Method for preparing heat-resistant resin by using ethylene tar as raw material

A technology of ethylene tar and heat-resistant resin, applied in the direction of adhesives, etc., can solve the problem of low actual utilization rate of ethylene tar, and achieve the effect of improving the quality content

Inactive Publication Date: 2017-04-19
CHANGCHUN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problem that the actual utilization rate of existing ethylene tar is low, the present invention adopts dialdehyde starch with lower price to replace the currently used cross-linking agent, and the cheap lignin sulfonic acid is used as a catalyst, and ethylene tar is used as raw material, successively through reducing Enrich the heavy fraction by pressure distillation, and then use aldehyde starch crosslinking agent and lignosulfonic acid as catalysts to obtain high-bonding heat-resistant resin through crosslinking

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Example 1 A method for preparing a heat-resistant resin using ethylene tar as a raw material, the steps and conditions are as follows: (1) Take ethylene tar and put it in a distillation bottle, raise the temperature to 140°C, and distill under reduced pressure at a vacuum of 90KPa to obtain Ethylene heavy tar, the mass yield is 79.8%;

[0011] (2) Add ethylene heavy tar and dialdehyde starch with a mass ratio of 5:1 into the reactor, and add lignosulfonic acid with 8% ethylene heavy tar mass, and raise the temperature to 160°C under the protection of nitrogen at 30mL / min. React for 5h to obtain heat-resistant resin. The mass yield of the resin is 96.4%, the softening point is 114°C, and the mass residual carbon rate is 41.5% at 500°C in air. Proven to have good heat resistance. The quality of its bonding performance is expressed by the content of toluene insoluble quinoline soluble matter-β resin, wherein the mass content of toluene insoluble matter is 21.6%, the mass...

Embodiment 2

[0012] Example 2 A method for preparing a heat-resistant resin using ethylene tar as a raw material, the steps and conditions are as follows: (1) Take ethylene tar and put it in a distillation bottle, raise the temperature to 160°C, and distill under reduced pressure at a vacuum of 90KPa to obtain Ethylene heavy tar; the mass yield is 80.0%.

[0013] (2) Add ethylene heavy tar and dialdehyde starch with a mass ratio of 5:1.5 into the reactor, and add lignosulfonic acid with 9% ethylene heavy tar mass, and raise the temperature to 150°C under the protection of nitrogen at 40mL / min. React for 4h to obtain heat-resistant resin. The mass yield of the resin is 96.7%, the softening point is 123°C, and the mass carbon residue rate is 42.1% at 500°C in air, which proves that it has good heat resistance. Its bonding performance is represented by the content of toluene-insoluble quinoline soluble matter-β resin. The mass content of toluene insoluble matter is 33.6%, the mass content o...

Embodiment 3

[0014] Example 3 A method for preparing a heat-resistant resin using ethylene tar as a raw material, the steps and conditions are as follows: Step (1) is the same as Example 1;

[0015] (2) Add ethylene heavy tar and dialdehyde starch with a mass ratio of 5:2 into the reactor, and add lignosulfonic acid with 10% ethylene heavy tar mass, and raise the temperature to 140°C under the protection of nitrogen at 50mL / min. React for 3h to obtain heat-resistant resin. The mass yield of the resin is 96.2%. The softening point is 118° C., and the carbon residue rate is 43.3 percent at 500° C. in air. Proven to have good heat resistance. Its bonding performance is expressed by the content of toluene insoluble quinoline soluble matter—β resin. The mass content of toluene insoluble matter is 24.7%, the mass content of quinoline insoluble matter is 6.5%, and the mass content of beta resin is 18.2%.

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Abstract

The present invention provides a method for preparing a heat-resistant resin by using ethylene tar as a raw material, wherein a reaction with ethylene tar is performed to prepare the heat-resistant resin by using low-price dialdehyde starch to replace other high-price cross-linking agents and by using low-price lignosulfonic acid as a catalyst, the heat-resistant resin has high adhesion, the highest yield of the obtained heat-resistant resin is 96.7%, and the softening point is 123 DEG C. Compared to the resin synthesized by using p-toluenesulfonic acid as the catalyst and using terephthalyl alcohol, divinylbenzene, s-trioxane and 1,4-phthalaldehyde as the cross-linking agents, the resin prepared through the method of the present invention has the following advantages that the mass carbon residue value and the beta resin mass content are substantially improved so as to provide the new approach for the industrial utilization of the ethylene tar. According to the present invention, the prepared ethylene tar resin can be used as the binder for molding of various graphite materials.

Description

technical field [0001] The invention belongs to the fields of utilization of petrochemical by-products and novel carbon materials, and relates to a method for preparing heat-resistant resins using ethylene tar as a raw material. Background technique [0002] After nearly ten years of rapid development, China's ethylene production capacity ranks second in the world. In 2005, the ethylene production capacity was 7.859 million tons per year, and in 2015 it exceeded 20 million tons per year. The main raw material for China's ethylene production is naphtha, accounting for about 65%. Compared with foreign companies that mainly use ethane as raw material, the production cost is high and the market competition is weak. At present, foreign ethylene tar is mainly used to produce carbon black and other products, and the economic benefits are considerable. Most of ethylene tar in China is mainly burned as fuel, which has low calorific value and pollutes the environment; a small part o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G61/02C09J165/00
CPCC08G61/02C08G2261/31C09J165/00
Inventor 张龙刘序宝
Owner CHANGCHUN UNIV OF TECH
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