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A kind of molecular weight regulator for emulsion polymerization and preparation method thereof

A technology of molecular weight regulator and emulsion polymerization, which is applied in ether preparation, ester reaction preparation of ether, organic chemistry, etc. It can solve the problems of poor molecular weight adjustment ability, solubility drop, unfavorable environmental protection, etc., to increase the diffusion rate and facilitate the synthesis process , The effect of simple reaction mechanism

Active Publication Date: 2022-04-05
JILIN INST OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As the thiol carbon chain grows, its solubility in water decreases sharply, which will lead to limited transfer of chain transfer agents to latex particles
Due to the decrease of the rate of diffusion from the water phase, the reaction rate of the monomer in the latex particles is very fast, so that the concentration of the chain transfer agent in the latex particles is lower than the concentration at the thermodynamic equilibrium, which eventually leads to a decrease in the regulation efficiency of the chain transfer agent.
[0008] In summary, the problems in the prior art are: (1) the molecular weight regulator tert-dodecyl mercaptan used in the existing emulsion polymerization has an unpleasant stench, which is not conducive to environmental protection
[0009] (2) The solubility of tert-dodecyl mercaptan in water is small, and when emulsion polymerization is carried out, the chain transfer agent is not easy to diffuse into the latex particles
[0010] (3) As a chain transfer agent, tert-dodecyl mercaptan has no emulsifying function and no ability to protect colloid
[0011] Difficulty in solving the above-mentioned technical problems: Compared with tert-dodecyl mercaptan, the prepared molecular weight regulator has slightly poor molecular weight regulation ability during emulsion polymerization

Method used

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  • A kind of molecular weight regulator for emulsion polymerization and preparation method thereof
  • A kind of molecular weight regulator for emulsion polymerization and preparation method thereof
  • A kind of molecular weight regulator for emulsion polymerization and preparation method thereof

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preparation example Construction

[0049] The preparation method of the molecular weight regulator for the emulsion polymerization that the embodiment of the present invention provides comprises:

[0050] Carry out Williamson etherification reaction of polyethylene glycol monomethyl ether and 2-bromo-3-pentanol in N,N-dimethylformamide solvent to obtain 2-polyethylene glycol monomethyl ether-3-pentanol crude Product, polyethylene glycol monomethyl ether and dodecyl trithiopropionic acid, with N, N-dimethylformamide as solvent, in dicyclohexylcarbodiimide (DCC) and 4-dimethyl A catalytic system composed of aminopyridine (DMAP) was used for esterification to obtain a crude product of polyethylene glycol monomethyl ether monododecyl trithiopropionate. The two crude products were separated and purified by column chromatography to obtain two Different types of low odor, all of them are molecular weight regulators with emulsifying function.

[0051] Specifically include:

[0052] In the presence of a catalyst, poly...

Embodiment 1

[0062] The preparation method of the tasteless, water-soluble and emulsifying molecular weight regulator provided by the embodiment of the present invention comprises the following steps:

[0063] The first step is to use polyethylene glycol monomethyl ether with different degrees of polymerization as raw materials to carry out etherification reaction with 2-bromo-3-pentanol. The specific method is: a 1000mL three-neck round bottom flask is equipped with a dropping funnel , reflux condenser and magnetic stirring, add 500mL of N,N-dimethylformamide, then add polyethylene glycol monomethyl ether and 2-bromo-3-pentanol, react according to the amount of substances 1:1.5 , such as adding 190 grams of polyethylene glycol monomethyl ether with an average molecular weight of 1900, 25 grams of 2-bromo-3-pentanol, and adding 20.7 grams of anhydrous K 2 CO 3 Carry out catalysis, heat to 60-70°C and stir the reaction, and monitor the reaction by pointing the plate at any time. The reacti...

Embodiment 2

[0068] The preparation method of the low-odor, water-soluble and emulsifying molecular weight regulator provided by the embodiments of the present invention comprises the following steps:

[0069] In the first step, add 35 grams of polyethylene glycol monomethyl ether with a molecular weight of 350 and 2-bromo-3-pentanol and 200 ml of N,N-dimethylformamide solvent into a 1000 ml reflux device In the three-necked flask, add 20.7 grams of anhydrous K 2 CO 3Carry out catalysis, heat to 65°C and stir the reaction, react for 6 hours, remove the solvent N,N-dimethylformamide by rotary evaporation, and use chromatographic column to separate and purify to obtain 2-polyethylene glycol monomethyl ether-3-pentanol Make chain transfer agent 3.

[0070] In the second step, 35 grams of polyethylene glycol monomethyl ether, 54.6 grams of dodecyl trithiopropionic acid and 200 ml of N,N-dimethylformamide solvent with a molecular weight of 350 are added to the reflux device In a 1000ml three...

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Abstract

The invention belongs to the technical field of molecular weight regulators, and discloses a molecular weight regulator for emulsion polymerization and a preparation method thereof. In the formamide solvent, the etherification reaction is carried out to obtain the 2-polyethylene glycol monomethyl ether-3-amyl alcohol crude product, and the polyethylene glycol monomethyl ether and the dodecyl trithiopropionic acid are mixed with N, N- Dimethylformamide is used as a solvent, and esterification is carried out in a catalytic system composed of dicyclohexylcarbodiimide and 4-dimethylaminopyridine to obtain polyethylene glycol monomethyl ether monododecyl trithiopropionate The crude product, the two crude products were separated and purified by column chromatography. The synthesis process of the invention is easy, the yield is high, there is no bad smell of mercaptan, and at the same time, it has different degrees of water solubility, exists in the water phase of the emulsion polymerization, is more easily diffused into the latex particles, increases the diffusion rate, and has protection The ability of colloid has a certain emulsifying ability.

Description

technical field [0001] The invention belongs to the technical field of molecular weight regulators, in particular to a molecular weight regulator for emulsion polymerization and a preparation method thereof. Background technique [0002] At present, in chain polymerization reactions, such as free radical polymerization, ring-opening polymerization, coordination polymerization and cationic addition polymerization reactions, in addition to chain initiation, chain growth, chain termination and other elementary reactions, it is often accompanied by chain transfer reactions. occur. [0003] In actual production, it is very common to apply the principle of chain transfer to control molecular weight. For example, the molecular weight of polyvinyl chloride is mainly determined by the transfer to the monomer, which is controlled by temperature; the molecular weight of styrene-butadiene rubber is regulated by tert-dodecyl mercaptan as a chain transfer agent; solution polymerization i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F2/38C08F136/06C08G65/334C08G65/337C07C43/11C07C41/16C07C329/00
CPCC08F2/38C08F136/06C08G65/337C08G65/3344C07C43/11C07C41/16C07C329/00C08G2650/04
Inventor 刘长玲宋岩佀庆波付雁杨洪雨
Owner JILIN INST OF CHEM TECH
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