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Process for preparing D-glucosamine hydrochlorate

A technology of glucosamine hydrochloride and a production method, which is applied to amino sugars, sugar derivatives, sugar derivatives, etc., can solve the problems of poor effect, large amount of acetic acid in hydrochloric acid, and low concentration of recycled hydrochloric acid, etc. The effect of pollution, reducing waste liquid discharge and improving utilization rate

Inactive Publication Date: 2008-12-03
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

After research, it is found that the effect of recycling hydrochloric acid is very poor, the main reason is that the concentration of recycled hydrochloric acid is low, and the amount of acetic acid contained in hydrochloric acid is relatively large

Method used

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  • Process for preparing D-glucosamine hydrochlorate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The production method of D-glucosamine hydrochloride comprises the steps: (see figure 1 )

[0018] (1) Add 240g chitin, 626g 37% hydrochloric acid and 200g ethanol in the reaction distillation device, the temperature is controlled at 50°C, after the addition is complete, the controlled temperature is 95°C for reaction, the top obtains distillate (ester and water etc. form a co- Boilers go up to the top of the distillation tower, and condense on the top of the tower, and are divided into two phases, the water phase refluxes and re-enters the reaction distillation device, while the oil phase is crude ester, which can be refined to obtain ethyl acetate) and the bottom to obtain the residual liquid ;

[0019] (2) filtering the residual liquid to remove slag, cooling the filtrate to precipitate solids, and separating the solid and liquid to obtain crude D-glucosamine hydrochloride and primary mother liquor;

[0020] (3) Dissolve the crude glucosamine in hot water at a mass...

Embodiment 2

[0025] The production method of D-glucosamine hydrochloride comprises the steps:

[0026] (1) Add chitin, sulfuric acid (mass fraction: 70%) and methanol into the reaction distillation device, heat up to 85° C., carry out the reaction, obtain the distillate at the top and obtain the residual liquid at the bottom;

[0027] (2) filtering the residual liquid to remove slag, cooling the filtrate to precipitate solids, and separating the solid and liquid to obtain crude D-glucosamine hydrochloride and primary mother liquor;

[0028] (3) Dissolve the crude D-glucosamine hydrochloride in hot water at a mass ratio of 1:1, add 2% activated carbon of the mass of the crude D-glucosamine hydrochloride, reflux for 20 minutes, and filter while hot, The filtrate was evaporated at 70°C to precipitate a solid. Dissolve the solid in ethanol, control the mass ratio of ethanol to the precipitated solid to be 3:1, stir, cool and stand still, crystals precipitated during the cooling process, filter...

Embodiment 3

[0031] The production method of D-glucosamine hydrochloride comprises the steps:

[0032] (1) Add chitin, 37% hydrochloric acid and propanol to the reaction distillation device, heat up to 110° C., carry out the reaction, obtain the distillate at the top and obtain the residual liquid at the bottom;

[0033] (2) filtering the residual liquid to remove slag, cooling the filtrate to precipitate solids, and separating the solid and liquid to obtain crude D-glucosamine hydrochloride and primary mother liquor;

[0034] (3) Dissolve the crude D-glucosamine hydrochloride in hot water at a mass ratio of 1:4, add 5% activated carbon of the mass of the crude D-glucosamine hydrochloride, reflux for 100 minutes, and filter while hot, The filtrate was evaporated at 80°C to precipitate a solid. Dissolve the solid in ethanol, control the mass ratio of ethanol to the precipitated solid to be 5:1, stir, cool and stand still, and crystals precipitated during the cooling process, filtered and wa...

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Abstract

The invention discloses a method for preparing D-glucoseamine hydrochloride, which comprises the steps as follows: (1) adding chitosan, inorganic acid and low-carbon alcohol to a reaction distillation device, and heating to a temperature of 85-110 DEG C to carry out a reaction to obtain a distillate at the tower top and a residual solution at the tower bottom; (2) filtering the residual solution to remove residue and obtain a filtrate, cooling the filtrate to separate out the solid, and carrying out solid-liquid separation to obtain coarse D-glucoseamine hydrochloride and a first mother liquid; dissolving the coarse D-glucoseamine hydrochloride into the hot water, adding activated carbon, refluxing, filtering, evaporating the filtrate to separate out the solid, dissolve the solid into ethanol, stirring, cooling, and standing to separate out crystals, filtering and drying to obtain D-glucoseamine hydrochloride. The method can remove the acetic acid generated from the reaction from the reaction system in time, thereby improving the utilization ratio of the raw material and the yield of D-glucoseamine hydrochloride and reducing the waste solution discharge and the environmental pollution.

Description

technical field [0001] The invention relates to a production method of D-glucosamine hydrochloride. Background technique [0002] For many years, the production of D-glucosamine hydrochloride has always been extracted from crustacean shells. The conventional process conditions are: the chitin raw material is hydrolyzed with hydrochloric acid, cooled, crystallized, and separated to obtain crude D-glucosamine hydrochloride , into the next refined production process. When separating the crude product, another part obtained simultaneously is D-glucosamine hydrochloride mother liquor. The mother liquor is evaporated under reduced pressure to recover hydrochloric acid; the mother liquor is cooled, crystallized, centrifuged, and recovered again to obtain a part of crude D-glucosamine hydrochloride. The secondary mother liquor obtained after separation is recycled with the evaporated low-strength hydrochloric acid, but because the recovered hydrochloric acid has a low concentratio...

Claims

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Application Information

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IPC IPC(8): C07H5/06C07H1/00
Inventor 王富民张旭斌蔡旺峰郭克伦孙高奎
Owner TIANJIN UNIV
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