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Preparation method of light-color glycerol ester of rosin

A rosin glyceride and light-colored technology, which is applied in the field of preparation of light-colored rosin glyceride, can solve the problems of increasing production and operation costs, increasing equipment investment, etc., and achieves the effects of short esterification time and improved hardness

Active Publication Date: 2015-06-10
桂林兴松林化有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Not only that, rosin also needs inert gas protection during esterification, which not only increases equipment investment, but also increases production and operation costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 1) The rosin is subjected to vacuum distillation under the conditions of a vacuum degree of 0 KPa and a temperature of 200° C. to obtain refined rosin.

[0016] 2) Put the refined rosin directly into the esterification reaction kettle, add a composite catalyst of 0.14% by weight of the refined rosin and glycerin of 10% by weight of the refined rosin, and react for 2.5 hours at 250° C. with a stirring speed of 50 r / min to obtain Reactant. The composite catalyst is composed of butyl stannoic acid, trinonylphenyl phosphite, neodymium oxide, lithium hydroxide and bis[-ethyl (3,5-di-tert-butyl-4-hydroxybenzyl) phosphoric acid] calcium salt, Its weight ratio is 1:1:1:1:1.

[0017] 3) The reactants are then decompressed to a vacuum of 0.2KPa and kept for 5 minutes to remove low boilers to obtain light-colored rosin glycerides. The color is Ghana color number 0.2, the acid value is 16mg / g, and the softening point is 90°C.

Embodiment 2

[0019] 1) The rosin is subjected to vacuum distillation at a vacuum degree of 1KPa and a temperature of 270° C. to obtain refined rosin.

[0020] 2) Put the refined rosin directly into the esterification reaction kettle, add a composite catalyst of 0.16% by weight of refined rosin and glycerin of 12% by weight of refined rosin, and react for 4 hours at 270° C. with a stirring speed of 50 r / min to obtain the reaction thing. The composite catalyst is composed of butyl stannoic acid, trinonylphenyl phosphite, neodymium oxide, lithium hydroxide and bis[-ethyl (3,5-di-tert-butyl-4-hydroxybenzyl) phosphoric acid] calcium salt, Its weight ratio is 5:3:4:3:2.

[0021] 3) The reactants are then decompressed to a vacuum of 2KPa and kept for 60 minutes to remove low boilers to obtain light-colored rosin glycerides. The color is Ghana color number 0.2, the acid value is 15.2mg / g, and the softening point is 88°C.

Embodiment 3

[0023] 1) The rosin is subjected to vacuum distillation under the conditions of a vacuum degree of 1KPa and a temperature of 250° C. to obtain refined rosin.

[0024] 2) Put the refined rosin directly into the esterification reaction kettle, add a composite catalyst of 0.15% by weight of refined rosin and glycerol of 10.8% by weight of refined rosin, and react for 3 hours at 260° C. with a stirring speed of 50 r / min to obtain the reaction thing. The composite catalyst is composed of butyl stannoic acid, trinonylphenyl phosphite, neodymium oxide, lithium hydroxide and bis[-ethyl (3,5-di-tert-butyl-4-hydroxybenzyl) phosphoric acid] calcium salt, Its weight ratio is 5:3:1:3:1.

[0025] 3) The reactants are then decompressed to a vacuum of 1KPa and kept for 30 minutes to remove low boilers to obtain light-colored rosin glycerides. The color is Ghana color number 0.1, the acid value is 15mg / g, and the softening point is 90°C.

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Abstract

The invention provides a preparation method of light-color glycerol ester of rosin. The method comprises the steps of 1) performing pressure-reduced rectifying for rosin to obtain refined rosin; 2) adding glycerinum and a composite catalyst to the refined rosin using as the raw material to obtain a reactant, wherein the composite catalyst is prepared from butylhydroxyoxo-stannane, trisnonvlphenyl phosphosphite, neodymium oxide, lithium hydroxide and bi[-ethyl(3,5-di-tert-4-acrinyl) phosphoric acid] calcium salt in weight ratio (1-5): (1-3): (1-4): (1-3): (1-2); 3) reducing the pressure of the reactant until the vacuum degree reaches 0.2 to 2KPa, maintaining for 5 to 60min, and removing to obtain low-boiling substances to obtain the light-color glycerol ester of rosin. The preparation method is free of inert gas protection during preparing the light-color glycerol ester of rosin, so that the esterification needs a short time, and the prepared glycerol ester of rosin is light in color.

Description

technical field [0001] The invention relates to a preparation method of modified rosin ester, in particular to a preparation method of light-colored rosin glyceride. Background technique [0002] Rosin is mainly composed of molecular formula C 19 h 29 The composition of various resin acids of COOH is a valuable natural forestry resource in our country. my country's annual output of rosin is about 400,000 tons, ranking first in the world. Because rosin is brittle, easy to crystallize, not resistant to aging, and has a high acid value, it is usually used after chemical modification. Esterification of rosin is one of the important means of rosin modification. After rosin is esterified, not only the acid value is reduced, the thermal stability is improved, but also the acid and alkali resistance of rosin is enhanced, which greatly broadens its application field. Various rosin esters account for more than 60% of rosin modified products, and are widely used in coatings, inks,...

Claims

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Application Information

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IPC IPC(8): C09F1/04
Inventor 董林鑫刘川刘桂芳范辂
Owner 桂林兴松林化有限责任公司
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