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Process for producing abietic acid

A technology of abietic acid and organic acid, applied in the separation/purification of carboxylic acid compounds, organic chemistry and other directions, can solve the problems of high industrialization cost of microwave technology, environmental pollution, lack of development value, etc., to avoid local peroxidation, reduce Production cost and effect of saving water resources

Inactive Publication Date: 2010-11-03
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The industrialization cost of microwave technology is high, and the post-treatment of acid catalyst causes environmental pollution, which has no development value

Method used

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  • Process for producing abietic acid
  • Process for producing abietic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A preparation method of abietic acid is as follows: add 10 parts by mass of rosin to an organic acid solvent with 2 to 6 carbons in 5 to 100 parts by mass, stir and mix evenly, and heat to 30 to 95°C to completely dissolve the rosin; The rosin solution is added to a fixed-bed reactor equipped with a solid acid-cation exchange resin catalyst, and the temperature of the fixed-bed reactor is maintained at 30-95°C. The rosin solution flows through the fixed-bed reactor from top to bottom to obtain an abietic acid isomerization liquid; The content of abietic acid in the abietic acid isomerization liquid is analyzed by gas chromatography, and the content of abietic acid is more than 70%. Put the abietic acid isomerization solution at room temperature for 3-8 hours, the abietic acid crystallization precipitates in the abietic acid isomerization solution, filter to obtain the crude abietic acid crystals, dissolve the crude abietic acid crystals in an organic solvent at 30-95°C ...

Embodiment 2

[0028] Put 10 parts of rosin into 10 parts of propionic acid solvent, slowly heat to 70°C, and dissolve it completely under stirring. The rosin that dissolves is added in the fixed bed reactor that 001 * 7 strongly acidic cation exchange resin (GB / T 13659-1992) catalyzer is housed, and this fixed bed reactor is heated before feeding, and keeps constant temperature 40 ℃. Rosin propionic acid solution flows through fixed-bed reactor from top to bottom, obtains abietic acid isomerization liquid; The content of abietic acid in this abietic acid isomerization liquid is analyzed by gas chromatography, and the content of abietic acid is 85.1%. Stand at room temperature for 4 hours, abietic acid crystallizes out in the abietic acid isomerization liquid, filter to obtain the crude abietic acid crystals, recover all the filtered propionic acid solvent for reuse, and dissolve the crude abietic acid crystals with solvent propanol at 50°C Recrystallization was repeated 3 times, and the cry...

Embodiment 3

[0030] Put 10 parts of rosin into 20 parts of butyric acid solvent, slowly heat to 50°C, and dissolve it completely under stirring.

[0031] The dissolved rosin is added to a fixed-bed reactor equipped with a three-layer mixed-bed special ion exchange resin (HG / T 2623-94) catalyst, which is heated before feeding and kept at a constant temperature of 50°C. Rosin butyric acid solution flows through the fixed bed reactor from top to bottom to obtain abietic acid isomerization liquid; the content of abietic acid in this abietic acid isomerization liquid is analyzed by gas chromatography, and the content of abietic acid is 86.0%. Stand at room temperature for 5 hours, abietic acid crystallizes out in the isomerization liquid of abietic acid, and filters to obtain the crude product of abietic acid crystals. The butyric acid solvent after filtration is all recovered and reused, and the crude product of abietic acid crystals is dissolved in acetone at 50° C. Crystallization was repeat...

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Abstract

The invention belongs to a method for separating and purifying every component of a colophony and discloses a method for preparing an abietic acid: step 1, adding ten mass fraction of colophony into 5 to 100 mass fraction of an organic acid solvent with 2 to 6 carbons, mixing uniformly and being heated to lead the colophony to be totally dissolved; step 2, adding the dissolved colophony liquid into a fixed bed reactor with a solid acid-cation exchange resin catalyst and the fixed bed reactor keeps a temperature between 30 DEG C and 90DEG C; the colophony liquid flows over the fixed bed reactor from top to bottom to acquire an abietic acid heterogeneous liquid; step 3, standing, crystallizing and filtering the abietic acid heterogeneous liquid under a room temperature to acquire a crude crystallizing product of the abietic acid; step 4, dissolving the crude crystallizing product of the abietic acid by an organic solvent and then recrystallizing, and then obtaining a pure abietic acid after drying the recrystallized abietic acid crystal by vacuum. The method uses solid acid-strong acid cation exchange resin catalyst as a reaction catalyst of hete over more than 85 percent.

Description

1. Technical field [0001] The invention belongs to a method for separating and purifying components from rosin, in particular to the separation and purification of abietic acid. 2. Background technology [0002] Abietic acid is one of the 13 chemical isomer components of abietic acid in rosin, which is a renewable resource, accounting for about 40% of rosin. Under the action of acid catalysis, the content of abietic acid increases from about 40% to more than 70% through isomerization and rearrangement after the abietic acid generates carbocations under the action of acid catalysis. Abietic acid is a tricyclic diterpenoid compound, which has various biological activities such as antibacterial, antiviral, antitumor, and antiulcer. It has great application prospects in the fields of cosmetics, agriculture and medicine. Richard F C uses the sodium salt crystallization method in US2296503.1942-09-02, Harris uses the organic amine salt crystallization method in J.Am.Chem.Soc., 1...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C57/26C07C51/42C07C51/47
Inventor 刘红军周永红
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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