CN1335322A

CN1335322A - Prepn of aminoglucose hydrochloride

Info

Publication number: CN1335322A
Application number: CN 01127784
Authority: CN
Inventors: 王成祥; 李江平
Original assignee: MEIYAN BLUE-GREEN ALGAL Co Ltd MEI COUNTY GUANGDONG PROV
Current assignee: MEIYAN BLUE-GREEN ALGAL Co Ltd MEI COUNTY GUANGDONG PROV
Priority date: 2001-08-24
Filing date: 2001-08-24
Publication date: 2002-02-13
Anticipated expiration: 2021-08-24
Also published as: CN1161367C

Abstract

The preparation process of aminoglucose hydrochloride includes the steps of: the crushing, water washing, acid pickling with dilute hydrochloric acid and stoving of chitin; deacetylation and hydrolysis of the chitin with concentrated hydrochloric acid inside a reactor and filtering; concentration of filtrate in a vacuum concentrator while absorbing the volatilized HCl gas with alkali solution; purification of the filtrate inside one other reactor with water and active carbon at vacuum filtering and re-filteirng; further concentration of the filtrate in the vacuum concentrator, and the cooling to room temperature, filtering, washing with sprayed ethanol and stoving of the concentrate. The present invention has low ethanol consumption, short production period and low cost.

Description

The preparation method of glucosamine hydrochloride

The present invention relates to a kind of preparation method of glucosamine hydrochloride, particularly a kind of method of producing glucosamine hydrochloride with the chitin after the screening of production chitosan.

D-glucosamine hydrochloride (D-Glucosamine Hydrochloride) is widely used in that medicine is synthetic, bacterial-infection resisting and immunological adjuvant, it is the activator of human body resisiting influenza virus, it can promote the synthetic of osteocyte protein-polysaccharide, improve the viscosity of joint lubrication liquid, improve the joint cartilage metabolism, effectively therefore treatment rheumatic arthritis be called by the world of medicine " agent of OA amelioration of disease ".It is the main raw material of synthetic cancer therapy drug NSC-178248.It also is the good medicine of treatment infantile diarrhea and long-term chronic intestinal inflammations.

The method of traditional mode of production glucosamine hydrochloride is: with chitin, concentrated hydrochloric acid and after add water and activated carbon powder is placed in the same retort, parameter and condition (temperature, churning time, reaction times etc.) control is bad, hydrolysis reaction is not thorough, forming short chain molecule and oligosaccharides and activated carbon is bonded together, make entire reaction be difficult to carry out, again contaminate environment; Even hydrolysis is complete, remaining hydrochloric acid need increase production cost with a large amount of washing with alcohol, has prolonged the production cycle.

Purpose of the present invention just provides a kind of with short production cycle, the preparation method of the glucosamine hydrochloride that cost is low.

The present invention can realize in the following manner: (1) pulverizes chitin, after washing and dilute hydrochloric acid are washed, and oven dry; (2) put into retort, add concentrated hydrochloric acid, after deacetylation and the hydrolysis, use the double deck screen net filtration; (3) filtrate changes vacuum concentration pot over to, concentrates, and absorbs the hydrogen chloride gas that volatilizes with alkali lye; (4) filtrate changes in another retort, adds entry and gac, and under vacuum filtration, the filtrate behind the purifying is passed through filter cloth; (5) filtrate changes vacuum concentration pot again over to, concentrates again, is cooled to room temperature, filters, and sprays ethanol, pumps ethanol, oven dry.Chitin is crushed to 3～15 millimeters.The concentration of dilute hydrochloric acid is 0.5～3%.The concentration of concentrated hydrochloric acid is 36～38%, adds 2～6 parts (weight parts, down together), and 50～100 ℃ of temperature controls were stirred 1～4 hour.30～80 millimeters of the net spacings of double-deck screen cloth, upper wire is 50～100 orders, lower net is 100～300 orders.45～85 ℃ of thickening temperature controls, vacuum tightness-0.075～-0.04MPa, 2～4 hours time.Add 0.5～5 part water and 0.05～0.2 part gac, granularity is 90～200 orders, and 50～90 ℃ of temperature controls were stirred 1～2 hour, and under vacuum filtration, the filtrate behind the purifying is discharged on 80～250 order filter clothes, carries out vacuum filtration.Crystal forwards on 80～250 order filter clothes, sprays ethanol, and suction filtration is clean, sprays again, pumps ethanol again, until pH value 3～5 o'clock, crystal is forwarded in the container, heats 40～90 ℃, vacuum tightness-0.07～-0.04MPa, 1～4 hour time.

The present invention utilizes the scrap stock chitin of producing after chitosan screens to be raw material, and absorb hydrochloric acid with the waste lye of producing chitosan, reduced the required consumption of ethanol of washing hydrochloric acid, consumption of ethanol only is 1/6～1/8 of a traditional technology, use the double deck screen net filtration, speed is fast, has the raw material comprehensive utilization, characteristics with short production cycle, that cost is low.

Below in conjunction with embodiment, the invention will be further described.

Embodiment one

(our company has applied for the preparation method of chitosan for raw material to utilize our company to produce chitin 1kg under food, the screening of medical grade chitosan, number of patent application 01107664.X), be crushed to 3 millimeters with pulverizer, when pulverizer is pulverized chitin, because coming off of pulverizer can produce the iron filings of minute quantity, then with the iron filings in the magnet absorption chitin, then, after the dilute hydrochloric acid of water flushing and concentration 0.5% is washed, dry or dry; Chitin after drying or drying drops in the acid tolerance response jar, adding 2kg concentration is 36% concentrated hydrochloric acid, temperature is controlled at 50 ℃, stirs 1 hour, finish deacetylation and hydrolysis reaction after, with the acidproof screen cloth of bilayer, the net spacing of double-deck screen cloth is 30 millimeters, and upper wire is 50 orders, and lower net is 100 orders, filter, discard filter residue; Filtrate is forwarded in the acidproof vacuum concentration pot, 45 ℃ of temperature controls, vacuum tightness-0.075Mpa, 2 hours time, concentrate, drive away the superfluous hydrochloric acid of most of reaction, absorb the hydrogen chloride gas that volatilizes with the waste lye of producing chitosan, to prevent polluted air; Filtrate is transferred in another retort, adds 0.5kg deionized water and 0.05kg activated carbon, and granularity is 90 orders, temperature is controlled at 50 ℃, stirs 1 hour, under vacuum filtration, solution behind the purifying is discharged into acidproof filter cloth (80 order), carries out vacuum filtration, reclaims filter cake and focuses on; Filtrate enters in the vacuum concentration pot again, concentrates again, shuts down cool to room temperature; separate out crystal, filter with 80 purpose filter clothes, filtrate is recovered to next operation; spray ethanol, suction filtration is clean, sprays again; pumping the ethanol of washing again, is 3 o'clock until pH value, and crystal is transferred in the enamel tray; put into vacuum drying oven, heat 40 ℃, vacuum tightness-0.07MPa; after 1 hour, promptly get glucosamine hydrochloride 0.45kg.

Embodiment two

(our company has applied for the preparation method of chitosan for raw material to utilize our company to produce chitin 1kg under food, the screening of medical grade chitosan, number of patent application 01107664.X), be crushed to 15 millimeters with pulverizer, when pulverizer is pulverized chitin, because coming off of pulverizer can produce the iron filings of minute quantity, then with the iron filings in the magnet absorption chitin, then, after the dilute hydrochloric acid of water flushing and concentration 3% is washed, dry or dry; Chitin after drying or drying drops in the acid tolerance response jar, adding 6kg concentration is 38% concentrated hydrochloric acid, temperature is controlled at 100 ℃, stirs 4 hours, finish deacetylation and hydrolysis reaction after, with the acidproof screen cloth of bilayer, the net spacing of double-deck screen cloth is 80 millimeters, and upper wire is 100 orders, and lower net is 300 orders, filter, discard filter residue; Filtrate is forwarded in the acidproof vacuum concentration pot, 85 ℃ of temperature controls, vacuum tightness-0.04Mpa, 4 hours time, concentrate, drive away the superfluous hydrochloric acid of most of reaction, absorb the hydrogen chloride gas that volatilizes with the waste lye of producing chitosan, to prevent polluted air; Filtrate is transferred in another retort, adds 5kg deionized water and 0.2kg activated carbon, and granularity is 200 orders, temperature is controlled at 90 ℃, stirs 2 hours, under vacuum filtration, solution behind the purifying is discharged into acidproof filter cloth (250 order), carries out vacuum filtration, reclaims filter cake and focuses on; Filtrate enters in the vacuum concentration pot again, concentrates again, shuts down cool to room temperature; separate out crystal, filter with 250 purpose filter clothes, filtrate is recovered to next operation; spray ethanol, suction filtration is clean, sprays again; pumping the ethanol of washing again, is 5 o'clock until pH value, and crystal is transferred in the enamel tray; put into vacuum drying oven, heat 90 ℃, vacuum tightness-0.04MPa; after 4 hours, promptly get glucosamine hydrochloride 0.48kg.

Claims

1, a kind of preparation method of glucosamine hydrochloride is characterized in that:

(1) chitin is pulverized, after washing and dilute hydrochloric acid are washed, oven dry;

(2) put into retort, add concentrated hydrochloric acid, after deacetylation and the hydrolysis, use the double deck screen net filtration;

(3) filtrate changes vacuum concentration pot over to, concentrates, and absorbs the hydrogen chloride gas that volatilizes with alkali lye;

(4) filtrate changes in another retort, adds entry and gac, and under vacuum filtration, the filtrate behind the purifying is passed through filter cloth;

(5) filtrate changes vacuum concentration pot again over to, concentrates again, is cooled to room temperature, filters, and sprays ethanol, pumps ethanol, oven dry.

2,, it is characterized in that chitin is crushed to 3～15 millimeters according to the described preparation method of claim 1.

3, according to the described preparation method of claim 1, the concentration that it is characterized in that dilute hydrochloric acid is 0.5～3%.

4, according to the described preparation method of claim 1, the concentration that it is characterized in that concentrated hydrochloric acid is 36～38%, adds 2～6 parts (weight parts, down together), and 50～100 ℃ of temperature controls were stirred 1～4 hour.

5, according to the described preparation method of claim 1, it is characterized in that 30～80 millimeters of the net spacings of double-deck screen cloth, upper wire is 50～100 orders, lower net is 100～300 orders.

6, according to the described preparation method of claim 1, it is characterized in that 45～85 ℃ of thickening temperature controls, vacuum tightness-0.075～-0.04MPa, 2～4 hours time.

7, according to the described preparation method of claim 1, it is characterized in that adding 0.5～5 part water and 0.05～0.2 part gac, granularity is 90～200 orders, 50～90 ℃ of temperature controls, stirred 1～2 hour, under vacuum filtration, the filtrate behind the purifying is discharged on 80～250 order filter clothes, carries out vacuum filtration.

8, according to the described preparation method of claim 1, it is characterized in that crystal forwards on 80～250 order filter clothes, spray ethanol, suction filtration is clean, sprays again, pump ethanol again, until pH value 3～5 o'clock, crystal is forwarded in the container, heat 40～90 ℃, vacuum tightness-0.07～-0.04MPa, 1～4 hour time.