Norbornene, acrylics and octafluorocyclopentene ternary polymerization catalyst and ternary polymerization method

An octafluorocyclopentene ternary copolymerization catalyst and technology of ternary copolymerization catalysts, which are applied in the field of high polymers, can solve the problems of little research, low yield of copolymers, and low degree of alternation of copolymers, and achieve easy washing Separation, low reaction temperature, high catalytic efficiency

Inactive Publication Date: 2014-11-12

NINGBO UNIVERSITY OF TECHNOLOGY

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AI-Extracted Technical Summary

Problems solved by technology

These synthetic methods currently used have disadvantages such as long reaction time, low yield of copolymers...

Abstract

The invention relates to a norbornene, acrylics and octafluorocyclopentene ternary polymerization catalyst. The norbornene, acrylics and octafluorocyclopentene ternary polymerization catalyst is characterized in that Fe(6-[1-{(2-methyl)imino}ethyl]-2-acetylpyridine)Cl2, tris(n-butylcyclopentadienyl)yttrium, carbon tetrachloride and a first solvent are placed in an inertia dry single-opening glass bottle, the bottle opening is sealed through a latex tube, and the ternary polymerization catalyst is obtained after dissolution. Norbornene monomers, acrylics monomers and octafluorocyclopentene monomers are prepared according to the mole ratio of 1:1:1, the mixture is added to an inertia dry container, and a second solvent is added to the container so that the mixture can be dissolved. The ternary polymerization catalyst is added and reacts for 2 hours to 8 hours at the constant temperature of 30 DEG C to 90 DEG C, the product is poured into a methanol solution containing 4.5 wt% to 5.5 wt% of hydrochloric acid so that the copolymer can deposit, the sediment is washed through methyl alcohol to be neutral and then dried in vacuum, and then the norbornene, acrylics and octafluorocyclopentene terpolymer is obtained. Raw materials of the catalyst are low in price and can be easily obtained, the catalytic efficiency is high, the reaction temperature is low, and the copolymer yield is high.

Technology Topic

Ethyl phosphateSolvent +19

Examples

Experimental program(15)

Example Embodiment

[0019] Example 1

[0020] Take 0.01 mole of 2-acetyl-6-(2-methylbenzimidyl) ethyl pyridine iron chloride, 0.01 mole of tris(butylcyclopentadiene) yttrium, 0.01 mole of carbon tetrachloride and 20 ml of cyclohexane The ketone is put into a single-mouth glass bottle that has been evacuated and baked with nitrogen for many times, and the mouth of the bottle is sealed with a latex tube to obtain an iron-gadolinium complex catalyst.

[0021] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene, 0.01 mole of tert-butyl methacrylate and 0.01 mole of octafluorocyclopentene monomer into a single-port glass that has been evacuated and baked with nitrogen for many times In the bottle, add 5ml cyclohexanone to dissolve. Take the iron-gadolinium complex catalyst according to the amount of 2-acetyl-6-(2-methylbenzimidyl)ethylpyridinium chloride as 1% of the total weight of the three monomers, and inject the above mixture with a syringe Put the single-mouth glass bottle into a constant temperature water tank and react at 40°C for 2 hours. The product was poured into a methanol solution containing 5% hydrochloric acid to precipitate the copolymer. The precipitate was washed to the center with methanol and dried under vacuum to obtain bicyclo[2,2,1]hept-2-ene and tert-butyl methacrylate. With octafluorocyclopentene terpolymer, the reaction yield is 57.8%.

[0022] The reaction yield is the weight of the terpolymer/(the total weight of the norbornene-based monomer, the acrylate-based monomer and the octafluorocyclopentene)×100%.

[0023] The calculation method of the reaction yield in the following examples is the same.

Example Embodiment

[0024] Example 2

[0025] Take 0.01 mole of 2-acetyl-6-(2-methylbenzimidyl) ethyl pyridine iron chloride, 0.08 mole of tris(butylcyclopentadiene) yttrium, 0.05 mole of carbon tetrachloride and 20 ml of toluene. Put it into a single-mouth glass bottle that has been evacuated and baked with nitrogen for many times, and the mouth of the bottle is sealed with a latex tube to obtain the iron-gadolinium complex catalyst.

[0026] Add 0.01 moles of 1-methylbicyclo[2,2,1]hept-2-ene, 0.01 moles of ethyl acrylate and 0.01 moles of octafluorocyclopentene monomer into a single port that has been vacuumed and baked with nitrogen for many times In a glass bottle, add 5ml of toluene to dissolve. Take the iron-gadolinium complex catalyst according to the amount of 2-acetyl-6-(2-methylbenzimidyl)ethylpyridinium chloride as 4% of the total weight of the three monomers, and inject the above mixture into the syringe , Put the single-mouth glass bottle in a constant temperature water tank and react at 70°C for 4 hours. The product was poured into a methanol solution containing 5% hydrochloric acid to precipitate the copolymer. The precipitate was washed to the center with methanol and dried under vacuum to obtain 1-methylbicyclo[2,2,1]hept-2-ene and ethyl acrylate. With octafluorocyclopentene terpolymer, the reaction yield is 66.7%.

Example Embodiment

[0027] Example 3

[0028] Take 0.01 mole of 2-acetyl-6-(2-methylbenzimidyl) ethyl pyridine iron chloride, 0.05 mole of tris(butylcyclopentadiene) yttrium, 0.04 mole of carbon tetrachloride and 20 ml of toluene. Put it into a single-mouth glass bottle that has been evacuated and baked with nitrogen for many times, and the mouth of the bottle is sealed with a latex tube to obtain the iron-gadolinium complex catalyst.

[0029] Add 0.01 moles of bicyclo[2,2,1]hept-2-ene, 0.01 moles of methyl methacrylate and 0.01 moles of octafluorocyclopentene into a single-mouth glass bottle that has been evacuated and baked with nitrogen for many times. Add 5ml toluene to dissolve. Take the iron-gadolinium complex catalyst according to the amount of 2-acetyl-6-(2-methylbenzimidyl)ethylpyridinium chloride as 3% of the total weight of the three monomers, and inject the above mixture with a syringe Put the single-mouth glass bottle in a constant temperature water tank and react at 90°C for 8 hours. The product was poured into a methanol solution containing 5% hydrochloric acid to precipitate the copolymer. The precipitate was washed to the center with methanol and dried in vacuum to obtain bicyclo[2,2,1]hept-2-ene, methyl methacrylate and octadecanoate. The fluorocyclopentene terpolymer has a reaction yield of 88.9%.

PUM

Description & Claims & Application Information

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Classification and recommendation of technical efficacy words

high yield
Easy to wash and separate

Reactor for production of chlorine dioxide, methods of production of same, and related systems and methods of using the reactor

ActiveUS20050244328A1high yieldreduce risk

Owner:FKOS LLC +1

Norbornene, acrylics and octafluorocyclopentene ternary polymerization catalyst and ternary polymerization method

AI-Extracted Technical Summary

Problems solved by technology

Abstract

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

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