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Method for continuously preparing block/star-shaped polymer on basis of tubular reaction device

A tubular reaction device and a star-shaped polymer technology are applied in the field of continuous preparation of block/star polymers based on a tubular reaction device, and can solve the problems of low conversion rate and complex method.

Inactive Publication Date: 2018-02-23
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

[0008] The purpose of the present invention is to provide a method for continuously preparing block / star polymers based on a tubular reaction device in order to solve the technical problems of low conversion rate and complex methods of the existing methods for preparing block / star polymers

Method used

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  • Method for continuously preparing block/star-shaped polymer on basis of tubular reaction device
  • Method for continuously preparing block/star-shaped polymer on basis of tubular reaction device
  • Method for continuously preparing block/star-shaped polymer on basis of tubular reaction device

Examples

Experimental program
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Effect test

Embodiment 1

[0043] The refined first monomer isoprene distilled from the raw material tank, the refined n-hexane distilled from the raw material tank and the n-butyllithium solution (concentration 1.6mol / L) were respectively adjusted according to the flow rate of 1L / H, 60L / H, 10mL / H enters the first static reactor from the respective raw material tanks, and reacts at 50°C for 120 minutes to obtain an active polymer; the inner diameter of the first static reactor is 3 mm, and the length is 20 meters. In a static reactor, the included angle of the first 5 meters of mixing blades is 90°, and the angle of the rear 15 meters of mixing blades is 45°;

[0044] The active polymer obtained is continuously entered into the second static reactor, and the coupling agent divinylbenzene in the second monomer or the coupling agent tank is added at the same time, the flow rate is 50mL / H, and the reaction is carried out at 50°C for 60min, the product After flowing out, the polyisoprene star-shaped polyme...

Embodiment 2

[0047] Isoprene, n-hexane and catalyst n-butyllithium (concentration 1.6mol / L) are respectively entered in the first static reactor according to the flow rate of 15L / H, 90L / H, and 150mL / H from respective raw material tanks, React at 50°C for 90 minutes to obtain an active polymer; the inner diameter of the first static reactor is 3 mm and the length is 20 meters. In the first static reactor, the angle of the first 5 meters of mixing blades is positive Intersection 90°, the angle of the last 15 meters of mixing blades is 45°;

[0048] The obtained active polymer is continuously put into the second static reactor, and the second monomer butadiene in the second monomer tank is added at the same time, the flow rate is 500mL / H, and the reaction is carried out at 50°C for 45min. After the product flows out, it is passed through methanol The block polymer is obtained after settling out; the inner diameter of the second static reactor is 3 millimeters, and the length is 12 meters. In ...

Embodiment 3

[0051] Isoprene, butadiene, n-hexane and catalyst n-butyllithium (concentration 1.6mol / L) are respectively according to the flow rate of 10L / H, 10L / H, 120L / H, 100mL / H from the respective raw material tanks Enter the first static reactor and react at 50°C for 60 minutes to obtain active polymer; the inner diameter of the first static reactor is 3 mm and the length is 20 meters. In the first static reactor, the first 5 The included angle of the mixing blade for 1m is 90°, and the angle of the mixing blade for the last 15m is 45°;

[0052] The active polymer obtained is continuously entered into the second static reactor, and the coupling agent divinylbenzene in the second monomer or the coupling agent tank is added at the same time, the flow rate is 500mL / H, and the reaction is carried out at 50°C for 30min, the product Obtain the star-shaped polymer after flowing out through methanol precipitation; The inner diameter of the second static reactor is 3 millimeters, and the length...

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Abstract

The invention provides a method for continuously preparing a block / star-shaped polymer on the basis of a tubular reaction device and belongs to the field of a polymer compounding method. According tothe method, a first static reactor and a second static reactor in the tubular reaction device are utilized to react; the sectional variable angle crossing blades in the first static reactor and the second static reactor and the size and connecting mode of the reactors are designed according to the characteristics of anionic polymerization reaction; a micro-channel reactor is combined with the reactors, so that the reaction speed and yield in the reaction process can be promoted; compared with intermittent kettle reaction, the reaction has the advantage that the reaction rate is increased by about 30 times; the device is capable of achieving 200 tons / year output and finally realizing the preparation for narrow distributed block / star-shaped polymer; the method is capable of realizing continuous stable production on the basis of the characteristics of the tubular reaction and promoting the product batch stability.

Description

technical field [0001] The invention belongs to the field of polymer synthesis methods, in particular to a method for continuously preparing block / star polymers based on a tubular reaction device. Background technique [0002] The star polymer prepared by anionic polymerization has a wide range of applications, mainly in the field of special rubber and additives. The industrial preparation of anionic polymerized block / star polymers is also a research hotspot in the chemical industry this year. The structure of the polymerization kettle for continuous polymerization is closely related to the reaction steps and product characteristics of anionic polymerization. The structure of the polymerization kettles of major rubber companies in the world has its own characteristics. [0003] USP3807422 of Phiiilps Company of the United States has developed a continuous solution polymerization reactor. Three stirrers are installed in the middle of the reactor, and the lower one is a six-b...

Claims

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Application Information

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IPC IPC(8): C08F293/00C08F297/04C08F2/01
Inventor 周光远聂赫然苏小龙张丽黄河张文铎
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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