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Method for terminating anionic polymerization reaction

An anionic polymerization and reaction technology, applied in the field of terminators, can solve the problems of terminator residues, alkali metal compound residues, etc.

Active Publication Date: 2022-05-13
IND TECH RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, initiators may cause alkali metal compounds to remain in the product, and terminators may remain in the product

Method used

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  • Method for terminating anionic polymerization reaction
  • Method for terminating anionic polymerization reaction

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Embodiment 1

[0043] Cyclohexane (100 mL) dehydrated was used as the reaction solvent and styrene (6 g) and butadiene (4 g) were used as comonomers, and the temperature was raised to 60° C. after stirring evenly. Add n-butyllithium (0.01g) as an initiator to carry out anionic polymerization reaction of styrene-butadiene copolymer. After reacting for 1 hour, cool down and take a sample to observe that the polymerization reaction liquid is orange-red, indicating that the polymer still maintains activity. After the active polymer solution was sampled to remove the solvent, it was dried in an oven at 100° C. for 2 hours, and its lithium metal concentration (122 ppm) was analyzed by an inductively coupled plasma atomic emission spectrometer (ICP-OES). Lignin (alkali lignin, purchased from Sigma-Aldrich's Lignin, alkali) is used as a terminator and metal remover for anionic polymerization and added to the active polymer solution, wherein the active polymer and lignin weight ratio is 100:5 , where...

Embodiment 2

[0045] Cyclohexane (100 mL) dehydrated was used as the reaction solvent and styrene (6 g) and butadiene (4 g) were used as comonomers, and the temperature was raised to 60° C. after stirring evenly. Add n-butyllithium (0.01 g) as an initiator to carry out anionic polymerization of styrene-butadiene copolymer. After reacting for 1 hour, the temperature was lowered and samples were taken to observe that the polymerization reaction solution was orange-red, indicating that the polymer still remained active. After the active polymer solution was sampled to remove the solvent, it was dried in an oven at 100° C. for 2 hours, and its lithium metal concentration (122 ppm) was analyzed by an inductively coupled plasma atomic emission spectrometer (ICP-OES). Diatomaceous earth (purchased from Sigma-Aldrich 545) as the terminator of anionic polymerization and metal removal agent and adding the solution of active polymer, wherein active polymer and diatomite weight ratio is 100:5, and wh...

Embodiment 3

[0047] Cyclohexane (100 mL) dehydrated was used as the reaction solvent and styrene (6 g) and butadiene (4 g) were used as comonomers, and the temperature was raised to 60° C. after stirring evenly. Add n-butyllithium (0.01g) as an initiator to carry out anionic polymerization reaction of styrene-butadiene copolymer. After reacting for 1 hour, cool down and take a sample to observe that the polymerization reaction liquid is orange-red, indicating that the polymer still maintains activity. After the active polymer solution was sampled to remove the solvent, it was dried in an oven at 100° C. for 2 hours, and its lithium metal concentration (122 ppm) was analyzed by an inductively coupled plasma atomic emission spectrometer (ICP-OES). Silica gel (Silica gel purchased from Sigma-Aldrich, particle size: 70 ~ 230mesh) is used as a terminator of anionic polymerization reaction and a metal remover and added to the solution of active polymer, wherein the weight ratio of active polymer ...

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Abstract

The invention relates to a method for terminating an anionic polymerization reaction, which comprises the following steps: mixing an organic alkali metal compound with a monomer containing double bonds, and carrying out an anionic polymerization reaction to form an active polymer; and adding a terminating agent to inactivate the active polymer wherein the terminating agent comprises a silicon oxide having a silanol group or a lignin having a hydroxyl group and a phenolic group.

Description

technical field [0001] The present disclosure pertains to methods of terminating anionic polymerization reactions, and more particularly to the terminators employed therefor. Background technique [0002] Anionic polymerization is often used to produce polydiene synthetic rubber, styrene-butadiene rubber, or thermoplastic elastomers, and is one of the important polymerization technologies. Polymers are suitable for tires, shoe materials, adhesives, sealing materials, or toughening agents, etc. [0003] Initiators and terminators are generally used in anionic polymerization reactions, and commonly used initiators include organic alkali metal compounds. The terminator can deactivate the active end of the polymer to achieve the purpose of terminating the reaction. However, initiators may cause alkali metal compounds to remain in the product, and terminators may remain in the product. [0004] To sum up, there is an urgent need for novel anionic polymerization terminators and...

Claims

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Application Information

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IPC IPC(8): C08F2/38C08F236/10C08F212/08
CPCC08F236/10C08F2/38C08F212/08
Inventor 谢峰铭王美华
Owner IND TECH RES INST
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