A kind of method for preparing rosin-lac ester by solid phase reaction

A technology for solid-phase reaction and esterification, which is applied in the field of mechanical grinding solid-phase reaction to prepare rosin-shellac esterification, can solve the problems of solvent pollution, high temperature and high energy consumption, etc., to avoid self-polymerization, solve high temperature, high energy consumption, and low energy consumption effect

Active Publication Date: 2020-11-27
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

It solves the shortcomings of the traditional rosin esterification process, such as high temperature, high energy consumption, and solvent pollution of the environment, and at the same time avoids the problem of self-polymerization of shellac at high temperature

Method used

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  • A kind of method for preparing rosin-lac ester by solid phase reaction
  • A kind of method for preparing rosin-lac ester by solid phase reaction

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Experimental program
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preparation example Construction

[0026] The preparation method comprises the steps of:

[0027] a. Mechanical grinding: Weigh shellac equivalent to 10-25% of the molar mass of rosin adduct and mix it with rosin adduct, add catalyst equivalent to 0.1% of rosin adduct mass, mix evenly, put into grinding tank, Add zirconia grinding balls of the same quality as the material; put the grinding tank into the ball mill, grind for 80-160 minutes at room temperature, and the ball mill speed is 250 rpm; separate the product from the grinding balls; the catalyst can be ZnO, Catalysts such as MgO, CaO, and solid superacids.

[0028] The dosage of the shellac is 10-25% of the molar mass of the rosin adduct.

[0029] The speed of the ball mill is 250 rpm, and the grinding time is 80-160 minutes.

[0030] b. Annealing reaction: place the ground material in a constant temperature blast drying oven, react at 60-100°C for 6-12h, and cool to room temperature with the furnace after the reaction;

[0031] The annealing reaction...

Embodiment 1

[0039] A method for preparing rosin-lac esters by solid phase reaction, comprising the steps of:

[0040] The first step, the preparation of rosin adduct: Weigh 100g of rosin, raise the temperature to 170°C, stir, slowly add 30g of maleic anhydride, and react at 195°C for 3h to obtain maleated rosin.

[0041] The second step, mechanical grinding: Weigh 40g (b) of maleic rosin, 25g (a) of shellac, and 0.04g of ZnO, mix them evenly, put them into a grinding jar, add grinding balls of the same quality as the materials; put the grinding jar into Ball mill, grind at normal temperature for 160 minutes, the ball mill rotating speed is 250 rev / min; product and grinding ball are separated, sampling (c).

[0042] The third step, annealing reaction: put the ground material in a constant temperature blast drying oven, react at 80°C for 12h, and cool to room temperature with the furnace after the reaction, and take a sample (d).

[0043] In the fourth step, wash with absolute ethanol 10 t...

Embodiment 2

[0045] A method for preparing rosin-lac esters by solid phase reaction, comprising the steps of:

[0046] The first step, the preparation of rosin adduct: Weigh 100g of rosin, raise the temperature to 170°C, stir, slowly add 30g of maleic anhydride, and react at 195°C for 3h to obtain maleated rosin.

[0047] The second step, mechanical grinding: weigh 40g of maleic rosin, 25g of shellac, and 0.04g of ZnO, mix them evenly, put them into a grinding tank, add grinding balls of the same quality as the materials; put the grinding tank into a ball mill, and grind at room temperature 160 minutes, the speed of the ball mill is 250 rpm; separate the product from the grinding balls. The third step, annealing reaction: put the ground material in a constant temperature blast drying oven, react at 80°C for 24h, and cool to room temperature with the furnace after the reaction.

[0048] In the fourth step, wash with absolute ethanol 10 times that of the product at room temperature, vacuum ...

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Abstract

The invention discloses a rosin-lac ester compound and a preparation method thereof. The method comprises the following steps of 1, rosin adduct preparation: rosin and unsaturated acid anhydride or unsaturated acid D-A perform an addition reaction to obtain a rosin adduct; 2, mechanical grinding: lac and the rosin adduct are mixed; a catalyst is added; the materials are uniformly mixed; grinding balls are charged; a grinding tank is charged into a grinding machine; grinding is performed for 80 to 160 minutes at normal temperature; a product and the grinding balls are separated; 3, annealing reaction: the ground materials are put into a constant-temperature blowing drying box; reaction is performed for 6 to 12h at 60 to 100 DEG C; after the reaction is finished, the materials are cooled to room temperature along with a furnace; 4, normal temperature washing by absolute ethyl alcohol, performing vacuum filtration and drying a solid part at 60 DEG C.

Description

technical field [0001] The invention relates to a method for preparing rosin-lac esters by mechanical grinding and solid-phase reaction. Background technique [0002] In recent years, people have paid great attention to green chemistry and environment-friendly engineering. Chemists strive to eliminate pollution from the source and devote themselves to the research of green organic synthesis. Solid-phase organic synthesis is an important part of green synthesis. It does not use solvents, and has significant advantages over solution in terms of reaction speed, yield, and selectivity. Solid-phase grinding reaction is an important aspect of solid-phase organic synthesis. It is an ideal synthetic method because of its mild conditions, simple operation, and environmental friendliness. [0003] Rosin is a mixture containing a variety of resin acids, which, like other monocarboxylic acids, can react with a variety of alcohols to form corresponding esters. However, since the carbox...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09F1/04
CPCC09F1/04
Inventor 高宏檀贯妮许嘉琍商士斌
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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