Preparation method of liquid polybutadiene with wide molecular weight distribution

A liquid polybutadiene, wide molecular weight distribution technology, applied in the field of preparation of liquid polybutadiene, can solve the problems of unfavorable industrial production, difficult conversion rate control, uneven molecular weight distribution, etc.

Active Publication Date: 2022-04-26
LIMING RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The relative molecular mass distribution of polybutadiene prepared by this method presents a bimodal distribution, the molecular weight distribution is uneven, and it is difficult to control the conversion rate of the monomer after the first initiation, which is not conducive to industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Under the protection of nitrogen, add 98g of tetrahydrofuran and 1000~1600g of n-hexane to the dry and sealed 5L reaction kettle in sequence, start stirring and stir well. After the temperature in the kettle reaches -10℃, add 10~30g of butadiene and 10~ 20g of the prepared n-butyllithium n-hexane solution was polymerized. After an interval of 10-25min, the n-hexane solution of butadiene and n-butyllithium was repeatedly added. After all the n-butyllithium was added, the remaining butadiene Diene until all butadiene is added, the total amount of butadiene is 360g, the amount of n-butyllithium is 0.11mol, and the number of additions of n-butyllithium is 11 times. During the whole process, the temperature was controlled at -10-10°C. After the reaction pressure no longer changes, continue the reaction for 20-30 minutes, add a terminator, continue stirring for 10-30 minutes, stop the reaction, filter the feed liquid and transfer it to a washing kettle for washing, and then a...

Embodiment 2

[0020] Under the protection of nitrogen, add 98g of tetrahydrofuran and 1000~1600g of n-hexane to the dry and sealed 5L reaction kettle in sequence, start stirring and stir well, after the temperature in the kettle reaches -10℃, add 10~20g of butadiene and 5~ 10g of n-butyllithium n-hexane solution prepared for polymerization reaction, after an interval of 10~25min, repeatedly add butadiene and n-butyllithium n-hexane solution, when n-butyllithium is completely added, continue to add the remaining butadiene Diene until all butadiene is added, the total amount of butadiene is 360g, the amount of n-butyllithium is 0.11mol, and the number of additions of n-butyllithium is 13 times. During the whole process, the temperature was controlled at -10-10°C. After the reaction pressure no longer changes, continue the reaction for 20-30 minutes, add a terminator, continue stirring for 10-30 minutes, stop the reaction, filter the feed liquid and transfer it to a washing kettle for washing,...

Embodiment 3

[0022] Under the protection of nitrogen, add 98g of tetrahydrofuran and 1000~1600g of n-hexane to the dry and sealed 5L reaction kettle in sequence, start stirring and stir well, after the temperature in the kettle reaches -10℃, add 10~20g of butadiene and 5~ 10g of n-butyllithium n-hexane solution prepared for polymerization reaction, after an interval of 10~25min, repeatedly add butadiene and n-butyllithium n-hexane solution, when all n-butyllithium is added, continue to add the remaining butane ene until all butadiene is added, the total amount of butadiene is 300g, the amount of n-butyllithium is 0.11mol, and the number of additions of n-butyllithium is 15 times. During the whole process, the temperature was controlled at -10-10°C. After the reaction pressure no longer changes, continue the reaction for 20-30 minutes, add a terminator, continue stirring for 10-30 minutes, stop the reaction, filter the feed liquid and transfer it to a washing kettle for washing, and then ad...

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Abstract

The invention relates to a preparation method of liquid polybutadiene with wide molecular weight distribution, which comprises the following steps: adopting organic lithium as an initiator, adding a polarity regulator and a solvent, adding butadiene and organic lithium in batches to carry out anionic polymerization reaction, after the organic lithium is completely added, continuously adding the residual butadiene into a reaction kettle to carry out reaction, and after the polymerization is finished, cooling to room temperature to obtain the liquid polybutadiene with wide molecular weight distribution. Adding a terminator to terminate the reaction; the butadiene and the organic lithium are fed in batches, the single-time feeding amount of the butadiene is 2-10% of the total mass of the butadiene, the single-time feeding amount of the organic lithium is 5-15% of the total mass of the organic lithium, the adding frequency of the organic lithium is 8-20, and the next-time feeding of the butadiene and the organic lithium is carried out after the butadiene added in the previous time completely reacts. The reaction conditions are mild, the molecular weight distribution of polybutadiene can be regulated and controlled by changing the feeding times and the single feeding amount of the initiator to obtain uniform single-peak width distribution, and the prepared product has good mechanical properties and processability.

Description

technical field [0001] The invention relates to the field of polymer synthesis, in particular to a method for preparing liquid polybutadiene with wide molecular weight distribution. Background technique [0002] Anionic polymerization generally uses organolithium as the initiator. Since the polymerization process only has chain initiation and chain growth, it is called "living polymerization". Because it can effectively realize the molecular structure design of the polymer, it is often used for the polymerization of butadiene Reacting. Polybutadiene has three microstructures: cis-1,4-structure, trans-1,4-structure, and 1,2-structure. The 1,2-structure content of polybutadiene can be adjusted by controlling additives and polymerization temperature, so that polybutadiene with different vinyl content can be prepared, which is widely used in adhesives, coatings and high-performance rubber and other fields . [0003] The molecular weight distribution of a polymer can affect it...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F136/06C08F4/48
CPCC08F136/06C08F2500/04C08F2500/055C08F4/48Y02T10/86
Inventor 孙亮亮张进李亚婷蒿银伟符立言
Owner LIMING RES INST OF CHEM IND
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