A kind of method that takes C9 fraction as raw material to prepare petroleum resin

A petroleum resin and raw material technology, applied in the field of petroleum resin preparation, can solve the problems of petroleum resin performance degradation, difficulty in catalyst removal, and influence on post-treatment process, etc., achieve stable performance, solve emulsification phenomenon, and easy control of reaction

Active Publication Date: 2017-10-24
抚顺科隆化工实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

where BF 3 Easy to store, easy to use, can increase the melting point of the resin at a lower temperature, easy to remove from the polymer, and easy to realize continuous production, moderate activity, lighter resin color, but more expensive; AlCl 3 The polymerization activity is higher than that of BF 3 , the softening point and yield of the resin are high, and the cost is low, the source is wide, the sewage treatment in the production is easy, but the catalyst is difficult to remove, and it is easy to form a gel with the alkali during neutralization and is not easy to remove from the reaction solution. The resin is darker in color and more corrosive to equipment
In the production process, catalyst removal is a key link. If the catalyst is not removed cleanly, it will not only lead to a decline in the performance of the petroleum resin, but also affect the entire post-treatment process.

Method used

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  • A kind of method that takes C9 fraction as raw material to prepare petroleum resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Dissolve 1 g of the template agent cetyltrimethylammonium bromide (CTAB) in 200 ml of deionized water, and stir in a water bath at 40°C. Then add 5ml of ammonia water, dropwise add 40g of tetraethyl orthosilicate, and add 4g of aluminum isopropoxide at the same time, then stir in a 40°C water bath for 4h. Then the liquid was transferred to a polytetrafluoroethylene-lined stainless steel reactor, crystallized at 80°C for 72 hours, filtered, washed with distilled water until neutral, and dried. Finally, it was put into a muffle furnace and calcined at 450°C for 6 hours to remove the template agent and obtain Al-MCM-41.

[0022] 5 g of the Al-modified MCM-41 carrier obtained above was added to 30 ml of 20% phosphotungstic acid ethanol solution, stirred at room temperature for 12 hours, and separated by filtration. Dry at 80°C for 8 hours, and bake at 450°C for 3 hours. An Al-MCM-41 molecular sieve-loaded phosphotungstic acid catalyst with a silicon-aluminum ratio of 10 a...

Embodiment 2

[0024] Dissolve 1 g of the template agent cetyltrimethylammonium bromide (CTAB) in 200 ml of deionized water, and stir in a water bath at 40°C. Then 5ml of ammonia water was added, 40g of ethyl orthosilicate was added dropwise, and 0.8g of aluminum isopropoxide was added at the same time, and then stirred in a water bath at 40°C for 4h. Then the liquid was transferred to a polytetrafluoroethylene-lined stainless steel reactor, crystallized at 80°C for 72 hours, filtered, washed with distilled water until neutral, and dried. Finally, put it into a muffle furnace and bake it at 500°C for 6 hours to remove the template agent to obtain Al-MCM-41.

[0025] 5 g of the Al-modified MCM-41 carrier obtained above was added to 30 ml of phosphotungstic acid ethanol solution with a mass fraction of 35%, stirred at room temperature for 18 hours, and separated by filtration. Dry at 100°C for 10 hours and bake at 500°C for 3 hours. An Al-MCM-41 molecular sieve-loaded phosphotungstic acid ca...

Embodiment 3

[0027] Dissolve 1 g of the template agent cetyltrimethylammonium bromide (CTAB) in 200 ml of deionized water, and stir in a water bath at 40°C. Then, 5ml of ammonia water was added, 40g of tetraethyl orthosilicate was added dropwise, and 0.4g of aluminum isopropoxide was added at the same time, and then stirred in a water bath at 40°C for 4h. Then the liquid was transferred to a polytetrafluoroethylene-lined stainless steel reactor, crystallized at 80°C for 72 hours, filtered, washed with distilled water until neutral, and dried. Finally, put it into a muffle furnace and bake it at 550°C for 6 hours to remove the template agent, and obtain Al-MCM-41.

[0028] 5 g of the Al-modified MCM-41 carrier obtained above was added to 30 ml of 50% phosphotungstic acid ethanol solution, stirred at room temperature for 24 hours, and separated by filtration. Dry at 110°C for 12 hours and bake at 550°C for 3 hours. An Al-MCM-41 molecular sieve-loaded phosphotungstic acid catalyst with a si...

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Abstract

The invention discloses a method for preparing petroleum resin with C9 fraction as the raw material, and aims at providing the preparation method which can increase the yield of petroleum resin, shorten the reaction time, improve product quality, improve the postprocessing process and reduce environment pollution generated by postprocessing. The method is technically characterized by including the steps of firstly, using n-heptane accounting for 15-25% of the volume of the raw material as solvent, adding the raw material and the solvent into a reactor with a stirring device, and adding phosphotungstic acid, loaded on an Al-MCM-41 molecular sieve, as a catalyst, wherein the use amount of the catalyst accounts for 1-3% of the mass of the raw material; secondly, adding nitrogen for replacement, starting stirring, setting the pressure in a kettle to be 0.4-0.9 MPa, heating the mixture to 60-100 DEG C, unceasingly stirring the mixture for 5-10 hours at the temperature, pressing out crude petroleum resin through nitrogen after the reaction is completed, conducting normal-temperature reduced pressure distillation, recycling solvent, and obtaining the C9 petroleum resin.

Description

technical field [0001] The invention provides a method for preparing petroleum resin, specifically, a method for preparing petroleum resin with C9 fraction as raw material. Background technique [0002] C9 petroleum resin is a thermoplastic resin obtained by polymerizing C9 distillate, a by-product of cracking ethylene plant, in the presence of a catalyst, or copolymerizing it with aldehydes, aromatic hydrocarbons, and terpenes. Its molecular mass is generally less than 2000, its softening point is less than 150°C, and it is a thermoplastic viscous liquid or solid. Due to its low softening point and relatively small molecular weight, it is generally not used alone as a material. Since the structure of C9 petroleum resin does not contain polar groups, it has good water resistance, acid and alkali resistance, weather resistance and light aging resistance, good solubility in organic solvents, and good compatibility with other resins. It also has brittleness, tackiness, cohesi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F240/00C08F4/22
CPCC08F4/22C08F240/00
Inventor 李小潞孙大雷蔡晓兰方岩雄郑育英谭伟阚一群
Owner 抚顺科隆化工实业有限公司
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