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Process for synthesizing stable sodium azulene sulfonate

A technology for the synthesis of sodium azulene sulfonate, which is applied in the field of stable sodium azulene sulfonate synthesis technology, can solve the problems of waste acid and organic solvent generation, high toxicity of dioxane, environmental pollution, etc., and achieve pollution reduction, The effect of solving the problem of toxic work

Active Publication Date: 2006-07-19
天津顶硕药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] But above-mentioned synthetic method has following deficiency: (1) waste acid and organic solvent are produced, pollute environment; (2) dioxane toxicity is bigger; (3) product stability is poor; (4) energy consumption is high

Method used

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  • Process for synthesizing stable sodium azulene sulfonate
  • Process for synthesizing stable sodium azulene sulfonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 300 ml of dichloroethane and 85 g of SB102 reagent into a 500 ml three-necked flask, feed in liquefied sulfur trioxide, control the temperature at 0°C, stop feeding after the weight increases to 80 g, and continue stirring for 20 minutes for later use .

[0028] Add the reagent obtained above dropwise to a solution container containing 100 grams of lanoleic hydrocarbon and 250 milliliters of dichloroethane at 0°C under stirring. After the addition, raise the temperature to 20°C and continue stirring for 30 minutes. In a container with 1000 grams of crushed ice, let it stand until the crushed ice melts, separate the organic layer and reuse it after fractional distillation. The aqueous layer was adjusted to PH=8 with sodium carbonate, washed with water and dried at 40°C for 3 hours, dissolved in water and added with 0.6 g of a stabilizer, recrystallized to obtain 120 g of flaky crystals, yield 75%, The water after washing and crystallization was extracted with 300 ml...

Embodiment 2

[0030] Add 200 ml of dichloroethane and 60 g of SB102 reagent into a 500 ml three-necked flask, feed in liquefied sulfur trioxide, control the temperature below 0°C, stop feeding when the weight increases to 55 g, and continue stirring for 20 minutes first stand-by.

[0031] The reagent obtained above was added dropwise to a solution of 67 g of lanoleic hydrocarbon and 170 ml of dichloroethane at 0° C. with stirring, and stirred at 20° C. for 30 minutes after the addition was completed. Transfer to the container that 700 grams of crushed ice is housed, stand until the crushed ice melts, separate the organic layer and reuse it after fractional distillation. The water layer was adjusted to PH=8 with sodium carbonate, washed with water, and dried at 80°C for 3 hours. The obtained product was dissolved in water and 0.4 g of stabilizer was added to recrystallize to obtain 78 g of flaky crystals, with a yield of 73%. Washed with water And crystallized water, use 200 milliliters of ...

Embodiment 3

[0033] Add 250 ml of dichloroethane and 75 g of SB102 reagent into a 500 ml three-necked flask, feed in liquefied sulfur trioxide, control the temperature below 0°C, stop feeding when the weight increases to 70 g, and continue stirring for 20 minutes first stand-by.

[0034] The reagent obtained above was added dropwise to a solution of 85 g of lanoleic hydrocarbon and 210 ml of dichloroethane at 0° C. with stirring, and stirred at 20° C. for 30 minutes after the addition was completed. Go to the container that 850 grams of crushed ice are housed, let stand until the crushed ice melts, separate the organic layer and reuse it after fractional distillation. The aqueous layer was adjusted to PH=8 with sodium carbonate, washed with water and dried at 80°C for 3 hours, dissolved in water and added with 0.5 g of a stabilizer, recrystallized to obtain 98 g of flaky crystals, yield 74%, The water after washing and crystallization was extracted with 250 ml of dichloroethane and SB102 ...

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Abstract

The stable synthesis technique for sodium azulenesulfonate comprises: using SB102 and C2H4Cl2 for weak complex reaction with SO3; taking the former product and azulene for sulfonation with SB102; cooling the liquid; separating the organic solvent from the liquid; fractionating in fractionator to discharge water; cleaning the resultant; drying, recrystallizing with stabilizer, and obtaining the product. This invention has no toxic operation, and reduces pollution.

Description

technical field [0001] The invention relates to a synthesis process of sodium azulene sulfonate, in particular to a synthesis process of sodium azulene sulfonate with no pollution, low cost and stable performance. Background technique [0002] Sodium azulene sulfonate, also known as water-soluble azulene. Water-soluble azulene is an active ingredient of chamomile flowers, which has strong anti-pepsin, anti-inflammatory, anti-bacterial, anti-allergic, and promotion of mucosal metabolism. Moreover, it has high safety and can be widely used in various pharmaceutical preparations. Especially for the treatment and prevention of skin and oral diseases, the effect is remarkable. It can also be used in the preparation of toothpaste, cream cosmetics, bath lotion and soap. [0003] Sodium azulene sulfonate, the chemical name is: 3.8-dimethyl-5(1-methylethyl)-1-sodium azulene sulfonate [sodium 3.8-dimethyl-5(1-methylethyl)-1-sulfonate]. Azulene compounds are chemically unstable, an...

Claims

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Application Information

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IPC IPC(8): C07C309/25C07C303/06
Inventor 许荧
Owner 天津顶硕药业股份有限公司
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