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A kind of preparation method of high-yield l-sodium antimony tartrate

A technology of sodium antimony tartrate and sodium hydrogen tartrate, which is applied in the field of preparation of sodium antimony tartrate, can solve the problems of uncomplicated, only 80% yield, and inability to obtain crystals, and achieve the effect of stable quality and easy operation

Active Publication Date: 2018-02-09
NANJING CHEM REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The synthesis of sodium antimony tartrate is not complicated in theory. Most of the existing materials use L-sodium hydrogen tartrate and antimony trioxide to react to produce L-sodium antimony tartrate. However, the synthetic solution of sodium antimony tartrate cannot be obtained by direct concentration. , although it has no obvious decomposition phenomenon at high temperature, after the synthesis liquid is concentrated, a paste-like suspension is obtained, and crystals cannot be obtained even if it is refrigerated for 24 hours
[0003] The preparation aspect data of L-sodium antimony tartrate reported in the literature is very little, and Zhang Jiuzhi published the preparation method of L-sodium antimony tartrate on the pharmacy bulletin of 1958, discloses to use 96% ethanol to add in the filtrate, can separate out L-tartaric acid Sodium antimony crystal, but the preparation of 100g sample needs to consume 500-600ml of 96% ethanol, and the yield is only 80%
Moreover, the content of sodium antimony tartrate reagent on the market is below 98%.

Method used

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  • A kind of preparation method of high-yield l-sodium antimony tartrate

Examples

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Effect test

Embodiment 1

[0020] Weigh 200g of L-sodium hydrogen tartrate and slowly add it to 1500mL of deionized water, and stir while heating. After it is completely dissolved, continue to heat the solution to 90°C, then add 160g of antimony trioxide solid in batches, and stir while adding. After the addition of antimony trioxide, continue to react in boiling state for 2 hours. After the reaction is complete, add 0.016g of sodium sulfide (made into an aqueous solution) to remove arsenic. After stirring for 20 minutes, filter with filter paper. Measure the clarity of the filtrate after filtration. After passing the test, heat and concentrate When the density reaches 1.70g / mL (70°C), cool naturally to room temperature, measure 300ml of absolute ethanol and pour it into a beaker, slowly add the concentrated solution, stir while adding, a large amount of white L-sodium antimony tartrate solid is precipitated, centrifuged for 10min Finally, the solid was dried at 80°C for 10 hours to obtain 333g of the sa...

Embodiment 2

[0024] Weigh 300g of L-sodium hydrogen tartrate and slowly add it to 3000mL of deionized water, and stir while heating. After it is completely dissolved, continue to heat the solution to 80°C, then add 240g of antimony trioxide solid in batches, and stir while adding. After the addition of antimony trioxide, continue to react in boiling state for 6 hours. After the reaction is complete, add 0.1g sodium sulfide (made into an aqueous solution) to remove arsenic. After stirring for 20 minutes, filter it with filter paper. Measure the clarity of the filtrate after filtration. After passing the test, heat and concentrate When the density reaches 1.50g / mL (90°C), cool naturally to room temperature, measure 400ml of absolute ethanol and pour it into a beaker, slowly add the concentrated solution, stir while adding, a large amount of white solid will precipitate out, centrifuge for 10min, and put the solid in Dry at 120° C. for 6 hours to obtain 501 g of the sample (theoretical calcula...

Embodiment 3

[0028] Add 165kg of deionized water to the reaction kettle, then add 33kg of L-sodium hydrogen tartrate in batches, turn on the steam heating, after it is completely dissolved, continue to heat the solution to 90°C, and then add 25kg of antimony trioxide solid in batches, while adding While stirring. After the addition of antimony trioxide, continue to react in a boiling state for 4 hours. After the reaction is complete, add 12.5 g of sodium sulfide (made into an aqueous solution) to remove arsenic. After stirring for 20 minutes, filter it with a four-layer filter bag. Measure the clarity of the filtered filtrate. Qualified, add 150g of activated carbon to re-filter, after the obtained filtrate has qualified clarity, heat and concentrate to a density of 1.60g / mL (85°C), then naturally cool to room temperature, then add 40kg of absolute ethanol to another reaction kettle, and the cooled The concentrated solution was added to absolute ethanol in batches, and stirred while adding...

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Abstract

The invention discloses a preparation method of L-sodium antimony tartrate. Firstly, L-sodium bitartrate is heated and dissolved into deionized water; after a solution is heated to the temperature of 80 DEG C to 90 DEG C; antimonous oxide solid powder is added in batches; the stirring is performed during the addition; after the addition, the reaction is taken for 2 to 6h in a boiling state; then, filtering is performed; filter liquid is heated and concentrated to the density of 1.5 to 1.7g / mL (70 DEG C to 90 DEG C); natural cooling is performed to the room temperature; then, a cooled solution is added into absolute ethyl alcohol in different batches; stirring is performed during the addition; a great amount of white L-sodium antimony tartrate solid is separated out; centrifugation and drying are performed; a finished product of the L-sodium antimony tartrate is obtained. The preparation method of the L-sodium antimony tartrate provided by the invention has the advantages that the quality is stable; the purity is high; the one-step yield reaches 98 percent or higher; the operation is convenient; the preparation method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of chemical reagent preparation, in particular to a method for preparing high-yield L-sodium antimony tartrate. Background technique [0002] Sodium antimony L-tartrate is a white solid powder. Sweet, hygroscopic, toxic, soluble in water, insoluble in ethanol, and its aqueous solution is acidic. It is mainly used as a mordant in the textile and leather industry and as a drug for treating schistosomiasis. The synthesis of sodium antimony tartrate is not complicated in theory. Most of the existing materials use L-sodium hydrogen tartrate and antimony trioxide to react to produce L-sodium antimony tartrate. However, the synthetic solution of sodium antimony tartrate cannot be obtained by direct concentration. , although it has no obvious decomposition phenomenon at high temperature, after the synthesis liquid is concentrated, a paste-like suspension is obtained, and crystals cannot be obtained even if it is refrigerate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/90C07F19/00C07C59/255C07C51/41
CPCC07C51/412C07F9/90C07F9/902
Inventor 丁春玉李清洁鲁华胜
Owner NANJING CHEM REAGENT
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