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A method of recovering tartaric acid from calcium tartrate using interfacial reaction

A calcium tartrate and interfacial reaction technology, applied in the chemical field, can solve the problems of low recycling cost, high cost, and high energy consumption in the recycling process, and achieve the effects of low recycling cost, improved purity and yield, and shortened concentration time

Inactive Publication Date: 2019-12-24
上海清研新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to solve the problems existing in the above-mentioned prior art, overcome the problems of large energy consumption and high cost of the existing tartaric acid recovery process, and provide a kind of process stable, high recovery rate, easy to control the reaction conditions from calcium tartrate reclaim tartaric acid The method reduces the amount of concentrated sulfuric acid and reduces the solvent distillation temperature. The method is simple in process, saves the time-consuming and energy-consuming water removal process in the product collection stage, reduces the time of the product at high temperature, avoids side reactions, and simplifies the purification process while using The reaction yield is improved, the recovery cost is low, the product purity is high, and the waste water is produced less

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In a 100L glass-lined reaction kettle, add 60kg of dioxane, 4.1kg of 98% sulfuric acid and stir, add about 8.57kg of calcium tartrate solid in batches, control the temperature in the kettle at 60°C, and stir at 60°C for 2 hours after the addition is completed. Suction filtration to remove impurities such as insoluble inorganic salt calcium sulfate, let stand, collect tartaric acid dioxane mother liquor to the storage tank, or directly transfer to the concentration kettle. Recover the solvent by distillation under normal pressure or reduced pressure, control the final vacuum degree to -0.07~-0.1Mpa, T ≤ 80°C, dry at 55~80°C for 4~6 hours, and obtain the tartaric acid product. Solvent applied with the next batch. The yield of recovered tartaric acid is 96.3%. After analysis: HPLC content ≥99%, melting point: 169-171°C.

Embodiment 2

[0021] In a 100L glass-lined reaction kettle, add 40kg of butanone, 9.5kg of 98% sulfuric acid and stir, add about 20kg of calcium tartrate solid in batches, control the temperature in the kettle to 80°C, and stir at 80°C for 1hr after the addition is completed. Suction filtration to remove impurities such as insoluble inorganic salt calcium sulfate, let stand, collect tartaric acid dioxane mother liquor to the storage tank, or directly transfer to the concentration kettle. Recover the solvent by distillation under normal pressure or reduced pressure, control the final vacuum degree to -0.07~-0.1Mpa, T ≤ 80°C, dry at 55~80°C for 4~6 hours, and obtain the tartaric acid product. Solvent applied with the next batch. The yield of recovered tartaric acid is 95.6%. After analysis, the HPLC content is ≥98.5%, and the melting point is 169-171°C.

Embodiment 3

[0023] In a 100L glass-lined reactor, add 50kg of dioxane, 5.5kg of 85% phosphoric acid and stir, add about 10kg of calcium tartrate solid in batches, control the temperature in the kettle to 70°C, and stir at 70°C for 1.5hr after the addition. Suction filtration to remove impurities such as insoluble inorganic salt calcium sulfate, let stand, collect tartaric acid dioxane mother liquor to the storage tank, or directly transfer to the concentration kettle. Recover the solvent by distillation under normal pressure or reduced pressure, control the final vacuum degree to -0.07~-0.1Mpa, T ≤ 80°C, dry at 55~80°C for 4~6 hours, and obtain the tartaric acid product. Solvent applied with the next batch. The yield of recovered tartaric acid is 94%. After analysis, the HPLC content is ≥98.2%, and the melting point is 169-171°C.

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Abstract

The invention discloses a method for recovering tartaric acid from reaction of calcium tartrate and inorganic acid by using interface reaction, which comprises the following steps: by using an inert organic solvent as a reaction medium system, performing acidifying precipitation, carrying out reduced pressure distillation to recover the solvent, and drying the material to obtain the target productwith the yield of 93-96% and the purity of more than 98%. The method is simple in process (recrystallization is not needed, and the organic solvent is easy to recover), high in recovery rate, easy tocontrol reaction conditions and free of wastewater generation, and overcomes the problems of high energy consumption and high cost of an existing tartaric acid recovery process.

Description

technical field [0001] The invention relates to the technical field of chemistry, in particular to a method for recovering tartaric acid from calcium tartrate by using interface reaction. Background technique [0002] Tartaric acid is an important organic raw material widely used in medicine, food, chemical and textile industries. As the starting material of various chemical reactions, especially the synthesis of chiral substances, tartaric acid has played an increasingly obvious role in the field of pharmaceutical synthesis in recent years. In actual production, if the tartaric acid in the waste water is not recycled and reused, it will cause great waste and greatly increase the production cost of the product. At present, the recovery method of tartaric acid is generally to add calcium chloride in waste water to react, generate calcium tartrate precipitation, make tartaric acid separate from waste water, then use water as solvent, add calcium tartrate, add sulfuric acid to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/02C07C59/255
CPCC07C51/02C07C59/255
Inventor 杜萍其他发明人请求不公开姓名
Owner 上海清研新材料科技有限公司
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