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Method for preparing rosin glyceride by microwave irradiation

A rosin glyceride and microwave technology is applied in the field of deep processing fine chemical catalyst technology, which can solve the problems of long reaction time, dark product color, equipment corrosion, etc., and achieves the advantages of shortening reaction time, solving equipment corrosion and improving product color Effect

Inactive Publication Date: 2009-02-25
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention can solve the problems of equipment corrosion, long reaction time, dark product color and high energy consumption

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In the microwave reactor, according to rosin: glycerol = 1.5-2:1 (mol), catalyst dosage 0.1-0.4% (based on rosin quality), microwave power: 500-1000W, reaction temperature: 250-280°C, reaction Time: 0.5-1h. The esterification reaction between rosin and glycerin was catalyzed by ZnO. After analysis, the relevant quality indicators of the esterification product are as follows:

[0029] Acid value: 8.8mgKOH / g, chroma (iron-cobalt method): 8, softening point: 87.9°C,

[0030] Solubility (1:1 with benzene), specific gravity (25°C / 25°C) 1.088, ash content: 0.05%.

Embodiment 2

[0032] In the microwave reactor, according to rosin: glycerol = 1.5-2:1 (mol), catalyst dosage 0.1-0.4% (based on rosin quality), microwave power: 500-1000W, reaction temperature: 250-280°C, reaction Time: 0.5-1h. The esterification reaction between rosin and glycerin was catalyzed by ZnO. After analysis, the relevant quality indicators of the esterification product are as follows:

[0033] Acid value: 8.2mgKOH / g, chromaticity (iron-cobalt method): 7, softening point: 87.2°C,

[0034] Solubility (1:1 with benzene), specific gravity (25°C / 25°C) 1.085, ash content: 0.03%.

Embodiment 3

[0036] In the microwave reactor, according to rosin: glycerol = 1.5-2:1 (mol), catalyst dosage 0.1-0.4% (based on rosin quality), microwave power: 500-1000W, reaction temperature: 250-280°C, reaction Time: 0.5-1h. The esterification reaction between rosin and glycerin was catalyzed by ZnO. After analysis, the relevant quality indicators of the esterification product are as follows:

[0037] Acid value: 8.6mgKOH / g, chroma (iron-cobalt method): 7, softening point: 87.5°C,

[0038] Solubility (1:1 with benzene), specific gravity (25°C / 25°C) 1.086, ash content: 0.04%.

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Abstract

The invention relates to a deep processing preparation technology of a fine chemical catalyst, in particular to a method using microwave irradiation to prepare rosin glyceride, especially using a microwave solid phase method to prepare solid acid ZnO catalyst and catalyzing rosin esterification in a WF-4000C microwave reaction system to prepare the rosin glyceride. The preparing technical conditions of ZnO are that zinc acetate and oxalic acid are porphyrized and mixed to be added in a beaker and then put in a microwave reactor. At the radiation of 300-800W, the mixed materials react for 3-8min and are immersed by ethanol and washed. After two times of air pump filtration, drying at 100 to 180 DEG C is implemented for 1-3h. Roasting at 400 to 600 DEG C in a muffle furnace is implemented for 2-4h. The technical conditions of esterification reaction of rosin and glycerol comprise: the ratio of rosin to glycerol is 1.5-2 to 1 (mol); the catalyst amount of ZnO is 0.1-0.4 percent (basing on the mass of rosin); the microwave power is 500-1000W; the reaction temperature is 250-280 DEG C; the reaction time is 0.5-1h. The acid value of esterified products is 6-9KOHmg / g, the chroma (iron cobalt method) is 6.7-8.8, the softening point is 86-89 DEG C, the solubility (1 to 1 compared with benzene) is low, the specific gravity (25 DEG C / 25 DEG C) is 1.082-1.088) and the ash content is 0.03-0.05 percent.

Description

technical field [0001] The invention relates to a catalyst technology for deep processing to prepare fine chemicals, in particular to a microwave-promoted method for preparing rosin glycerides. Background technique [0002] Microwave is an electromagnetic wave with a frequency of 300MHz-300GHz, its wavelength is between 100cm-1mm, and its energy is about several Jmol -1 . Microwaves are a form of energy that can be converted into energy in a medium. At present, microwave energy is used in synthetic chemistry, material science, rubber industry, paper industry, leather, plastic and other industries. [0003] Catalysts used to catalyze the esterification of rosin include protonic acids, inorganic salts, organic reagents and solid acid catalysts. The protonic acid catalyst corrodes the reaction equipment seriously, and it is difficult to separate from the product, and the rosin esterification product has a darker color; the inorganic salt and the product are also difficult to...

Claims

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Application Information

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IPC IPC(8): C09F1/04
Inventor 王亚明曹振恒蒋丽红郭会仙贾庆明陕绍云张思华
Owner KUNMING UNIV OF SCI & TECH
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