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Preparation method of hydrogenated rosin without crystallization tendency

A hydrogenated rosin, non-crystallization technology, which is applied in the fields of natural resin refining and natural resin chemical modification, etc., can solve the problems of large loss of precious metal catalysts, affecting product application safety, high equipment requirements, etc., and achieves reduction of precious metal catalyst residues, good economical Benefits and effects in a wide range of applications

Active Publication Date: 2014-03-12
广东科茂林产化工股份有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The water-white hydrogenated rosin currently on the market adopts the traditional precious metal palladium-carbon catalytic hydrogenation production process to produce hydrogenated rosin, and then undergoes high-vacuum distillation at absolute pressure (0.400-4.00) kPa in the later stage, and collects fractions with a distillation temperature of 195-250°C , after condensation, water-white hydrogenated rosin with low precious metal content can be obtained, but this method cannot separate the hydrogenated rosin part that has crystallization tendency in hydrogenated rosin
[0011] The production of hydrogenated rosin by the above method mainly has the following disadvantages: one is that the production pressure is high and the requirements for equipment are high; the other is that the loss of precious metal catalyst is large, the economic cost is high, and the product contains lost precious metals, which affects the later stage of the product The application is safe; the third is that the prepared hydrogenated rosin has a crystallization tendency, which limits the application of the product in some special adhesives, especially in the application of advanced electronic fluxes.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A kind of embodiment of the preparation method of hydrogenated rosin without crystallization tendency of the present invention, the method described in this embodiment comprises the following steps:

[0033] (1) Add 400 grams of super-grade rosin (acid value 169mgKOH / g, softening point 77°C, Ghana color 5+) into a high-pressure reactor with a volume of 2L, and add n-hexane to adjust the rosin content to 30%-50%. Add powdery 5% palladium carbon catalyst (water content 50%) according to 0.3-1% of the weight of rosin, vacuumize, replace the air in the kettle with nitrogen for 2-3 times, and then fill the nitrogen in the hydrogen replacement kettle for 2-3 times, and then Heat to 90-120°C to dissolve, adjust the hydrogen pressure in the kettle, start the heating and stirring system of the autoclave, continuously replenish hydrogen, keep the hydrogen pressure at 50-100 kg pressure / square centimeter, and raise the temperature to 180-240°C until the hydrogen pressure Stop the ...

Embodiment 2

[0038] A kind of embodiment of the preparation method of hydrogenated rosin without crystallization tendency of the present invention, the method described in this embodiment comprises the following steps:

[0039] (1) Add 400 grams of super-grade rosin (acid value 169mgKOH / g, softening point 77°C, Ghana color 5+ dissolved in toluene to form a 50% solution) into a 2L high-pressure reactor, add pinane, and adjust When the rosin content is 30%-70%, add powdery 5% palladium carbon catalyst (50% water content) according to 0.3-1% of the rosin weight, vacuumize, replace the air in the kettle with nitrogen gas twice, and then fill the hydrogen replacement kettle Medium nitrogen 2-3 times, then heated to 100-160°C to dissolve, adjust the hydrogen pressure in the autoclave, start the heating and stirring system of the autoclave, continuously replenish hydrogen, keep the hydrogen pressure at 80-160 kg pressure / square centimeter, and raise the temperature to 180-260°C, until the hydroge...

Embodiment 3

[0044] A kind of embodiment of the preparation method of hydrogenated rosin without crystallization tendency of the present invention, the method described in this embodiment comprises the following steps:

[0045] (1) Add 300 grams of super-grade rosin (acid value 169 (mgKOH / g), softening point 77 ° C, Ghana color 4-) into a high-pressure reactor with a volume of 2 L, add n-octane, and adjust the rosin content to 20% -50%, according to 5%-10% of the weight of rosin powdered Raney nickel, vacuumize, replace the air in the kettle with nitrogen for 2 times, then fill in hydrogen to replace the nitrogen in the kettle for 2-3 times, and then heat to 90- Dissolve at 120°C, adjust the hydrogen pressure in the autoclave, start the heating and stirring system of the autoclave, continuously replenish hydrogen, keep the hydrogen pressure at 100-150 kg pressure / square centimeter, and raise the temperature to 160-240°C until the hydrogen pressure no longer drops. Reaction, the reaction ti...

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Abstract

The invention discloses a preparation method of hydrogenated rosin without crystallization tendency. The method comprises the following steps: (1) dissolving a C5-C8 saturated alkane for existing hydrogenated rosin, wherein the weight ratio of the C5-C8 saturated alkane to the existing hydrogenated rosin is more than 1, agitating to sufficiently dissolve, stopping agitating when the dissolving balance is achieved; (2) keeping the solution of the step (1) at 0-25 DEG C, standing for 4-8 hours to sufficiently crystallize and separate out the hydrogenated rosin with crystallization tendency, filtering the crystallized hydrogenated rosin, separating filtrate by distillation to separate a solvent to obtain the hydrogenated rosin without crystallization tendency. The method is simple in process and the hydrogenated rosin which is free from crystallization tendency, low in ash content and high in stability can be obtained through the method. And meanwhile, the invention further discloses the hydrogenated rosin without crystallization tendency prepared by using the method, the hydrogenated rosin without crystallization tendency is oxidation resistant and ageing resistant, and can be widely applied to the fields of adhesive, electronic soldering flux, coating, printing ink, rubber and the like.

Description

technical field [0001] The invention relates to a method for preparing hydrogenated rosin, in particular to a method for preparing hydrogenated rosin with no crystallization tendency, low ash content and high stability. Background technique [0002] Rosin is a renewable natural resource. my country is rich in pine resources. The rosin produced by it is the most important product of my country's forestry chemical industry, and it is also a pillar industry. Because of its special molecular structure and properties, rosin is widely used in coatings, inks, adhesives, electronics and other industries. With the rapid development of technology in various industries, the quality requirements for rosin and its deep-processed products are also continuously increasing. Anti-crystallization, Aging resistance has become one of the important quality indicators of rosin and its deep-processed products. It has good compatibility, no crystals, and excellent aging resistance, which has become...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09F1/02C09F1/04C22B11/00C22B23/00
Inventor 沈亮升徐社阳范德明曾广建
Owner 广东科茂林产化工股份有限公司
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