Preparation method of sulfoacetic acid disodium salt

A technology of sodium acetate sulfonate and sodium chloroacetate, applied in the directions of sulfonate preparation, organic chemistry, etc., can solve the problems of reduced synthesis yield, slow synthesis efficiency, low yield, etc., and achieves improved reaction temperature and shortened reaction time. , the effect of improving the reaction efficiency

Active Publication Date: 2019-05-24
广州花语精细化工有限公司
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AI Technical Summary

Problems solved by technology

[0005] Both of the above two technologies have shortcomings such as low yield and slow synthesis efficiency
The main reason is: the temperature during the reaction between chloroacetic acid or ethyl acetate and sodium sulfite should not be too high, generally controlled at 50-60°C, otherwise it will cause chloroacetic acid or ethyl acetate to volatilize and reduce the synthesis yield, while the temperature will be too low. The reaction efficiency is abnormally slow, and the comprehensive yield is less than 60%.

Method used

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preparation example Construction

[0027] A preparation method of sodium sulfonate (chemical reaction equation is shown in reaction formula II), comprising:

[0028] Liquid preparation step: dissolve chloroacetic acid, add sodium hydroxide to neutralize, control the temperature of the system not to exceed 50°C, and obtain a sodium chloroacetic acid solution with a pH of 6-7; at this time, chloroacetic acid is not completely neutralized, mainly The reason is that the pH value after complete neutralization is alkaline, which will cause the hydrolysis of chloroacetic acid to glycolic acid, thereby reducing the final conversion rate;

[0029] Dissolving step: Put sodium sulfite into the reaction kettle, add water and stir to dissolve, and raise the temperature to 60-80°C;

[0030] Reaction steps: drop sodium chloroacetate solution into the reaction kettle, maintain the temperature in the reaction kettle at 60-80°C, control the pH at 8-10, control the dropping time at 1-5h, and keep warm for reaction after the dropp...

Embodiment 1

[0050] A preparation method of sodium sulfonate, comprising:

[0051] Solution preparation step: add water to dissolve 40g of chloroacetic acid to 100g, and add 48g of 32% sodium hydroxide to neutralize, control the adding speed of lye so that the temperature of the system is 45-50°C, and obtain pH = 6-7 Sodium chloroacetate solution;

[0052] Dissolving step: put 56g of sodium sulfite into the reaction kettle, add 144g of water to stir and dissolve, and raise the temperature to 75-80°C;

[0053] Reaction steps: drop the sodium chloroacetate solution into the reaction kettle, maintain the temperature in the reaction kettle at 75-80°C, control the pH at 8.5-9.5, add the dropping time for 5 hours, and keep warm for 3 hours after the dropping is completed;

[0054] Precipitation step: Carry out rotary evaporation of the reacted material at a vacuum degree of -0.095MPa and a temperature of 85-90°C. When evaporating to a saturated solution, lower the temperature to 15-20°C, place it...

Embodiment 2

[0057] The difference between embodiment 2 and embodiment 1 is:

[0058] In the liquid preparation step, 40 g of chloroacetic acid was dissolved in water to 100 g, and 48 g of sodium hydroxide with a concentration of 32% was added for neutralization, and the addition rate of lye was controlled so that the temperature of the system was 35-40°C;

[0059] In the dissolving step, put 58g of sodium sulfite into the reaction kettle and heat up to 60-65°C;

[0060] In the reaction step, the temperature in the reactor is maintained at 60-65°C, the pH is controlled at 9-10, the dropping time is 1h, and the reaction is kept for 1h after the dropping;

[0061] In the precipitation step, the material after the reaction is subjected to rotary evaporation at a vacuum degree of -0.095MPa and 80-85°C, cooled to 20-25°C, and placed for 20h for precipitation; and the crystal is dissolved in anhydrous In ethanol, impurities such as sodium chloroacetate, sodium chloride, and sodium sulfite can b...

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Abstract

The invention discloses a preparation method of a sulfoacetic acid disodium salt. The method comprises the steps of solution preparation: chloroacetic acid is dissolved, sodium hydroxide is added to neutralize, the temperature of a system is controlled to not exceed 50 DEG C, and a sodium chloroacetate solution with pH=6-7 is obtained; dissolving: sodium sulphite is put into a reaction kettle, water is added to stir and dissolve, and the temperature is increased to 60-80 DEG C; reaction: the sodium chloroacetate solution is added to the reaction kettle dropwisely, the temperature in the reaction kettle is maintained to be 60-80 DEG C, the pH is 8-10, the dropwise adding time is 1-5 hours, and heat preservation reaction is conducted for 1-3 hours after dropwise adding; precipitation: reacted raw materials are steamed until the solution is saturated, crystals are obtained after precipitation and filtering, and the crystals are dissolved in absolute alcohol to obtain a semi-finished product; drying: the semi-finished product is distilled and dried to obtain sulfoacetic acid disodium salt crystals. The preparation method has the advantages that the reaction efficiency is high, the reaction time is short, and the comprehensive yield is improved to 85% or above.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of sodium sulfoacetate. Background technique [0002] As an intermediate of various chemical raw materials, sodium sulfonate acetate is widely used, mainly in the fields of washing and daily chemical industry. Synthetic sodium sulfoacetate mainly contains two kinds in prior art: 1, use chloroacetic acid to react directly with sodium sulfite, 2, use ethyl acetate to react with sodium sulfite. Wherein, the chemical equation of chloroacetic acid and sodium sulfite reaction is: [0003] Cl-CH 2 COOH+Na 2 SO 3 →NaSO 3 CH 2 COOH+NaCl [0004] Reaction formula Ⅰ [0005] The above two technologies all have the disadvantages of low yield and slow synthesis efficiency. The main reason is that the temperature during the reaction between chloroacetic acid or ethyl acetate and sodium sulfite should not be too high, generally controlled at 50-60 ° C, ot...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/32C07C309/17
Inventor 刘振华张涌
Owner 广州花语精细化工有限公司
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