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Rhodizonic acid raffinate reusing synthesis process

A synthesis process, the technology of palmitic acid, which is applied in the field of multiplexing synthesis process of palmitic acid residue, can solve the problems of reducing the production cost of palmitic acid, poor atom economy, etc., and achieve the reduction of production cost and environmental cost, and low raw material cost , the effect of mild reaction conditions

Inactive Publication Date: 2014-06-11
TAISHAN MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the traditional synthesis route of palmitic acid is obtained from glyoxal through trimerization and decarboxylation, and the total yield is less than 10%. Widely used, but about 90% of the glyoxal in this process is not fully utilized in one reaction, the atom economy is very poor, and a large amount of waste liquid is produced, which contains a large amount of inorganic salts and organic matter that can be reused. Can be recycled, can greatly reduce the production cost of palmitic acid

Method used

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  • Rhodizonic acid raffinate reusing synthesis process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: The reusing synthetic process of palmitic acid residue, characterized in that it comprises the following steps:

[0019] (1) Weigh anhydrous sodium sulfite 55: dissolve it in water, stir until it is completely dissolved to obtain a mixed solution;

[0020] (2) Weigh out sodium bicarbonate 30 dissolved in water and mix with the above mixture, and control the temperature at 40

[0021] ℃, after the liquid is evenly stirred, add 100 mL of glyoxal (low mass concentration is 30%);

[0022] (3) Control the temperature at 48°C and blow in the air for 0.5 hours, then heat to 100°C to obtain a brown-black mixture, which is cooled and filtered under pressure to obtain a filtrate;

[0023] (4) Use the above-mentioned filtrate as the reaction liquid, and glyoxal (low mass concentration is 30%), and the ratio of the reaction liquid to glyoxal is 4:1.

Embodiment 2

[0025] The technical scheme of the present invention is: a reusable synthesis process of palmitic acid residue, which is characterized in that it comprises the following steps:

[0026] (1) Weigh 62g of anhydrous sodium sulfite and dissolve in water, stir until completely dissolved, to obtain a mixed solution;

[0027] (2) Weigh 40g of sodium bicarbonate, dissolve in water and mix with the above mixture, and control the temperature at 46

[0028] ℃, after the liquid is evenly stirred, add 100 mL of glyoxal (low mass concentration is 30%);

[0029] (3) Control the temperature at 52°C and blow in air for 1.5 hours, and then heat to 100°C to obtain a brown-black mixture, which is cooled and filtered under pressure to obtain a filtrate;

[0030] (4) Use the above-mentioned filtrate as the reaction liquid, and glyoxal (low mass concentration is 30%), and the ratio of the reaction liquid to glyoxal is 6:1.

Embodiment 3

[0032] The technical scheme of the present invention is: a reusable synthesis process of palmitic acid residue, which is characterized in that it comprises the following steps:

[0033] (1) Weigh 58g of anhydrous sodium sulfite and dissolve in water, stir until completely dissolved, to obtain a mixed solution;

[0034] (2) Weigh 34g of sodium bicarbonate, dissolve in water and mix with the above mixture, and control the temperature at 42

[0035] ℃, after the liquid is evenly stirred, add 100 mL of glyoxal (low mass concentration is 30%);

[0036] (3) The temperature is controlled at 50°C and air is blown in for 0.8 hours, and then heated to 100°C to obtain a brown-black mixture, which is cooled and filtered under pressure to obtain a filtrate;

[0037] (4) Use the above-mentioned filtrate as the reaction liquid, and glyoxal (low mass concentration is 30%), and the ratio of the reaction liquid to glyoxal is 5:1.

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Abstract

The invention relates to a rhodizonic acid raffinate reusing synthesis process, which comprises the following steps of weighing 55-62g of anhydrous sodium sulphite to be dissolved in water, blending until the anhydrous sodium sulphite is completely dissolved to obtain mixed liquor, weighing 30-40g of sodium bicarbonate to be soluble in water and be mixed with the mixed liquor, enabling the temperature to be controlled at 40-46 DEG C, evenly blending liquor, enabling 100mL of glyoxal (with the mass concentration of 30%) to be added in the liquor, enabling the temperature to be controlled at 48-52 DEG C, enabling air to be led in for 0.5-1.5 hours, heating until the temperature reaches 100 DEG C, reacting to obtain brownish black mixture, cooling and filter-pressing the mixture to obtain filter liquor, enabling the filter liquor to be served as stand-by reaction liquor, and enabling the glyoxal (with the mass concentration of 30%) to be added during reaction. The rhodizonic acid raffinate reusing synthesis process is mild in reaction condition and low in material cost, reduces liquid waste discharge, lowers production cost and environment cost, and provides a new approach to mass preparation of rhodizonic acid and deriving coloring matters of the rhodizonic acid.

Description

Technical field [0001] The invention relates to a process for multiplexing and synthesizing a residue of palmitic acid. Background technique [0002] Rhodizonate is the basic raw material for the synthesis of croconic acid. Croconic dyes have good photo-thermal stability and show excellent application performance in the fields of near-infrared optical recording and laser display. At present, the traditional synthetic route of phyllanic acid starts from glyoxal and is prepared by trimerization and decarboxylation. The total yield is less than 10%. This synthetic process is a chemical synthesis carried out in water as a medium, and the cost is relatively low. Widely used, but in this process, about 90% of glyoxal is not fully utilized in one reaction. The atom economy is very poor, and a large amount of waste liquid is generated, which contains a large amount of inorganic salts and organic matter that can be reused. It can be recycled and can greatly reduce the production cost of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/713C07C45/72
Inventor 陈红余李平张熙曼汪海
Owner TAISHAN MEDICAL UNIV