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Method for producing C* petroleum resin with chlorine alumine acid ion liquid catalyzed polymerization

A technology of ionic liquid and petroleum resin, which is applied in the field of catalyzed polymerization of chloroaluminate ionic liquid to prepare light-colored C5 petroleum resin, which can solve the problems of long polymerization time, increased reaction rate, decreased yield and softening point, etc., and achieves easy reaction control, mild reaction process, and improved solubility

Active Publication Date: 2008-05-07
SINOPEC LANZHOU GASOLINEEUM CHEM IND CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently C 5 Petroleum resin production mostly uses pure anhydrous AlCl 3 or BF 3 The diethyl ether complex is a catalyst. Because the activity of the catalyst is too high, the cationic catalytic polymerization reaction is an exothermic reaction. If the heat of reaction cannot be removed in time, the reaction temperature will be too high, which will not only increase the volatilization loss of the reaction material, reduce the polymerization yield, but also make the The increase of the reaction rate will deepen the hue of the petroleum resin product and affect the quality of the product; at the same time, a large amount of gel will be generated, which will reduce the yield and softening point of the resin, and the hue will also be dark
[0003] Use solid AlCl 3 As a catalyst, there are many problems in production: 1. The polymerization time is too long, about 10 to 12 hours; 2. It is easy to cause sudden polymerization and overflow; 3. The consumption of catalyst is large; 4. The moisture content of raw materials Need to adjust with batch

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1, with 100 parts of C 5 Add the distillate into an open reactor protected by dry nitrogen, raise the temperature to 90°C, add 1.6 parts of chloroaluminate ionic liquid under stirring, continue to heat up to 120°C for polymerization for 6 hours, then raise the temperature to 150°C for 3 hours, A viscous liquid was obtained. Pour out the viscous liquid while it is hot, cool at room temperature, and the viscous liquid solidifies into a brittle solid. Use crushing equipment to crush the brittle solid into ultrafine powder below 400 mesh, and then soak it in 5 parts of 0.5% NaOH solution for 24 hours. The color of the resin changes from dark brown to light yellow. Partially watered, vacuum dried at 80°C and 150°C for 3 hours, respectively, to obtain light-colored C 5 petroleum resin.

[0018] Income C 5 The softening point of the petroleum resin is 102° C., the relative molecular mass is 1120, the Gardner color is 9, and the reaction conversion rate is 92%. ...

Embodiment 2

[0019] Example 2. Add 100 parts of C5 fraction into a dry and closed reactor, raise the temperature to 110°C, add 2.6 parts of chloroaluminate ionic liquid with stirring, raise the temperature to 130°C for polymerization for 6 hours, then continue to heat up to 150°C for 3 hours, A viscous liquid was obtained. The viscous liquid obtained above was poured out while it was hot, cooled at room temperature, and the viscous liquid solidified into a brittle solid. Use crushing equipment to crush the brittle solid into ultrafine powder below 400 mesh, and then soak it in 8 parts of 0.5% NaOH solution for 24 hours. After partially watering, vacuum-dry at 80°C and 150°C for 3 hours respectively to obtain light-colored C5 petroleum resin.

[0020] The obtained C5 petroleum resin has a softening point of 95° C., a relative molecular mass of 960, a Gardner color of 11, and a reaction conversion rate of 96%.

Embodiment 3

[0021] Example 3: Add 100 parts of C5 fraction into a dry and closed reactor, raise the temperature to 100°C, add 0.8 parts of chloroaluminate ionic liquid with stirring, raise the temperature to 150°C and polymerize for 6 hours to obtain a viscous liquid. The viscous liquid obtained above was poured out while it was hot, cooled at room temperature, and the viscous liquid solidified into a brittle solid. Use crushing equipment to crush the brittle solid into ultrafine powder below 400 mesh, then soak it in 10 parts of 0.5% NaOH solution for 24 hours, the color of the resin changes from dark brown to light yellow, then wash it with distilled water until neutral, filter to remove After partially watering, vacuum-dry at 80°C and 150°C for 3 hours respectively to obtain light-colored C5 petroleum resin.

[0022] The obtained C5 petroleum resin has a softening point of 112° C., a relative molecular mass of 1300, a Gardner color of 12, and a reaction conversion rate of 93%.

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Abstract

The present invention provides a method for preparing C5 petroleum resin by catalyzed polymerization of chloroaluminate ionic liquid. The method is to add the C5 fraction into a dry airtight or inert gas-protected reactor, raise the temperature to 90-120°C, and add the C5 fraction under stirring. Chloroaluminate ionic liquid with a mass of 0.8-3.0% is polymerized at 120-150°C for 6-10 hours to obtain a viscous liquid; cool the viscous liquid at room temperature to solidify the viscous liquid into a brittle solid and crush it into an ultra-fine powder below 400 meshes, then soaked in 0.5% NaOH solution for 20-24 hours, then washed with distilled water until neutral, filtered to remove most of the water, and vacuum-dried at 80°C and 150°C for 3 hours respectively to obtain Light colored C5 petroleum resin. The invention overcomes the phenomenon that the use of solid AlCl3 as a catalyst easily causes sudden polymerization and kettle overflow, the reaction process is mild, the reaction is easy to control, and the obtained C5 petroleum resin product has stable performance and light color.

Description

technical field [0001] The invention belongs to the field of petrochemical industry, and relates to a kind of chloroaluminate ionic liquid catalytic polymerization to prepare light-colored C 5 Petroleum resin method. Background technique [0002] C 5 Petroleum resin is cracked C by-product of ethylene plant 5 Distillation is the resin obtained after separation and polymerization of raw materials. due to C 5 The composition of fractions is complex, and it changes with the changes of cracking raw materials, cracking depth, cracking equipment and other factors. The composition of different sampling times also varies greatly, which makes the quality control of petroleum resins quite difficult. How to effectively control the softening point and reduce the hue of petroleum resin products during polymerization and post-treatment is the key to stabilizing and improving product quality. Currently C 5 Petroleum resin production mostly uses pure anhydrous AlCl 3 or BF 3 The die...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F240/00C08F4/14
Inventor 潘广勤卢灿辉王福善张耀亨夏和生李亮程嘉杰张军华徐惠俭齐永新崔树勋刘秀兰曹耀强毛兵肖军黄英张霖张英杰
Owner SINOPEC LANZHOU GASOLINEEUM CHEM IND CORP
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