Initiator complex for copolymerization of styrene and butadiene and polymerization method

A technology of butadiene and styrene is applied in the field of preparation of initiator complexes for initiating the copolymerization of styrene and butadiene to achieve the effect of mature technology and simple process

Active Publication Date: 2017-11-14
青岛竣翔科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Although this invention can also realize random copolymerization and even uniform random copolymerization of styrene and butadiene (that is, the styrene units are evenly distributed in the macromolecular chain), what this invention uses is THF and potassium alkoxide. system, and potassium alkoxide is used as an auxiliary agent in the polymerization system, and as a component of the initiator, it is not mentioned that it is used to form a complex with the initiator

Method used

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  • Initiator complex for copolymerization of styrene and butadiene and polymerization method
  • Initiator complex for copolymerization of styrene and butadiene and polymerization method
  • Initiator complex for copolymerization of styrene and butadiene and polymerization method

Examples

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Effect test

example 1

[0031] Under the protection of nitrogen, quickly add 100ml of 0.5M sec-butyl lithium hexane solution and 1ml of 0.05M t-BuOK THF solution to the dry initiator reactor successively, place it in a 60°C water bath and stir for 30min to obtain Initiator complexes for the copolymerization of styrene and butadiene.

[0032] Under the protection of nitrogen, add organic solvent, styrene and organic solvent dissolved in butadiene to the dry and deoxygenated autoclave, the total monomer concentration of styrene and butadiene is 30g / 100mL, in the total monomer Butadiene content is 70%, add A 8.0×10 -5 mol / 100mL polymerization solution, react at 50°C for 1 h, then add the initiator complex for preparing styrene and butadiene copolymerization, the ratio of the molar number of Li in the initiator complex to the gram number of monomer added is 7× 10 -6 mol / g, react at 50°C for 2 hours, stop with ethanol, condense the polymer with excess ethanol, wash and extrude with steam, and dry in vac...

Embodiment 2

[0040] Under the protection of nitrogen, quickly add 100ml of 10M n-butyllithium hexane solution and 10ml of 0.1M t-BuOK THF solution to the dry initiator reactor successively, place it in a water bath at 10°C and stir for 60min to obtain the used Initiator complex for copolymerization of styrene and butadiene.

[0041] Under the protection of nitrogen, add organic solvent, styrene and organic solvent dissolved in butadiene to the dry and deoxygenated autoclave, the total monomer concentration of styrene and butadiene is 20g / 100mL, in the total monomer Butadiene content is 80%, add A 2.0×10 -4 mol / 100mL polymerization liquid, react at 30°C for 0.5h, then add the initiator complex for preparing styrene and butadiene copolymerization, the molar ratio of Li in the initiator complex to the gram number of monomer added is 2 ×10 -5 mol / g, react at 30°C for 4 hours, stop with ethanol, condense the polymer with excess ethanol, wash and extrude with steam, and dry in vacuum to obtain s...

example 3

[0046] Under the protection of nitrogen, quickly add 50ml of 2M sec-butyllithium hexane solution and 10ml of 0.1M t-BuOK THF solution to the dry initiator reactor successively, place it in a water bath at 30°C and stir for 240min to obtain the used Initiator complex for copolymerization of styrene and butadiene.

[0047] Under the protection of nitrogen, add organic solvent, styrene and organic solvent dissolved in butadiene to the dry and deoxygenated autoclave, the total monomer concentration of styrene and butadiene is 10g / 100mL, in the total monomer Butadiene content is 50%, add A 5.0×10 -5 mol / 100mL polymerization solution, react at 70°C for 20min, then add the initiator complex for preparing styrene and butadiene copolymerization, the ratio of the molar number of Li in the initiator complex to the gram number of monomer added is 4× 10 -6 mol / g, react at 70°C for 1 hour, stop with ethanol, coagulate the polymer with excess ethanol, wash and extrude with steam, and dry i...

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Abstract

The invention relates to an initiator complex for the copolymerization of styrene and butadiene and a polymerization method. The components of the initiator complex and the proportion thereof are as follows: (A) organic lithium: the general formula is RLi, wherein R is a C1-C6 alkyl group, a C3-C12 cycloalkyl group, a C7-C14 aralkyl group or a C6-C12 aryl group; and n-butyllithium or sec-butyllithium is preferred; (B) potassium alkyloxide: comprising at least one of potassium tert-butoxide, 1,1-potassium dimethylpropyloxide and 1,1-potassium dimethylamyloxide; and the molar ratio of the component A to the component B of B to A is equal to 1 to (100 to 100000). The composition of the initiator disclosed by the invention is added with a component and a novel preparation method is established, and the highly effective initiator is prepared under the specified dosing sequence and proportion by the way of aging. Under the mode of polymerization after impurity pre-removal, the initiator can be used for synthesizing styrene butadiene rubber, of which the styrene monomer is uniformly and irregularly distributed in macromolecular chains.

Description

technical field [0001] The invention belongs to the preparation of an initiator complex for initiating the copolymerization of styrene and butadiene, a preparation method and a method for preparing a copolymer of styrene and butadiene. Background technique [0002] There are many literature reports on the random copolymerization of styrene-butadiene rubber. The main method is to change the relative reactivity of the two monomers, or to control the raw material ratio of the two monomers in the system. Generally speaking, there are four commonly used methods: high temperature copolymerization, adding randomizer, adjusting monomer addition speed and constant monomer concentration method. However, the present invention proposes a brand-new concept of realizing random copolymerization, and prepares styrene-butadiene random copolymers by preparing initiator complexes for initiating the copolymerization of styrene and butadiene. The initiator complex contains multiple active cent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F236/10C08F4/48C08F4/46
CPCC08F236/10C08F2410/04C08F4/461
Inventor 张杰王萌李龙王鸿飞左继强
Owner 青岛竣翔科技有限公司
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