Preparation of light colore high softening point maleated rosin pentaerythritol

A technology of rosin pentaerythritol ester and high softening point, which is applied in the chemical modification of natural resins, etc., can solve problems such as difficult color reduction, and achieve the effect of improving hardness

Inactive Publication Date: 2009-07-08
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the currently reported lightening mechanism is to achieve the effect of improving the color of the product through the action of additives on the conjugated double bonds in the resin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0019] Example 1

[0020] A preparation method of light-colored high-softening point maleic rosin pentaerythritol ester, comprising the following steps:

[0021] In the first step, the rosin is refined under the conditions of a vacuum degree of 0-1kPa and a temperature of 200-270℃ to obtain a refined rosin with a softening point of 80-86℃;

[0022] In the second step, under the protection of inert gas, add maleic anhydride with 5-14% of the refined rosin mass and a reducing agent with 0.03-1.0% of the refined rosin mass to the molten refined rosin, and put it at a temperature of 150-230℃ The lower reaction is 0.5-2h; among them, the reducing agent is phosphite or phosphite ester: such as sodium phosphite, triphenyl phosphite, monophenyl diisooctyl phosphite, 3,5-di-tertiary group -4-Hydroxybenzyl diethyl phosphonate one or a mixture of several in any proportion; the proportion of maleic rosin in the quality of refined rosin can be 5%, 8%, 9%, 10%, 11% , 12%, the proportion of redu...

Example Embodiment

[0027] Example 2

[0028] Refining 98g rosin to make 87g refined rosin, pass N 2, Heat to melt, add 0.183g of triphenyl phosphite, 4.4g of maleic anhydride, increase the temperature to 180℃, keep it for 1h, continue to increase the temperature, add bis(3,5-di-tert-butyl-4-hydroxybenzyl) Monoethyl phosphonate) calcium 0.17g, 2,2'-thiobis(4-methyl-6-tert-butylphenol) 0.17g, pentaerythritol 11.4g, pentaerythritol is uniformly added to the reaction system within 0.5 hours . The temperature was raised to 270°C, and after 1 h, tetra[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid]pentaerythritol ester 0.15 and alkylphenol disulfide oligomer 0.15g were added. Timed sampling. When the acid value drops to 20mg / g, vacuumize under reduced pressure.

[0029] After 2.5 hours of esterification in this example, the acid value of the product dropped to 16 mg / g, the color was Ghana color No. 2, and the softening point was 124°C.

Example Embodiment

[0030] Example 3

[0031] Refining 114g of rosin to obtain 102g of refined rosin, pass N 2 , Heat to melt, add 0.05g of triphenyl phosphite, 7.2g of maleic anhydride, increase the temperature to 180℃, keep it for 1h, continue to increase the temperature, add tetra[β-(3,5-di-tert-butyl-4) -Hydroxyphenyl) propionic acid] pentaerythritol ester 0.11g, 4,4'-thiobis(6-tert-butyl-3-methylphenol) 0.15g, pentaerythritol 14.1g, pentaerythritol is uniformly added to the reaction within 0.5 hours System. Raise the temperature to 270℃, add 0.13g of bis(3,5-di-tert-butyl-4-hydroxybenzylphosphonate monoethyl) calcium, 2,2'-thiobis(4-methyl-6- Tert-butylphenol) 0.11g. Timed sampling. When the acid value drops to 20mg / g, vacuumize under reduced pressure.

[0032] After 2.5 hours of esterification in this example, the acid value of the product dropped to 15.6 mg / g, the color was Garner No. 2+, and the softening point was 135°C.

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Abstract

The invention relates to a method for preparing maleic rosin pentaerythritol ester with shallow color and high softening point. The method comprises the following steps that: under the conditions of vacuum degree of between 0 and 1 kPa and temperature of between 200 and 270 DEG C, rosin is refined to form refined rosin having a softening point of between 80 and 86 DEG C; under the protection of inert gas, the molten refined rosin is added with maleic acid anhydride accounting for 5 to 14 percent of the mass of the refined rosin and a reducing agent accounting for 0.03 to 1.0 percent of the mass of the refined rosin, and reacts for 0.5 to 2 hours at a temperature of between 150 and 230 DEG C; pentaerythritol accounting for 10 to 20 percent of the mass of the refined rosin, a catalyst accounting for 0.1 to 1.0 percent of the mass of the refined rosin and a discoloring agent accounting for 0.1 to 1.0 percent of the mass of the refined rosin are added to a reaction system and react at temperature of between 230 and 290 DEG C; reaction is finished till acid value is less than 20 mg/g; the reactants are decompressed, vacuumized and kept at vacuum degree of between 0 and 2 kPa for 5 to 60 minutes; and a low-boiling-point substance is removed and the maleic rosin pentaerythritol ester with shallow color and high softening point is perpared.

Description

1. Technical field [0001] The invention relates to a preparation method of a light-colored high-softening point modified rosin resin, in particular to a preparation method of a light-colored high-softening point maleic rosin pentaerythritol ester. 2. Background technology [0002] Rosin is an important natural renewable resource in our country. Due to its unique structure and performance, it has attracted widespread attention. Its deep-processed products can be widely used in various departments of daily life and occupy an important position in national economic life. It is a kind of Indispensable chemical raw materials. As one of the important modified rosin products, maleic rosin is the addition product of rosin and maleic anhydride. If maleate rosin is esterified with polyols such as glycerin and pentaerythritol, a product with a higher softening point can be produced. Because of its excellent comprehensive performance, it can be widely used in paints, coatings, inks and...

Claims

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Application Information

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IPC IPC(8): C09F1/04
Inventor 商士斌李建芳高宏宋湛谦饶小平
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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