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Preparation method of butyl methacrylate-dimethylaminoethyl methacrylate block copolymer

A technology of dimethylaminoethyl methacrylate and butyl methacrylate, which is applied in the field of polymer chemistry, can solve the problems of high cost, catalyst residue in polymers, and large amount of catalyst, so as to achieve low production cost and solve the problem of durability. Reduction of heat and aging resistance, effect of ease of handling

Active Publication Date: 2013-09-25
青冈县三通新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved in the present invention is: in order to overcome the problems that the amount of catalyst used in the process of preparing PBMA-b-PDMAEMA by ATRP in the prior art is large, the cost is high, and the obtained polymer has catalyst residues, a method for preparing butyl methacrylate is provided. Method for ester-dimethylaminoethyl methacrylate block copolymer

Method used

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  • Preparation method of butyl methacrylate-dimethylaminoethyl methacrylate block copolymer
  • Preparation method of butyl methacrylate-dimethylaminoethyl methacrylate block copolymer
  • Preparation method of butyl methacrylate-dimethylaminoethyl methacrylate block copolymer

Examples

Experimental program
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Effect test

Embodiment 1

[0023] (1) Polymerization formula: The molar ratio of monomer (BMA), initiator (AIBN), and 1,1-diphenylethylene is 100:0.4:0.8, and toluene equal to 50% of the total mass is added as a solvent.

[0024] Polymerization step: Add 50g (0.35mol) of BMA monomer, 0.2310g (0.0014mol) of initiator AIBN, 0.5070g (0.0028mol) of 1,1-diphenylethylene into a 250mL four-necked flask equipped with a thermometer and a magnetic stirrer ), the solvent toluene 50g, mixed evenly, the system was repeatedly evacuated and argon flowed three times, and reacted at 70°C for 25h.

[0025] Purification of polybutyl methacrylate: After the reaction, the solvent in the system was removed by rotary evaporation until the liquid in the rotary evaporator stopped dripping, and a colorless, transparent and slightly viscous product was obtained. The product after rotary evaporation was dropped into excess methanol to precipitate, filtered, and the obtained precipitate was added to chloroform to dissolve completel...

Embodiment 2

[0030] The PBMA synthesized in step (1) of Example 1 was used as the macroinitiator, and the mass ratio of PBMA and DMAEMA was 1:5, and then 50% of the total amount of butyl acetate was added as a solvent.

[0031] Polymerization step: Add 10g of PBMA, 50g of monomer DMAEMA, and 20g of butyl acetate into a 100mL four-neck flask equipped with a thermometer and a magnetic stirrer. ℃ under the reaction 6h.

[0032] Purification of butyl methacrylate-dimethylaminoethyl methacrylate block copolymer: after the reaction, the solvent in the system was removed by rotary evaporation to obtain a colorless, transparent and viscous product. Rotate the product in a rotary evaporator to remove the solvent until the liquid in the rotary evaporator no longer drips, drop the product after rotary evaporation into excess petroleum ether to precipitate, filter, and add the obtained precipitate to THF Completely dissolve, then drop the THF solution of the precipitate into excess petroleum ether to p...

Embodiment 3

[0034] (1) Polymerization formula: The molar ratio of monomer (BMA), initiator (AIBN), and 1,1-diphenylethylene is 100:1:2, and butyl acetate equal to 50% of the total mass is added as a solvent.

[0035] Polymerization step: Add 50g (0.35mol) of BMA monomer, 0.2310g (0.0035mol) of initiator AIBN, 0.5070g (0.0070mol) of DPE, 50g of solvent toluene into a 250mL four-neck flask equipped with a thermometer and a magnetic stirrer, and mix Evenly, react at 75°C for 20h.

[0036] Purification of polybutyl methacrylate: After the reaction, the solvent in the system was removed by rotary evaporation until the liquid in the rotary evaporator stopped dripping, and a colorless, transparent and slightly viscous product was obtained. The product after rotary evaporation was dropped into excess methanol to precipitate, filtered, and the obtained precipitate was added to chloroform to dissolve completely, then, the precipitate chloroform solution was dropped into excess methanol to precipita...

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Abstract

The invention relates to a preparation method of a butyl methacrylate-dimethylaminoethyl methacrylate block copolymer. A polybutyl methacrylate precursor is obtained through a reaction among a reaction system monomer BMA (butyl methacrylate), an initiator AIBN, a molecular weight regulator 1,1-diphenylethlene and a solvent; the polybutyl methacrylate precursor is used as an initiator of the dimethylaminoethyl methacrylate reaction; and the butyl methacrylate-dimethylaminoethyl methacrylate block copolymer is obtained by heating polymerization. Compared with the butyl methacrylate-dimethylaminoethyl methacrylate block copolymer prepared by an ATRP (atom transfer radical polymerization) method, the preparation method of a butyl methacrylate-dimethylaminoethyl methacrylate block copolymer, provided by the invention, has the advantages of simple reaction conditions, easiness in operation, low production cost and no residue of inorganic catalyst, is favorable for industrial production, and has a broad application prospect in the field of coating dispersants.

Description

technical field [0001] The invention relates to the technical field of polymer chemistry, in particular to a preparation method of a butyl methacrylate-dimethylaminoethyl methacrylate block copolymer. Background technique [0002] Amphiphilic block copolymers refer to copolymers composed of hydrophilic and lipophilic segments. Amphiphilic polymers have become one of the current research hotspots in the field of polymer science due to their special properties. This type of polymer forms a micellar structure with the hydrophilic segment as the shell and the hydrophobic segment as the core in water. Then the "reverse micelles" with the opposite structure are formed. Studies have shown that micelles may also form regular aggregates through further assembly. Amphiphilic block copolymers can promote the mixing of water phase and oil phase, and are widely used in the fields of surfactants and dispersants. [0003] At present, the well-developed method for synthesizing block copol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F220/18C08F220/34C08F2/38C08F4/04
Inventor 任强王莉莉李坚汪称意
Owner 青冈县三通新材料科技有限公司
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