CN103360432A - Production method for glucosamine hydrochloride - Google Patents
Production method for glucosamine hydrochloride Download PDFInfo
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- CN103360432A CN103360432A CN2013102883584A CN201310288358A CN103360432A CN 103360432 A CN103360432 A CN 103360432A CN 2013102883584 A CN2013102883584 A CN 2013102883584A CN 201310288358 A CN201310288358 A CN 201310288358A CN 103360432 A CN103360432 A CN 103360432A
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Abstract
The invention discloses a production method for glucosamine hydrochloride. The production method comprises the following steps of: loading, namely loading citric acid residue or chitin in a reactor after carrying out rough filtration on the citric acid residue or chitin with the water content of 30-80%; aeration, namely continuously aerating hydrogen chloride from the bottom of the reactor; gelatinization, namely continually stifling and swelling the chitin or the citric acid residue by the hydrogen chloride so as to form paste; hydrolysis, namely heating the paste in a hydrolysis kettle to 70-90 DEG C under the normal pressure, and maintaining the temperature for 2-4 hours, so as to obtain a glucosamine hydrochloride crude product; carrying out decoloration, filtration, crystallization, cleaning and drying, so as to prepare a glucosamine hydrochloride finished product. According to the preparation method for the glucosamine hydrochloride, the hydrogen chloride is directly utilized to stifle and swell the raw materials, during the stifling and swelling process, the reaction materials are preheated and are simultaneously combined with water to generate hydrochloric acid, and the generated hydrochloric acid is throughout in a saturation state; the method has the advantages that not only can the process be reasonable, the cost is lowered, but also the production efficiency is high, and the quality is stable.
Description
Technical field
The present invention relates to a kind of method for manufacturing of glucosamine hydrochloride, relate in particular to a kind of method that adopts chitin or citric acid waste to produce glucosamine hydrochloride.
Background technology
D-Glucosamine Hydrochloride (D-Glucosamine Hydrochloride, GAH) has another name called the grape amine hydrochlorate, formal name used at school is D-Glucosamine Hydrochloride, and molecular formula is: C6H13NO5HCl, molecular weight 215.63, CAS number: 66-84-2, structural formula is:
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 knuckle synovia, improve metabolism of articular cartilage, effectively therefore treatment rheumatic arthritis be called by the world of medicine " agent of OA amelioration of disease ".Can be used as diabetic subject's nutritious subsidy agent.A large amount of uses are harmless to health.Amino acid glucose and derivative have a wide range of applications in fields such as medical science, light industry, makeup.Pharmaceutically, as antibacterial-anti-inflammatory drug, be used for the treatment of rheumatism joint inflammation and treatment gastric ulcer, if use with microbiotic, can promote the absorption of microbiotic in blood, but reducing the simultaneously also growth of anticancer of side reaction, is the main raw material of synthesizing new anticarcinogen NSC-178248.In food, be a kind of important micro-carbohydrate content that add in the infant formulas Ruzhong, or the starting raw material of synthetic VB6 and riboflavin intermediate, can be applicable to again in addition in makeup and the fodder additives, purposes is very extensive, and demand all increases day by day both at home and abroad.
The raw material that adopts in the present industrial glucosamine hydrochloride production mainly is chitin oven dry material, the oven dry material of using citric acid waste is also arranged, its water ratio all need be controlled at below 10%, therefore no matter be chitin oven dry material, or citric acid waste oven dry material all will be with special drying plant, and in drying course, inhomogeneous owing to bake out temperature, effective constituent a large amount of in the raw material is destroyed, even forfeiture; The simultaneously oven dry of material also can produce the oven dry cost.
Another main raw material of producing glucosamine hydrochloride is concentrated hydrochloric acid, for concentration and the quality that guarantees concentrated hydrochloric acid, its concentrated hydrochloric acid is to be absorbed by specific equipments such as film-falling absorption towers by hydrogenchloride to prepare, owing in absorbing preparation process, will add the raw materials such as water, can cause the unstable of concentration of hydrochloric acid and purity, thereby affect the quality of the finished product; Simultaneously also can produce preparation cost.
When glucosamine hydrochloride is produced, be will oven dry chitin or citric acid waste put into reaction vessel with whipping appts, making dry chitin or citric acid waste be immersed in concentrated hydrochloric acid reacts and makes the glucosamine hydrochloride crude product, the glucosamine hydrochloride crude product after the postprocessing working procedures such as cleaning, filtration, crystallization, oven dry are refining, obtains the glucosamine hydrochloride finished product again.The deficiency that existing this production technique exists is: whole production process is gap operating, and production efficiency is low; The concentration of hydrochloric acid of reaction process is unstable, and along with the carrying out of reaction, the concentration of hydrochloric acid is constantly successively decreased, and concentration of hydrochloric acid is lower, hydrolysis reaction more is difficult to carry out, and reaction time is longer, does not reach desirable reaction effect, also be unfavorable for the crystallization of product, production efficiency is low, and product yield is low.
Summary of the invention
Technical problem to be solved by this invention provides a kind of production method of glucosamine hydrochloride, and not only technique is reasonable for the method, cost, and production efficiency is high, steady quality.
In order to solve the problems of the technologies described above, the production method of glucosamine hydrochloride of the present invention, this production method comprises the steps:
(1) charging: be that 30 ~ 80% citric acid waste or chitin carry out the coarse filtration impurity elimination to water ratio, make citric acid waste or chitin material group maximum particle diameter less than 10cm, the citric acid waste after coarse filtration or chitin are packed in the reactor;
(2) air inlet: pass into continuously hydrogen chloride gas from reactor bottom, the temperature in the reactor is controlled at 30 ~ 80 ℃;
(3) gelatinization: hydrogen chloride gas is constantly fumigated swelling and is formed mashed prod chitin or citric acid waste, will change hydrolysis kettle over to from chitin or the acid mashed prod of citric acid waste of reactor overflow mouth outflow swelling, and the temperature of mashed prod is controlled at 30 ~ 80 ℃;
(4) hydrolysis: under normal pressure, the mashed prod in the hydrolysis kettle is heated to 70 ~ 90 ℃, is incubated 2 ~ 4 hours, obtain the glucosamine hydrochloride crude product;
(5) decolouring: change the glucosamine hydrochloride crude product over to the vacuum concentration still, successively add successively again pure water and gac in the vacuum concentration still, keep temperature 60 C ~ 80 ℃ 1 ~ 2 hour to obtain the crude product that decolours; The add-on of pure water is glucosamine hydrochloride crude product quality 5-10 times, and the input amount of gac is glucosamine hydrochloride crude product quality 0.01% ~ 0.02%, and this gac fineness is 100 ~ 200 orders;
(6) filter: make glucosamine hydrochloride filtrate with filter-cloth filtering decolouring crude product, the order number of filter cloth is 60 ~ 300 orders;
(7) crystallization: with filter cloth filter glucosamine hydrochloride filtrate be transferred to and carry out vacuum extraction in the crystallization kettle and obtain the glucosamine hydrochloride crystallisate, Tc is controlled at 70 ℃-80 ℃;
(8) cleaning-drying: drop into whizzer after the glucosamine hydrochloride crystallisate is cooled to normal temperature, in whizzer, add dehydrated alcohol again, flood after 0.5 ~ 1 hour centrifuge dehydration and make glucosamine hydrochloride and clean crystallisate; Glucosamine hydrochloride is cleaned crystallisate to be dropped into vacuum dryer and dries and obtain the glucosamine hydrochloride finished product; Its bake out temperature is controlled at 60 ~ 70 ℃, dries 0.5 ~ 1.5 hour.
Vacuum tightness 0.08 ~ the 0.1MPa of described reactor upper space.
Described hydrogen chloride gas passes in the reactor by gas distributor.
Mashed prod in the described hydrolysis kettle is heated to 75 ~ 85 ℃, is incubated 2 ~ 3 hours, obtains the glucosamine hydrochloride crude product
Described filter cloth adopts the three stacked filter clothes that add, and its first layer filter cloth order number is 201 ~ 300 orders, and second layer filter cloth order number is 101 ~ 200 orders, and the 3rd metafiltration cloth order number is 60 ~ 100 orders.
In whizzer, add dehydrated alcohol, dipping, centrifuge dehydration, this process triplicate.
Method for producing aminoglucose hydrochloride of the present invention compared with prior art has following advantage:
1, the present invention directly adopts the chitin of high-moisture percentage or citric acid by product citric acid waste as raw material, do not need through pre-treatment such as super-dries, thereby the drying processes such as centrifugal, oven dry have been reduced, not only reasonable whole technological process, reduced production cost Shrink short citric acid waste cycle of processing, improved the processing efficiency of citric acid waste; And this processing method avoided the high temperature of drying process to damage and the energy consumption of effective constituent, also avoided the environmental pollution that brings in the preprocessing process.
2, another raw material of the present invention directly adopts hydrogen chloride gas, and hydrogen chloride gas is the byproduct of chlorination reaction process in numerous chlorization products productions, do not need it is done special processing, directly hydrogen chloride gas is passed in the reactor and do not make pretreated moisture chitin or citric acid waste hybrid reaction, both removed by-product hydrogen chloride gas from through the tail gas absorbing system cooling, separate, the steps such as absorption generate the complex processes such as hydrochloric acid, shortened again the vent gas treatment time of chloralkane or other chlorination reaction, also reduced energy consumption, rationally technological process, reduced production cost.
3, the advantage that the present invention gives prominence to is that also the swelling that it directly adopts hydrogen chloride gas to participate in chitin or citric acid waste is hydrolyzed, hydrogen chloride gas is the process to the reaction mass preheating in the process that passes into chitin or citric acid waste, it also is the process that generates hydrochloric acid of being combined with moisture content, the concentration of hydrochloric acid that generates is in state of saturation all the time, hydrogen chloride gas also produces a large amount of heats in dissolution process, reaction mass is played preferably heat effect, at a certain temperature, make chitin or the continuous swelling of citric acid waste of continuous suction form mashed prod, along with increasing of mashed prod, mashed prod can flow out continuously from the reactor overflow mouth, mashed prod flows into hydrolysis kettle, generate the glucosamine hydrochloride crude product, crude product is through decolouring, filter, crystallization, the last handling processes such as cleaning-drying generate the glucosamine hydrochloride finished product.The method is remaining the high density that hydrochloric acid is stable, has effectively guaranteed the stable of quality of item, and the technological process of optimizing has simultaneously guaranteed again the raising of production efficiency effectively.
4, the present invention has changed and has added the technique that concentrated hydrochloric acid and preheating can be used in the traditional technology, directly pass in chitin or the citric acid waste, generate continuously mashed prod (chitin or citric acid waste swelling thing), the traditional technology Raw is dried respectively, absorbed, and then both merge three gap technological processs of carrying out respectively that heat swelling, be merged into a continuous operation, operation is simplified, Gong Qi Shrink is short, work efficiency improves, production cycle shortens greatly, production efficiency promotes greatly, the products obtained therefrom excellent performance, the product yield is between 3 ~ 10%.It is short that material after swelling, Shui are separated Shi Jian Shrink, only 1.5 ~ 4 hours times spent.Do not use noxious solvent in the production process simultaneously, guarantee the cleaning of production process, residual without hazardous and noxious substances in the product, final product quality is excellent.
5, raw material sources of the present invention are extensive, and cost is low, simple and reliable process, main raw material is easy to get, and all supports the use its byproduct with adjacent enterprise, is a last ring of industrial chain, production importance is high, has greatly improved economic benefit and the social benefit of whole industrial chain.
Embodiment
Embodiment 1:
Take chitin as raw material, at first chitin raw material is carried out coarse filtration and removal impurity wherein, the water ratio of chitin raw material (per-cent that the quality of water accounts in the raw material total mass in the raw material) is controlled between the 30%-80%, maximum particle diameter is controlled in 10 cm, to keep efficient and the yield of reaction.In the continuous tower-type mixing reactor of 4 meters of virtual heights, utilize vacuum to suck above-mentioned through the pretreated chitin of coarse filtration removal of impurities, such as water ratio 50%, the particle diameter chitin less than 8cm; Vacuum tightness 0.08 ~ the 0.1MPa of reactor upper space, the bed depth in the reactor exceed 4 meters or when being lower than 1.5 meters, material loading vacuum intake system automatically stops or automatically starting.The hydrogen chloride gas distribution apparatus that arranges from continuous tower-type mixing reactor bottom continuously passes into hydrogen chloride gas, start simultaneously temperature elevation system and program, this temperature elevation system adopts heat riser commonly used, material temperature is controlled at 30 ~ 80 ℃, be preferably 50 ~ 60 ℃, keep this temperature swelling after 30 minutes, flow out continuously mashed prod from the above 1 meter reactor overflow mouth in continous way tower mixing reactor bottom, this mashed prod enters insulation storage in the mashed prod storage tank continuously through U-shaped pipeline, and the mashed prod temperature is controlled at 50 ~ 60 ℃.Take out from storage tank in the hydrolysis kettle of 500kg mashed prod input 1000L under normal pressure, this hydrolysis kettle is enamel reaction still, is heated to 78 ± 2 ℃, is incubated 2.5 hours, generates the glucosamine hydrochloride crude product.
The glucosamine hydrochloride crude product is changed in the vacuum concentration still, 60 ℃ ± 2 ℃ insulations 1.5 hours, vacuum drawn sour gas wherein, and fully absorbed by tail gas absorbing system; Add 300kg pure water dissolving glucosamine hydrochloride crude product, rear adding 5g gac makes the decolouring crude product again, and the gac fineness is 200 orders.Then above-mentioned decolouring crude product solution is made glucosamine hydrochloride filtrate through Filter Press, filter cloth is formed by 300 orders, 150 orders and 80 orders, three metafiltration cloth stack combinations.Glucosamine hydrochloride filtrate through bed filtration, be transferred in the crystallization kettle and carry out vacuum extraction at 78 ± 2 ℃, when the mass crystallization thing occurring, stop Heat preservation, after crystallisate is cooled to normal temperature, the glucosamine hydrochloride crystallisate is dropped into whizzer, centrifuge filtering cloth is combined by 200 orders and 400 orders, two metafiltration cloth, in whizzer, add 100 liters of dehydrated alcohols, flooded 0.5 hour, centrifugal, the overlapping investment dehydrated alcohol, dipping and centrifugation step three times make glucosamine hydrochloride through three times centrifuge dehydrations and clean crystallisate, after glucosamine hydrochloride is cleaned crystallisate change vacuum dryer over to and dry, bake out temperature is controlled at 68 ℃ ± 2 ℃, dries after 1 hour, obtains 39kg glucosamine hydrochloride finished product.
Embodiment 2:
Take citric acid waste as raw material, at first the citric acid waste raw material is carried out coarse filtration and removal impurity wherein, the moisture control of citric acid waste raw material is between 30%-80%, and maximum particle diameter is controlled in 10 cm.In the tower mixing reactor of continous way of 4 meters of virtual heights, utilize vacuum to suck not pretreated citric acid waste (water ratio 40%, particle diameter is less than 10cm), bed depth reaches 4 meters or when being lower than 1.5 meters, material loading automatically stops or automatically starting.The hydrogenchloride distribution apparatus that arranges from the tower mixing reactor of continous way bottom passes into hydrogen chloride gas, start simultaneously heating schedule, material temperature is controlled at 50 ~ 60 ℃, keep this temperature swelling after 30 minutes, flow out continuously mashed prod from the above 1 meter overflow port in continous way tower mixing reactor bottom, mashed prod enters insulation storage in the mashed prod storage tank continuously through U-shaped pipeline, and the mashed prod temperature control is at 50 ~ 60 ℃.Under normal pressure, from the mashed prod storage tank, take out the 500kg mashed prod and drop in the 1000L enamel reaction still, be heated to 78 ± 2 ℃, be incubated 2 hours, generate the glucosamine hydrochloride crude product.
The glucosamine hydrochloride crude product is changed in the vacuum concentration still, insulation is at 60 ℃ ± 2 ℃, vacuum drawn sour gas wherein, and fully absorbed by tail gas absorbing system, add again 300kg pure water dissolving glucosamine hydrochloride crude product, rear adding 10g gac makes the decolouring crude product, and the gac fineness is 100 orders.Then the crude product solution of should decolouring is through Filter Press, filter cloth is by 80 orders, 150 orders and 300 order filter clothes combine, filtrate through bed filtration, be transferred in the crystallization kettle and carry out vacuum extraction at 78 ± 2 ℃, when the mass crystallization thing occurring, stopped heating, after the glucosamine hydrochloride crystallisate is cooled to normal temperature, it is dropped into whizzer, centrifuge filtering cloth is combined by 200 orders and 400 orders, two metafiltration cloth, adds 100 liters of dehydrated alcohols in whizzer, floods 0.5 hour, centrifugal, the overlapping investment dehydrated alcohol, dipping and centrifugation step three times, after glucosamine hydrochloride crystallisate input vacuum dryer is dried, bake out temperature is controlled at 68 ℃ ± 2 ℃, dry after 1 hour, obtain 36kg glucosamine hydrochloride finished product.
Claims (6)
1. the production method of a glucosamine hydrochloride, it is characterized in that: this production method comprises the steps: (1) charging: be that 30～80% citric acid waste or chitin carry out the coarse filtration impurity elimination to water ratio, make citric acid waste or chitin material group maximum particle diameter less than 10cm, the citric acid waste after coarse filtration or chitin are packed in the reactor; (2) air inlet: pass into continuously hydrogen chloride gas from reactor bottom, the temperature in the reactor is controlled at 30～80 ℃; (3) gelatinization: hydrogen chloride gas is constantly fumigated swelling and is formed mashed prod chitin or citric acid waste, will change hydrolysis kettle over to from chitin or the acid mashed prod of citric acid waste of reactor overflow mouth outflow swelling, and the temperature of mashed prod is controlled at 30～80 ℃; (4) hydrolysis: under normal pressure, the mashed prod in the hydrolysis kettle is heated to 70～90 ℃, is incubated 2～4 hours, obtain the glucosamine hydrochloride crude product; (5) decolouring: change the glucosamine hydrochloride crude product over to the vacuum concentration still, successively add successively again pure water and gac in the vacuum concentration still, keep temperature 60 C～80 ℃ 1～2 hour to obtain the crude product that decolours; The add-on of pure water is glucosamine hydrochloride crude product quality 5-10 times, and the input amount of gac is glucosamine hydrochloride crude product quality 0.01%～0.02%, and this gac fineness is 100～200 orders; (6) filter: make glucosamine hydrochloride filtrate with filter-cloth filtering decolouring crude product, the order number of filter cloth is 60～300 orders; (7) crystallization: with filter cloth filter glucosamine hydrochloride filtrate be transferred to and carry out vacuum extraction in the crystallization kettle and obtain the glucosamine hydrochloride crystallisate, Tc is controlled at 70 ℃～80 ℃; (8) cleaning-drying: drop into whizzer after the glucosamine hydrochloride crystallisate is cooled to normal temperature, in whizzer, add dehydrated alcohol again, flood after 0.5～1 hour centrifuge dehydration and make glucosamine hydrochloride and clean crystallisate; Glucosamine hydrochloride is cleaned crystallisate to be dropped into vacuum dryer and dries and obtain the glucosamine hydrochloride finished product; Its bake out temperature is controlled at 60～70 ℃, dries 0.5～1.5 hour.
2. the production method of glucosamine hydrochloride according to claim 1 is characterized in that: the vacuum tightness 0.08～0.1MPa of described reactor upper space.
3. the production method of glucosamine hydrochloride according to claim 1, it is characterized in that: described hydrogen chloride gas passes in the reactor by gas distributor.
4. the production method of glucosamine hydrochloride according to claim 1, it is characterized in that: the mashed prod in the described hydrolysis kettle is heated to 75～85 ℃, is incubated 2～3 hours, obtains the glucosamine hydrochloride crude product.
5. the production method of glucosamine hydrochloride according to claim 1, it is characterized in that: described filter cloth adopts the three stacked filter clothes that add, its the first layer filter cloth order number is 60～100 orders, and second layer filter cloth order number is 101～200 orders, and the 3rd metafiltration cloth order number is 201～300 orders.
6. the production method of glucosamine hydrochloride according to claim 1 is characterized in that: add dehydrated alcohol, dipping, centrifuge dehydration in whizzer, this process triplicate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111606957A (en) * | 2020-07-01 | 2020-09-01 | 山东润德生物科技有限公司 | Process and device for producing and decoloring glucosamine hydrochloride |
| CN112851724A (en) * | 2021-02-20 | 2021-05-28 | 江苏澳新生物工程有限公司 | Preparation method of vegetarian D-glucosamine hydrochloride |
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| CN111606957A (en) * | 2020-07-01 | 2020-09-01 | 山东润德生物科技有限公司 | Process and device for producing and decoloring glucosamine hydrochloride |
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Application publication date: 20131023 |