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Preparation method of triethylene glycol hydrogenated rosinate

A technology of rosin triethylene glycol ester and hydrogenated rosin, which is applied in the chemical field, can solve the problems of dark color, difficult to meet the use requirements of light-colored hydrogenated rosin triethylene glycol ester, long reaction time, etc., and achieve low acid value and light color of the product , Improve the effect of product color

Inactive Publication Date: 2013-03-27
广西梧州日成林产化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the hydrogenated rosin triethylene glycol ester produced by the traditional process has the problems of long preparation reaction time and dark color, which is about 9-10 (iron-cobalt color number), which is difficult to meet the requirements of light-colored hydrogenated rosin triethylene glycol in downstream applications. Ester usage requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Put 1000g of refined hydrogenated rosin into a four-neck flask with a stirring paddle, pass through nitrogen to replace and heat to melt, raise the temperature to 170-180°C, start stirring after the material is completely melted, add 300g of triethylene glycol and 4,4'- Thiobis(6-tert-butyl-3-methylphenol) 1.5g, nano-nanometer zinc oxide 1.0g, heat up to 272-278°C at a rate of 10°C per hour, and keep the reaction at 272-278°C for 6 hours After vacuuming, after evacuating for 5 hours, the temperature was lowered and the material was discharged to obtain hydrogenated rosin triethylene glycol ester.

[0022] The appearance of the hydrogenated rosin triethylene glycol ester product is a transparent liquid, the acid value is 9.3mg / g, the color (iron-cobalt color number) is 6+, and the viscosity at 100°C is 99.8mpa.s.

Embodiment 2

[0024] Put 850g of refined hydrogenated rosin and 150g of refined rosin into a four-necked flask with a stirring paddle, pass through nitrogen to replace and heat to melt, raise the temperature to 170-180°C, start stirring after the materials are completely melted, add 300g of triethylene glycol, alkane Base phenol disulfide oligomer 1.5g and nano-zinc oxide 1.0g, heat up to 272-278°C at a rate of 10°C per hour, and keep warm at 272-278°C for 6 hours, then vacuumize, and after vacuumize for 3 hours , cooling and discharging to obtain hydrogenated rosin triethylene glycol ester.

[0025] The appearance of the hydrogenated rosin triethylene glycol ester product is transparent liquid, the acid value is 5.8mg / g, the color (iron-cobalt color number) is 6-, and the viscosity at 100°C is 84.3mpa.s.

Embodiment 3

[0027] Put 850g of refined hydrogenated rosin and 150g of refined rosin into a four-neck flask with a stirring paddle, pass through nitrogen to replace and heat to melt, raise the temperature to 170-180°C, start stirring after the materials are completely melted, add 300g of triethylene glycol, 4 , 1.5g of 4'-thiobis(6-tert-butyl-3-methylphenol) and 0.5g of nano-zinc oxide, heat up to 272-278°C at a rate of 10°C per hour, and keep at 272-278°C After reacting for 5 hours, vacuumize, and after vacuumize for 3 hours, cool down and discharge to obtain hydrogenated rosin triethylene glycol ester.

[0028] The appearance of the hydrogenated rosin triethylene glycol ester product is a transparent liquid, the acid value is 6.9g / g, the color (iron-cobalt color number) is 6+, and the viscosity at 100°C is 89.4mpa.s.

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Abstract

The invention discloses a preparation method of triethylene glycol hydrogenated rosinate, relating to the technical field of chemical industry. The preparation method comprises the following steps of: (A) under protection of inert gas, performing melt refining on a hydrogenated rosin raw material; (B) after complete melting, adding an antioxidant, alcohol and a catalyst, and heating to 272-278 DEG C; (C) preserving heat at 272-278 DEG C and reacting for 5-10 hours so that the acid value index of the material reaches a set value; and (D) vacuumizing for 3-5 hours, cooling and discharging to obtain the triethylene glycol hydrogenated rosinate. According to the preparation method disclosed by the invention, the product color is improved by adding an anti-oxidation aid with good performance; and by adding nano zinc oxide as a catalyst, an obvious catalysis effect is realized, and the reaction time can be reduced by about 1 / 2.

Description

technical field [0001] The invention relates to the technical field of chemistry, in particular to a method for preparing hydrogenated rosin triethylene glycol ester. Background technique [0002] As a renewable resource, rosin has been widely used in adhesives, inks, coatings, synthetic rubber, papermaking, electronics, pesticides, food and cosmetics industries directly or after modification and deep processing, and is indispensable to the national economy. Chemical raw materials. The modification of rosin generally utilizes reactive groups such as conjugated double bonds and carboxyl groups in the molecular structure of rosin, through reactions such as addition, disproportionation, hydrogenation, polymerization, aminolysis, salt formation, esterification, etc. Disproportionated rosin, hydrogenated rosin, polymerized rosin, rosin amine, rosin salt and various rosin esters and other deep-processed products. [0003] Liquid rosin resin has been more and more widely used in ...

Claims

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Application Information

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IPC IPC(8): C09F1/04
Inventor 李前林克忠侯文彪江文夺吴嘉超
Owner 广西梧州日成林产化工股份有限公司
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