Meglumine production process capable of recycling solvent

A production process, the technology of meglumine, which is applied in the field of solvent reuse meglumine production process, can solve the problems of poor dehydration effect, achieve the effects of increased recovery rate, reduced water content, and reduced recovery cost

Inactive Publication Date: 2021-04-06
弘健制药(上海)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Anhydrous ethanol is used as a solvent. It needs to be distilled to remove water before it can be reused. The dehydration effect is poor, and only a small proportion of ethanol can be reused.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] The preparation steps of the catalyst are as follows: melt 50g of aluminum at 800°C, melt 7g of rhodium, 40g of nickel, and 3g of chromium at a temperature of 2500°C, then add the molten rhodium, nickel, and chromium to the molten aluminum, stir evenly, and cool , and then the alloy is melted, sprayed, and rapidly cooled by a spray method to obtain an aluminum-nickel-chromium-rhodium alloy, and the particle size of the screened aluminum-nickel-chromium-rhodium alloy is 80-100 mesh.

[0038] Then stir the 25wt% sodium hydroxide solution and raise the temperature to 43°C, then gradually add the aluminum-nickel-chromium-rhodium alloy powder. After 2.6 hours, let cool to 60° C., stop stirring, wash repeatedly with water until the pH is 7, and then wash with absolute ethanol until the content of ethanol in the feed liquid is 96%.

[0039] A kind of meglumine production technique of solvent recycling, comprises the following steps:

[0040] S1: Pass monomethylamine gas into ...

Embodiment 2

[0049] The difference with embodiment 1 is:

[0050]Add sulfuric acid to the mother liquor obtained in step S2 to adjust the pH to 7, add silica gel particles, the mass ratio of silica gel to mother liquor is 1:2.2, and continue to stir and mix for 10 minutes, then filter out the silica gel particles to obtain the filtrate, and add oxidation Calcium and keep stirring, until the calcium oxide no longer reacts, continue to add calcium oxide, and the mass ratio of the calcium oxide to the concentrated sulfuric acid that continues to be added is 1:2, after the calcium oxide is added, add 98wt% concentrated sulfuric acid, until The pH is 7, and the ethanol recovery liquid is obtained by distillation.

[0051] After the silica gel particles filtered out of the mother liquor are dried at 105°C for 1.5 hours, the mother liquor can be further dried.

Embodiment 3

[0053] The difference with embodiment 1 is:

[0054] Add sulfuric acid to the mother liquor obtained in step S2 to adjust the pH to 7, add silica gel particles, the mass ratio of silica gel to mother liquor is 1:2, and continue to stir and mix for 20 minutes, then filter out the silica gel particles to obtain the filtrate, add oxidation Calcium and keep stirring, until the calcium oxide no longer reacts, continue to add calcium oxide, and the mass ratio of the calcium oxide to the concentrated sulfuric acid that continues to add is 1:1.85, after the calcium oxide is added, add the concentrated sulfuric acid of 98wt%, until The pH is 7, and the ethanol recovery liquid is obtained by distillation.

[0055] After the silica gel particles filtered out of the mother liquor are dried at 100°C for 2 hours, the mother liquor can be further dried.

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Abstract

The invention relates to a meglumine production process capable of recycling a solvent. The meglumine production process comprises the following steps: S1, condensing monomethylamine with glucose in absolute ethyl alcohol to obtain a Schiff's salt; S2, adding a catalyst and absolute ethyl alcohol into the Schiff's salt, introducing hydrogen for a reaction to obtain hydride, conducting crystallizing to obtain solid hydride and mother liquor, separating the solid hydride, melting the hydride, adding disodium ethylene diamine tetraacetate, conducting concentrating under reduced pressure, and carrying out centrifugal filtration to obtain a crude meglumine product; S3, recrystallizing the crude meglumine product in methanol to obtain a methanol mother solution and a wet meglumine product, and distilling the methanol mother solution under reduced pressure to obtain a methanol recovery solution; and S4, adding sulfuric acid into the mother solution obtained in the step S2 to adjust a pH value to 6-7, adding silica gel particles, continuously conducting stirring and uniform mixing, filtering out the silica gel particles to obtain a filtrate, and conducting distilling to obtain an ethanol recovery solution. The process of the invention has the effect of improving ethanol recovery and dehydration effect.

Description

technical field [0001] The present application relates to the field of meglumine production, in particular to a solvent recycling meglumine production process. Background technique [0002] Meglumine, also known as glucose methylamine or 1-deoxy-1-methylamine sorbitol, is used for the preparation of contrast agent drugs diatrizoate meglumine and biliary meglumine, and is also used as an adjuvant or intermediate for other drugs. [0003] In the related technology, glucose is firstly condensed with methylamine in absolute ethanol to form Schiff's salt, hydrogen is used as hydrogen source, Raine's nickel is used as catalyst to synthesize meglumine, and it is produced by catalytic hydrogenation. [0004] Anhydrous ethanol is used as a solvent, and it needs to be distilled to remove water before it can be reused. The dehydration effect is poor, and only a small proportion of ethanol can be reused. Contents of the invention [0005] In order to improve the dehydration effect, t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/02C07C213/10C07C215/10C07C29/74C07C29/76C07C29/88C07C31/08
CPCC07C213/02C07C213/10C07C249/02C07C29/74C07C29/76C07C29/88
Inventor 卿文彬张征彬李琳张来弟周秋火柏挺华吉涛
Owner 弘健制药(上海)有限公司
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