. Background technique [0002] Butyl rubber is a synthetic rubber obtained by copolymerizing isobutylene and a small amount of isoprene, referred to as IIR. Compared with other general-purpose rubbers, butyl rubber is characterized by good air tightness, and is widely used in the manufacture of inner tubes, medical rubber plugs, vulcanizing bladders, etc. The production of butyl rubber generally adopts a slurry process. The monomers of isobutylene and isoprene are cationic polymerized in methyl chloride to obtain a copolymer. The polymerization temperature is generally -90°C to -100°C. After...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F210/12C08F8/22C08K3/26
Inventor 徐宏德华炜王冬萍邱迎昕包巧云钟林
Owner CHINA PETROLEUM & CHEM CORP