Method for preparing butyl rubber polymer

Abstract

The invention relates to a method for preparing a butyl rubber polymer. In the method, a mixture of C4-C8 monoolefine monomer and C4-C14 polyene monomer serving as a main material is subjected to polymerization at the temperature of between -90 and -70 DEG C and in absence of water and oxygen by taking the mixture of ionized water, hexane and monoalkyl aluminum dihalide as a catalyst and the mixture of methyl chloride and hexane as a solvent to form the butyl rubber polymer. The method has the advantages of simplicity, high polymerization temperature, low cost, high stability and initiation efficiency of the catalyst, high number average molecular weight of a product, high conversion rate and narrow molecular weigh distribution.

Description

technical field

[0001] The present invention relates to a kind of preparation method of butyl rubber polymer, specifically, adopt the mixture of deionized water and hexane and monoalkyl aluminum dihalide as catalyst, take methyl chloride and hexane mixture as solvent, use C 4 ~C 8 monoolefin monomer and C 4 ~C 14 The multi-olefin monomer mixture is used as a raw material, and the polymerization reaction is carried out at a temperature of -90°C to -70°C under anhydrous and oxygen-free conditions to form a butyl rubber polymer, which belongs to the field of chemical industry. Background technique

[0002] Butyl rubber is considered a copolymer of an isoolefin and one or more, preferably conjugated, multiolefins as comonomers. Butyl rubber polymer generally has two preparation methods: solution method and slurry method. The solution method is to prepare butyl rubber polymer in solution, using an aluminum trihalide catalyst system, and using aluminum trichloride or aluminum t...

Examples

Embodiment 1

[0025] Add 48.6 μl of deionized water into 13.9ml of hexane solvent and mix evenly, then add 2.7ml of methyl aluminum dichloride at a temperature of 25°C to make a mixed catalyst with a concentration of 0.16mol / l, keep it warm for later use, Mix 60ml of methyl chloride and 240ml of hexane to make a mixed solvent, mix 70g of isobutene and 30g of isoprene under anhydrous and oxygen-free conditions to make a mixed raw material, then add the above mixed solvent to the above mixed raw material, Cool to -70°C and then add 16.6ml of mixed catalyst, continue to carry out the polymerization reaction at -70°C under anhydrous and oxygen-free conditions to generate butyl rubber polymer, wash the polymer with methanol, and dry it in a vacuum oven at 45 °C evaporated to constant weight to obtain butyl rubber polymer product.

Embodiment 2

[0027] Add 52.2 μl of deionized water into 8.7ml of hexane solvent and mix evenly, then add 2.2ml of ethyl aluminum dichloride at a temperature of 0°C to make a mixed catalyst with a concentration of 0.18mol / l, keep it warm for later use, Mix 90ml of methyl chloride and 210ml of hexane to make a mixed solvent. Under anhydrous and oxygen-free conditions, mix 80g of 2-methyl-1-butene and 20g of butadiene to make a mixed raw material, and then mix the above Add the solvent to the above mixed raw material, cool to -75°C and then add 10.9ml of mixed catalyst, continue to carry out polymerization reaction at -75°C under anhydrous and oxygen-free conditions to form butyl rubber polymer, wash the polymer with methanol , evaporated to constant weight at 45°C in a vacuum oven to obtain a butyl rubber polymer product.

Embodiment 3

[0029] Add 8.6 μlg of deionized water into 4.0ml of hexane solvent and mix evenly, then add 0.4ml of ethylaluminum dichloride at -20°C to make a mixed catalyst with a concentration of 0.08mol / l, and keep it warm for later use , mix 30ml of methyl chloride with 270ml of hexane to make a mixed solvent, and mix 45g of isobutene and 45g of 2-methyl-1-butene with 5g of isoprene and 5g of butadiene under anhydrous and oxygen-free conditions , to make a mixed raw material, then add the above mixed solvent to the above mixed raw material, cool to -80°C and then add 4.4ml of mixed catalyst, continue to carry out polymerization reaction at -80°C under anhydrous and oxygen-free conditions to form butyl For rubber polymer, the polymer was washed with methanol, and evaporated to constant weight in a vacuum oven at 45°C to obtain a butyl rubber polymer product.

technical field

[0001] The present invention relates to a kind of preparation method of butyl rubber polymer, specifically, adopt the mixture of deionized water and hexane and monoalkyl aluminum dihalide as catalyst, take methyl chloride and hexane mixture as solvent, use C 4 ~C 8 monoolefin monomer and C 4 ~C 14 The multi-olefin monomer mixture is used as a raw material, and the polymerization reaction is carried out at a temperature of -90°C to -70°C under anhydrous and oxygen-free conditions to form a butyl rubber polymer, which belongs to the field of chemical industry. Background technique

[0002] Butyl rubber is considered a copolymer of an isoolefin and one or more, preferably conjugated, multiolefins as comonomers. Butyl rubber polymer generally has two preparation methods: solution method and slurry method. The solution method is to prepare butyl rubber polymer in solution, using an aluminum trihalide catalyst system, and using aluminum trichloride or aluminum t...

Examples

Embodiment 1

[0025] Add 48.6 μl of deionized water into 13.9ml of hexane solvent and mix evenly, then add 2.7ml of methyl aluminum dichloride at a temperature of 25°C to make a mixed catalyst with a concentration of 0.16mol / l, keep it warm for later use, Mix 60ml of methyl chloride and 240ml of hexane to make a mixed solvent, mix 70g of isobutene and 30g of isoprene under anhydrous and oxygen-free conditions to make a mixed raw material, then add the above mixed solvent to the above mixed raw material, Cool to -70°C and then add 16.6ml of mixed catalyst, continue to carry out the polymerization reaction at -70°C under anhydrous and oxygen-free conditions to generate butyl rubber polymer, wash the polymer with methanol, and dry it in a vacuum oven at 45 °C evaporated to constant weight to obtain butyl rubber polymer product.

Embodiment 2

[0027] Add 52.2 μl of deionized water into 8.7ml of hexane solvent and mix evenly, then add 2.2ml of ethyl aluminum dichloride at a temperature of 0°C to make a mixed catalyst with a concentration of 0.18mol / l, keep it warm for later use, Mix 90ml of methyl chloride and 210ml of hexane to make a mixed solvent. Under anhydrous and oxygen-free conditions, mix 80g of 2-methyl-1-butene and 20g of butadiene to make a mixed raw material, and then mix the above Add the solvent to the above mixed raw material, cool to -75°C and then add 10.9ml of mixed catalyst, continue to carry out polymerization reaction at -75°C under anhydrous and oxygen-free conditions to form butyl rubber polymer, wash the polymer with methanol , evaporated to constant weight at 45°C in a vacuum oven to obtain a butyl rubber polymer product.

Embodiment 3

[0029] Add 8.6 μlg of deionized water into 4.0ml of hexane solvent and mix evenly, then add 0.4ml of ethylaluminum dichloride at -20°C to make a mixed catalyst with a concentration of 0.08mol / l, and keep it warm for later use , mix 30ml of methyl chloride with 270ml of hexane to make a mixed solvent, and mix 45g of isobutene and 45g of 2-methyl-1-butene with 5g of isoprene and 5g of butadiene under anhydrous and oxygen-free conditions , to make a mixed raw material, then add the above mixed solvent to the above mixed raw material, cool to -80°C and then add 4.4ml of mixed catalyst, continue to carry out polymerization reaction at -80°C under anhydrous and oxygen-free conditions to form butyl For rubber polymer, the polymer was washed with methanol, and evaporated to constant weight in a vacuum oven at 45°C to obtain a butyl rubber polymer product.

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