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Polmerization method of catalysis chain transfer for methyl methacrylate

A methyl methacrylate, catalyzed chain transfer technology, which is applied in the field of organic polymerization, can solve the problems of not using microwave technology, etc., and achieve the effect of increasing the chain transfer constant, increasing the reaction speed, and speeding up the reaction speed

Inactive Publication Date: 2007-05-09
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no report on the use of microwave technology in the catalytic chain transfer polymerization of methyl methacrylate.

Method used

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  • Polmerization method of catalysis chain transfer for methyl methacrylate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: Catalyzed chain transfer polymerization of methyl methacrylate with 5,10,15,20-tetraphenyl-21H, 23H-cobaltpurine (CoP) as a catalytic chain transfer reagent under microwave irradiation:

[0018] Monomer methyl methacrylate (methyl methacrylate, MMA, Shanghai Reagent Company) was washed with deionized water to neutrality after being washed with alkali to colorless, and then used by vacuum distillation after drying with anhydrous magnesium sulfate; the initiator azobis Isobutyronitrile (AIBN, Shanghai Reagent Company) was recrystallized twice with ethanol and then dried in vacuum at room temperature; the catalytic chain transfer reagent CoP was purchased directly from Aldrich; the rest of the reagents were products of Shanghai Reagent Factory, and were used after being treated by the usual method.

[0019] The polymerization device adopts the single-mode microwave reactor of the Discover series of the American CEM company. The microwave radiation power is adj...

Embodiment 2

[0025] Embodiment two: Catalyzed chain transfer polymerization of methyl methacrylate with bis(boron trifluoride) bis(diphenyl)cobaloxime (CoPhBF) as catalytic chain transfer reagent under microwave irradiation

[0026] Monomer methyl methacrylate (Shanghai Reagent Company) was purified by vacuum distillation after alkali washing, water washing and drying. The initiator azobisisobutyronitrile (AIBN) was purified by recrystallization from ethanol. Phenylcobaloxime was synthesized according to literature method (Andreja BakaE, Mark E.Brynildson, and James H.Espenson, Inorganic Chemistry, 1986, 25, 4108-4114).

[0027] Methyl methacrylate and toluene were sparged with argon for three hours and then transferred to an anaerobic operating box. Add 50ml toluene to 2.8mg CoPhBF to make a catalyst solution. 60 mg of AIBN was dissolved in a mixed solution of 12 ml of methyl methacrylate and 18 ml of toluene to prepare an initiator solution. Add 5ml initiator solution in each reaction...

Embodiment 3

[0033] Embodiment three: Catalytic chain transfer polymerization of methyl methacrylate with bis(boron trifluoride) bis(dimethyl)cobaloxime (CoBF) as catalytic chain transfer reagent under microwave irradiation

[0034] Monomer methyl methacrylate (Shanghai Reagent Company) was purified by vacuum distillation after alkali washing, water washing and drying. The initiator azobisisobutyronitrile (AIBN) was purified by recrystallization from ethanol. Methylcobaloxime was synthesized according to literature method (Andreja BakaE, Mark E. Brynildson, and James H. Espenson, Inorganic Chemistry, 1986, 25, 4108-4114).

[0035] Methyl methacrylate and toluene were sparged with argon for three hours and then transferred to an anaerobic operating box. Add 50ml of toluene to 2.8mg of CoBF to make a catalyst solution. 60 mg of AIBN was dissolved in a mixed solution of 12 ml of methyl methacrylate and 18 ml of toluene to prepare an initiator solution. Add 5ml of initiator solution to each...

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Abstract

The present invention discloses a catalytic chain transfer polymerization method of methyl methacrylate. It is characterized by that said method includes the following steps: adding methyl methacrylate and solvent, the described solvent is selected from toluene, 2-butanone and methyl alcohol, in the presence of initiator and catalytic chain transfer agent using microwave to make continuous irradiation, reaction temp. is 40-70 deg.C and reaction time is above 1.5 min. and the weight ratio of monomer methyl methacrylate and catalyst is 10 to the power 7:1-10 to the power 5:1. The adoption of said method cna make the chain transfer constant of catalytic chain transfer agent by high, and its reaction speed be obviously raised.

Description

technical field [0001] The invention relates to a method for polymerizing organic matter, in particular to a catalytic chain transfer polymerization method for methyl methacrylate. Background technique [0002] Catalytic chain transfer polymerization is a very effective method to control the molecular weight of polymers. The advantage of this method is that a polymer with controllable molecular weight and unsaturated double bonds at the end can be obtained by using a small amount of catalytic chain transfer reagent, and the obtained polymer can be used as a macromonomer, which can be further connected with other monomers. branch or block copolymerization. The amphiphilic graft or block copolymer obtained by this polymerization method has been widely used in coatings, ink modification and other fields. [0003] Considering the problem of wastewater treatment caused by using water as the medium, bulk polymerization or solution polymerization is usua...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/14C08F2/38C08F2/06
Inventor 朱秀林王刚朱健程振平
Owner SUZHOU UNIV
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