CN101503433B - Preparation of plant source glucosamine hydrochloride - Google Patents
Preparation of plant source glucosamine hydrochloride Download PDFInfo
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- CN101503433B CN101503433B CN2009100196336A CN200910019633A CN101503433B CN 101503433 B CN101503433 B CN 101503433B CN 2009100196336 A CN2009100196336 A CN 2009100196336A CN 200910019633 A CN200910019633 A CN 200910019633A CN 101503433 B CN101503433 B CN 101503433B
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Abstract
The invention relates to a method for preparing a plant-source D-glucosamine hydrochloride. The plant-source D-glucosamine hydrochloride is mainly prepared by taking waste residues generated in the process of using the plant fermentation method to produce citric acid as raw material, and adopting the steps of acidolysis, cooling, filter pressing, decoloring, distillation and condensation, crystallization, washing, drying, and the like. Compared with prior art, the invention has the advantages of rich raw material resource, no heavy metal or antibiotic pollution, cheapness and easy obtaining. While effectively reducing the production cost, the invention finds a proper approach for treating the environment pollution so as to change waste into a treasure and also save the cost for treating the environment pollution. The invention also has simple and easy production process, good product quality, good economical and social benefit and wide market prospect.
Description
Technical field
The present invention relates to a kind of preparation method of plant-sourced glucosamine hydrochloride, particularly a kind of method of utilizing waste residue to prepare glucosamine hydrochloride.
Background technology
Glucosamine hydrochloride claims Portugal's amine sugar hydrochloride again, be white crystalline powder, in fields such as medicine, food purposes is widely arranged, can be used as bacterial-infection resisting and immunological adjuvant, can make the nutrition accessory agent for the diabetic subject, be the activator of human body resisiting influenza virus, have the treatment rheumatic arthritis, strengthen function of human body and the anti-ageing effect of waiting for a long time.In addition, also can be applicable in makeup, the fodder additives and as food preservatives.At present, demand to glucosamine hydrochloride increases just day by day, the method of traditional production glucosamine hydrochloride is a raw material with the chitin that extracts in the arthropodan shells such as shrimp, crab and insect generally, through acidolysis, filtration, concentrate, steps such as purifying, reconcentration, cooling, filtration, oven dry make, there is following shortcoming in this production method: one, because supply of raw material is subjected to the influence in region and season, and shrimp, crab shell calcium content height cause difficulty to extraction; Add overfishing in recent years, shrimp crab quantity is sharply reduced, thereby cause the chitin resource more in short supply; Two, especially the problem of water pollution is serious day by day in environmental pollution, and existing the detection found to have pesticide residue in the chitin, and therefore the problem that heavy metal and antibiotic content exceed standard is that the quality product that raw material is produced also is subjected to greatly threatening with the chitin; Three, this technological process of production is long and complicated, has increased production cost equally.Therefore, be necessary to explore the method for new production glucosamine hydrochloride.
In recent years, the production development of citric acid is rapid, tradition generally adopts fermentation method production, produces a large amount of waste residues in the fermenting process, once is used as feed and tries out, but because of feed becomes acid, can't apply, thereby cause a large amount of waste residues in time not handle, and mouldy corruption, therefore, the problem for the suitable treatment process of waste residue searching needs to be resolved hurrily.
Summary of the invention
For solving the problems referred to above that exist, the present invention aims to provide the preparation method of the plant-sourced glucosamine hydrochloride that a kind of raw materials cost is low, quality product is high.
The present invention is achieved by the following technical solutions:
The preparation method of described plant-sourced glucosamine hydrochloride, its special character is to adopt following steps:
(1) acidolysis: in the airtight acid-resistant container that has whipping appts, add the waste residue that produces in 300～1000 kilograms of fermentative Production citric acid processes earlier, adding mass concentration again is the hydrochloric acid 600-1200 kilogram of 20%-38%, open and stir, temperature rises to 50-95 ℃, insulation reaction 6-15 hour;
(2) cooling, press filtration: above-mentioned reacted feed liquid cooling is cooled to below 10 ℃, crystallization is separated out from feed liquid, filter, get crude product, it is transferred in another acid-resistant container, adds the deionized water of 1000-1500 kilogram, under stirring condition, heat, make the crude product dissolving, press filtration then;
(3) decolouring: the filtrate after the above-mentioned press filtration is changed in the acid-resistant container of band stirring, add the impurity treatment agent, open and stir, temperature rises to 50-90 ℃, and insulation was decoloured 1～3 hour, filters then, collects filtrate; Described impurity treatment agent is hydrated barta or bariumchloride;
(4) distillation concentrates: above-mentioned filtrate is changed in the encloses container of vacuum-pumping, vacuum distillation, keeping distillation vacuum tightness is 0.06-0.09MPa, when material liquid volume to be steamed is the 70-80% of former filtrate volume, stops distillation, concentrated solution;
(5) crystallization: above-mentioned concentrated solution is cooled to below 35 ℃, have a large amount of solid matters slowly crystallization separate out, filter, obtain crude product;
(6) washing and drying: above-mentioned crude product is not less than 95% washing with alcohol with purity, and the volume ratio of ethanol and crude product is 1: 1.5-3.0; Wash three times, centrifugal or suction filtration gets solids component, and oven dry obtains product then.
For guaranteeing the productive rate of product, temperature preferably rises to 60～85 ℃, insulation reaction 6-10 hour in the step (1); Temperature preferably rises to 60～80 ℃ in the step (3).
According to the difference of gained filtrate quality after step (2) press filtration, the amount that adds the impurity treatment agent in the step (3) is 0.1%～0.5% of a filtrate weight.
The chitin to extract in shrimp, the crab shell that the inventor breaks traditions is the thinking of feedstock production glucosamine hydrochloride, and as raw material, generally the waste residue of producing citric acid with plant fermentation is a raw material with the waste produced; And original manufacturing condition optimized, having simplified technical process, the present invention compared with prior art has following advantage:
The raw materials used waste residue that derives from the fermentative Production citric acid process of the present invention, aboundresources, heavy metal, antibiotic content all do not exceed standard, cheap and easy to get, when effectively reducing production cost, for environmental pollutant have found suitable processing approach, turn waste into wealth, also saved the expense of curbing environmental pollution; Production technique is simple, and quality product is secure, and market outlook are preferably arranged.
Embodiment
The invention will be further described below in conjunction with specific embodiment.
Embodiment 1
The preparation method of plant-sourced glucosamine hydrochloride of the present invention, adopt following steps:
(1) acidolysis: in the airtight acid-resistant container that has whipping appts, add the mycelium that produces in 300 kilograms of fermentative Production citric acid processes earlier, add mass concentration again and be 600 kilograms of 25% hydrochloric acid, open and stir, temperature rises to 65 ℃, insulation reaction 10 hours;
(2) cooling, press filtration: above-mentioned reacted feed liquid cooling is cooled to below 10 ℃, crystallization is separated out from feed liquid, filter, get crude product, it is transferred in another acid-resistant container, add 1000 kilograms deionized water, under stirring condition, heat, crude product is dissolved, then press filtration again;
(3) decolouring: the filtrate after the above-mentioned press filtration is changed in the acid-resistant container that band stirs, add 0.2% the hydrated barta that accounts for the filtrate quality, open and stir, temperature rises to 65 ℃, and insulation decolouring 1.5 hours is filtered then, collects filtrate;
(4) distillation concentrates: above-mentioned filtrate is changed in the encloses container of vacuum-pumping, vacuum distillation, keeping distillation vacuum tightness is 0.06-0.09MPa, when material liquid volume to be steamed is the 70-80% of former filtrate volume, stops distillation, concentrated solution;
(5) crystallization: above-mentioned concentrated solution is cooled to below 35 ℃, have a large amount of solid matters slowly crystallization separate out, filter, obtain crude product;
(6) washing and drying: with above-mentioned crude product purity is 98% washing with alcohol, and the volume ratio of ethanol and crude product is 1: 3; Wash three times, centrifugal or suction filtration gets solids component, and oven dry obtains product then, and productive rate is 4.9%.
Embodiment 2
The preparation method of plant-sourced glucosamine hydrochloride of the present invention, mainly adopt following steps:
(1) acidolysis: in the airtight acid-resistant container that has whipping appts, add the mycelium that produces in 600 kilograms of fermentative Production citric acid processes earlier, add mass concentration again and be 800 kilograms of 20% hydrochloric acid, open and stir, temperature rises to 50 ℃, insulation reaction 15 hours;
(2) cooling, press filtration: above-mentioned reacted feed liquid cooling is cooled to below 10 ℃, crystallization is separated out from feed liquid, filter, get crude product, it is transferred in another acid-resistant container, add 1200 kilograms deionized water, under stirring condition, heat, crude product is dissolved, then press filtration again;
(3) decolouring: the filtrate after the above-mentioned press filtration is changed in the acid-resistant container that band stirs, add 0.3% the bariumchloride that accounts for the filtrate quality, open and stir, temperature rises to 80 ℃, and insulation decolouring 1 hour is filtered then, collects filtrate;
(4) distillation concentrates: above-mentioned filtrate is changed in the encloses container of vacuum-pumping, vacuum distillation, keeping distillation vacuum tightness is 0.06-0.09MPa, when material liquid volume to be steamed is the 70-80% of former filtrate volume, stops distillation, concentrated solution;
(5) crystallization: above-mentioned concentrated solution is cooled to below 35 ℃, have a large amount of solid matters slowly crystallization separate out, filter, obtain crude product;
(6) washing and drying: with above-mentioned crude product purity is 97% washing with alcohol, and the volume ratio of ethanol and crude product is 1: 1.5; Wash three times, centrifugal or suction filtration gets solids component, and oven dry obtains product then, and productive rate is 5.2%.
Embodiment 3
The preparation method of plant-sourced glucosamine hydrochloride of the present invention, mainly adopt following steps:
(1) acidolysis: in the airtight acid-resistant container that has whipping appts, add the mycelium that produces in 800 kilograms of fermentative Production citric acid processes earlier, add mass concentration again and be 1200 kilograms of 30% hydrochloric acid, open and stir, temperature rises to 80 ℃, insulation reaction 9 hours;
(2) cooling, press filtration: above-mentioned reacted feed liquid cooling is cooled to below 10 ℃, crystallization is separated out from feed liquid, filter, get crude product, it is transferred in another acid-resistant container, add 1500 kilograms deionized water, under stirring condition, heat, crude product is dissolved, then press filtration again;
(3) decolouring: the filtrate after the above-mentioned press filtration is changed in the acid-resistant container that band stirs, add 0.1% the bariumchloride that accounts for the filtrate quality, open and stir, temperature rises to 90 ℃, and insulation decolouring 2 hours is filtered then, collects filtrate;
(4) distillation concentrates: above-mentioned filtrate is changed in the encloses container of vacuum-pumping, vacuum distillation, keeping distillation vacuum tightness is 0.06-0.09MPa, when material liquid volume to be steamed is the 70-80% of former filtrate volume, stops distillation, concentrated solution;
(5) crystallization: above-mentioned concentrated solution is cooled to below 35 ℃, have a large amount of solid matters slowly crystallization separate out, filter, obtain crude product;
(6) washing and drying: with above-mentioned crude product absolute ethanol washing, the volume ratio of ethanol and crude product is 1: 2; Wash three times, centrifugal or suction filtration gets solids component, and oven dry obtains product then, and productive rate is 5.1%.
Embodiment 4
The preparation method of plant-sourced glucosamine hydrochloride of the present invention, mainly adopt following steps:
(1) acidolysis: in the airtight acid-resistant container that has whipping appts, add the waste residue that produces in 600 kilograms of fermentative Production citric acid processes earlier, add mass concentration again and be 1000 kilograms of 38% hydrochloric acid, open and stir, temperature rises to 95 ℃, insulation reaction 6 hours;
(2) cooling, press filtration: above-mentioned reacted feed liquid cooling is cooled to below 10 ℃, crystallization is separated out from feed liquid, filter, get crude product, it is transferred in another acid-resistant container, add 1200 kilograms deionized water, under stirring condition, heating, dissolving again, press filtration then;
(3) decolouring: the filtrate after the above-mentioned press filtration is changed in the acid-resistant container that band stirs, add 0.5% the hydrated barta that accounts for the filtrate quality, open and stir, temperature rises to 50 ℃, and insulation decolouring 3 hours is filtered then, collects filtrate;
(4) distillation concentrates: above-mentioned filtrate is changed in the encloses container of vacuum-pumping, vacuum distillation, keeping distillation vacuum tightness is 0.06-0.09MPa, when material liquid volume to be steamed is the 70-80% of former filtrate volume, stops distillation, concentrated solution;
(5) crystallization: above-mentioned concentrated solution is cooled to below 35 ℃, have a large amount of solid matters slowly crystallization separate out, filter, obtain crude product;
(6) washing and drying: with above-mentioned crude product purity is 95% washing with alcohol, and the volume ratio of ethanol and crude product is 1: 1.5; Wash three times, centrifugal or suction filtration gets solids component, and oven dry obtains product then, and productive rate is 4.8%.
Claims (4)
1. the preparation method of a plant-sourced glucosamine hydrochloride is characterized in that adopting following steps:
(1) acidolysis: in the airtight acid-resistant container that has whipping appts, add the waste residue that produces in 300～1000 kilograms of fermentative Production citric acid processes earlier, adding mass concentration again is the hydrochloric acid 600-1200 kilogram of 20%-38%, open and stir, temperature rises to 50-95 ℃, insulation reaction 6-15 hour;
(2) cooling, press filtration: above-mentioned reacted feed liquid cooling is cooled to below 10 ℃, crystallization is separated out from feed liquid, filter, get crude product, it is transferred in another acid-resistant container, adds the deionized water of 1000-1500 kilogram, under stirring condition, heat, make the crude product dissolving, press filtration then;
(3) decolouring: the filtrate after the above-mentioned press filtration is changed in the acid-resistant container of band stirring, add the impurity treatment agent, open and stir, temperature rises to 50-90 ℃, and insulation was decoloured 1～3 hour, filters, and collects filtrate; Described impurity treatment agent is hydrated barta or bariumchloride;
(4) distillation concentrates: above-mentioned filtrate is changed in the encloses container of vacuum-pumping, vacuum distillation, keeping distillation vacuum tightness is 0.06-0.09MPa, when material liquid volume to be steamed is the 70-80% of former filtrate volume, stops distillation, concentrated solution;
(5) crystallization: above-mentioned concentrated solution is cooled to below 35 ℃, have a large amount of solid matters slowly crystallization separate out, filter, obtain crude product;
(6) washing and drying: above-mentioned crude product is not less than 95% washing with alcohol with purity, and the volume ratio of ethanol and crude product is 1: 1.5-3.0; Wash three times, centrifugal or suction filtration gets solids component, and oven dry obtains product then.
2. the preparation method of plant-sourced glucosamine hydrochloride according to claim 1 is characterized in that: temperature rises to 60～85 ℃, insulation reaction 6-10 hour in the step (1).
3. the preparation method of plant-sourced glucosamine hydrochloride according to claim 1 is characterized in that: temperature rises to 60～80 ℃ in the step (3).
4. according to the preparation method of claim 1 or 3 described plant-sourced glucosamine hydrochlorides, it is characterized in that: the amount that adds the impurity treatment agent in the step (3) is 0.1%～0.5% of a filtrate weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2009100196336A CN101503433B (en) | 2009-03-06 | 2009-03-06 | Preparation of plant source glucosamine hydrochloride |
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| CN2009100196336A CN101503433B (en) | 2009-03-06 | 2009-03-06 | Preparation of plant source glucosamine hydrochloride |
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| CN101503433B true CN101503433B (en) | 2010-09-01 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101628921B (en) * | 2009-07-30 | 2012-05-09 | 扬州日兴生物科技股份有限公司 | Preparation method of plant source D-glucosamine hydrochloride |
| CN102167713B (en) * | 2010-08-02 | 2013-08-21 | 南通市外贸医药保健品有限公司 | Preparation method of D-Glucosamine Hydrochloride |
| CN102408458A (en) * | 2010-09-26 | 2012-04-11 | 南通市外贸医药保健品有限公司 | Production process for refining glucosamine hydrochloride through membrane separation |
| CN102464679A (en) * | 2010-11-04 | 2012-05-23 | 江苏江山制药有限公司 | Production process for preparing high-purity D-glucosamine hydrochloride from citric acid fermentation residues |
| CN102633844B (en) * | 2012-04-15 | 2014-06-25 | 耿福能 | Method for preparing D-glucosamine hydrochloride by taking periplaneta americana as raw material |
| CN103319547B (en) * | 2013-04-10 | 2015-07-01 | 扬州日兴生物科技股份有限公司 | Preparation method for glucosamine hydrochloride |
| CN103360432A (en) * | 2013-07-10 | 2013-10-23 | 东台市天元化工有限公司 | Production method for glucosamine hydrochloride |
| CN103450289A (en) * | 2013-08-27 | 2013-12-18 | 上海应用技术学院 | Preparation method of D-glucosamine hydrochloride |
| CN109504723A (en) * | 2018-11-20 | 2019-03-22 | 扬州日兴生物科技股份有限公司 | A kind of ammonia sugar preparation method based on bioconversion fermentations |
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