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Method for recovering DHPG (D-para-hydroxyphenylglycine) from DT (D-para-hydroxyphenylglycine-tosilate) decolorization waste activated carbon

A technology of waste activated carbon and activated carbon, which is applied in the field of medicine and chemical industry, can solve the problems of waste of materials, impact on solid waste-waste activated carbon regeneration treatment, increased cost of DHPG, etc., and achieve the effect of reducing emissions

Inactive Publication Date: 2015-11-25
HENAN NEWLAND PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This will cause a lot of waste of materials, resulting in higher cost of DHPG
At the same time, because the water content in waste activated carbon is too high, it will increase the discharge of solid waste, and because of the existence of part of DHPG carried by it, it will affect the regeneration treatment of solid waste-waste activated carbon

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Add 500ml of pure water and 1000g of DT-containing waste activated carbon (this waste activated carbon is decolorized activated carbon in the synthesis of DHPG, which is a by-product of the reaction, the same below, containing about 2% of DT), into the 1# reaction bottle, Start the stirring device, start the constant temperature water bath to make the temperature reach 60°C, stir at constant temperature for 0.5h, it can be regarded as that DT has been completely dissolved in water, and use a vacuum filter bottle to drain the mixed solution to separate the solid and liquid, and obtain slightly dry waste activated carbon 780g, the filtrate is transferred to 2# reaction flask, add new activated carbon 1.2g, stir and decolorize at 70°C for 0.5h, then filter, and the filtrate enters 3# reaction flask, at 50°C, use 10% liquid Adjust the pH to 5.0 with alkali to precipitate DHPG crystals, then centrifuge to separate 23.7g of DHPG crystals, 21.3g of dry product, and detect that ...

Embodiment 2

[0013] Put 500ml of pure water and 1000g of DT-containing waste activated carbon into the 1# reaction bottle, start the stirring device, start the constant temperature water bath to make the temperature reach 90°C, and stir at constant temperature for 0.5h, which can be regarded as DT has been completely dissolved in the water. Vacuum suction filter bottle mixed solution is drained, and solid-liquid separation is obtained, and slightly dry waste activated carbon 770g is obtained, and filtrate is transferred in 2# reaction bottle, adds new activated carbon 1.2g, stirs and decolorizes 0.5h under 95 DEG C of conditions, then Filter, and the filtrate enters the 3# reaction bottle, and at 75°C, adjust the pH to 7.0 with 25% liquid caustic soda to precipitate DHPG crystals, and then centrifuge to separate 24.7g of DHPG crystals, 22.3g of dry products, and detect the optical rotation of DHPG is -141.6°.

Embodiment 3

[0015] Put 500ml of pure water and 1000g of DT-containing waste activated carbon into the 1# reaction bottle, start the stirring device, start the constant temperature water bath to make the temperature reach 75°C, and stir at constant temperature for 0.5h, which can be regarded as DT has been completely dissolved in the water. With vacuum filter bottle, mixed solution is drained, and solid-liquid separation is obtained, and slightly dry waste activated carbon 750g is obtained, and filtrate is transferred in 2# reaction bottle, adds new activated carbon 1.2g, stirs and decolorizes 0.5h under 80 DEG C of conditions, Then filter, and the filtrate is transferred to 3# reaction bottle, and under the condition of 70 DEG C, the pH is adjusted to 6.0 with 25% liquid caustic soda, the DHPG crystallization is separated out, then the DHPG crystal 25.7g is separated by centrifugation, and the dry product 22.5g is detected. The optical rotation of DHPG is -148.6°.

[0016] Sufficiently fi...

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PUM

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Abstract

The invention belongs to the technical field of medical chemical industry, and relates to a method for recovering DHPG (D-para-hydroxyphenylglycine) from DT (D-para-hydroxyphenylglycine-tosilate) decolorization waste activated carbon, which comprises the following steps: a. waste activated carbon soaking and washing: adding the DT-containing waste activated carbon into 60-90-DEG C water, and stirring; b. solid-liquid separation: putting the mixture obtained in the step a into a centrifuge to obtain a filtrate and a filter cake; c. decolorization: heating the filtrate obtained in the step b to 70-95 DEG C, adding new activated carbon and stirring; d. solid-liquid reseparation: filtering the mixed solution obtained in the step c to obtain a filtrate and a filter cake; e. hydrolysis and crystallization: dropwisely adding 10-40% of liquid alkali into the filtrate obtained in the step d at 50-75 DEG C until the pH value reaches 5-7 to precipitate a crystal, and carrying out solid-liquid separation to obtain the crystal DHPG crude product. The method can effectively recover part of expensive DHPG.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and in particular relates to a technology for recovering DHPG from DT decolorization waste activated carbon. Background technique [0002] L-p-hydroxyphenylglycine (DHPG) is an important pharmaceutical intermediate. It is DHPG after purification, decolorization and hydrolysis of L-p-hydroxyphenylglycine-p-toluenesulfonate (DT). [0003] During the decolorization process of DT, activated carbon is used, and a part of DT will be taken away by the activated carbon, and more will be adhered and taken away in winter or when the temperature is low. This will cause a lot of material waste, resulting in increased cost of DHPG. At the same time, because the water content in waste activated carbon is too high, it will increase the discharge of solid waste, and because of the existence of part of DHPG carried by it, it will affect the regeneration treatment of solid waste-waste activ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/36C07C227/30C07C227/34C07C309/30C07C303/32C07C303/44
Inventor 谢建中车云峰王利英师红亮吴佳王鹏举
Owner HENAN NEWLAND PHARMA