CN109504723A - A kind of ammonia sugar preparation method based on bioconversion fermentations - Google Patents

A kind of ammonia sugar preparation method based on bioconversion fermentations Download PDF

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Publication number
CN109504723A
CN109504723A CN201811381061.1A CN201811381061A CN109504723A CN 109504723 A CN109504723 A CN 109504723A CN 201811381061 A CN201811381061 A CN 201811381061A CN 109504723 A CN109504723 A CN 109504723A
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China
Prior art keywords
acid
ammonia sugar
method based
kilograms
filtrate
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CN201811381061.1A
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Chinese (zh)
Inventor
丁振中
李会
雷鹏
曾哲灵
邓红兵
张超
平立凤
高小燕
徐俊山
方祥
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YANGZHOU RIXING BIO-TECH Co Ltd
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YANGZHOU RIXING BIO-TECH Co Ltd
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Priority to CN201811381061.1A priority Critical patent/CN109504723A/en
Publication of CN109504723A publication Critical patent/CN109504723A/en
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    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/02Monosaccharides

Abstract

The ammonia sugar preparation method based on bioconversion fermentations that the invention discloses a kind of, includes the following steps;The first step, acidolysis: in the closed acid-resistant container with agitating device, first put into the waste residue generated during 800 to 1000 kilograms of fermentation method production citric acids, add 900-1200 kilograms of hydrochloric acid that mass concentration is 30%-38%, stirring is opened, temperature rises to 75-95 degree, and insulation reaction 12-15 hours, second step, cooling and filters pressing: by the feed liquid cooling down after above-mentioned reaction to l degrees Celsius or less, crystallization is precipitated from feed liquid, filters, obtains crude product.The ammonia sugar preparation method based on bioconversion fermentations, it is used to prepare ammonia sugar using citric acid waste residues, it avoids tradition and prepares ammonia sugar bring chitin using crust substance, the risk for reducing sufferer allergy can simultaneously be effectively inhibits primary and secondary bone and joint diseases, slow down the abrasion of articulating joint surface cartilage by plant source ammonia sugar, hyperplasia, inhibition of pain.

Description

A kind of ammonia sugar preparation method based on bioconversion fermentations
Technical field
The present invention relates to ammonia sugar preparation technical field, specially a kind of ammonia sugar preparation method based on bioconversion fermentations.
Background technique
Ammonia sugar is the compound after a hydroxyl of glucose is replaced by amino, belongs to monosaccharide composition, can be used for arthrosis The treatment of illness, bone and joint diseases mainly influence cartilage, and cartilage is the smooth tissue in intra-articular covering bone end, healthy Cartilage enables bone mutually to slide, and reduces movement bring impact force;People with Osteoarthritis cartilage top layer rupture and Consume, this makes the bone rubs mutually below cartilage, and this friction can cause pain, swelling and range of motion to subtract Small, joint may deform at any time, and joint margins can grow sliding thorn, the bone of the die crack floated in articular cavity and soft Bone can lead to more pain and damage, and ammonia sugar largely can expedite the emergence of and supplement knuckle synovia for human body, so that constantly lubrication is closed Cartilage surface is saved, abrasion is reduced, makes joint part nimbly and freely.
The preparation of existing ammonia sugar is extracted from crab shrimp shell, and Glucosamine Sulphate and aminoglucose hydrochloride are divided into Two kinds, because crab shrimp shell will appear chitin during the preparation process, acidic materials are then added in chitin, reheat reflux point Solution is prepared into Glucosamine Sulphate and aminoguanidine hydrochloride grape, for the people of some marine product allergy, is prepared out Glucosamine Sulphate and aminoguanidine hydrochloride grape in the part chitin that has can still generate great harm, practicability compared with Difference.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the ammonia sugar preparation method based on bioconversion fermentations that the present invention provides a kind of, solution Still remaining chitin in existing ammonia sugar preparation process of having determined, the problem of greatly defining the ammonia sugar scope of application.
(2) technical solution
To achieve the above object, the invention provides the following technical scheme: a kind of ammonia sugar preparation based on bioconversion fermentations Method includes the following steps;
The first step, acidolysis:
In the closed acid-resistant container with agitating device, first puts into 800 to 1000 kilograms of fermentation methods and produce citric acid The waste residue generated in the process adds 900-1200 kilograms of hydrochloric acid that mass concentration is 30%-38%, opens stirring, temperature liter To 75-95 degree, insulation reaction 12-15 hours;
Second step, cooling and filters pressing:
By the feed liquid cooling down after above-mentioned reaction to l degrees Celsius hereinafter, crystallization is precipitated from feed liquid, filtering is obtained slightly Product transfers them in another acid-resistant container, and 1200-1500 kilograms of deionized water is added, heats under stirring conditions, Dissolve crude product, then filters pressing;
Third step, decoloration:
Filtrate after above-mentioned filters pressing is transferred in the acid-resistant container with stirring, impurity treatment agent is added, opens stirring, temperature 70-90 degrees Celsius is risen to, then heat preservation decoloration 2 to 3 hours filters, collects filtrate;
4th step, distillation and concentration:
Above-mentioned filtrate is transferred in the closed container of vacuum-pumping, vacuum distillation, keeping distillation vacuum degree is 0.06- 0.09MPa stops distillation, obtains concentrate when steaming the 70-80% that material liquid volume is former filtrate volume;
5th step, crystallization:
Above-mentioned concentrate is cooled to 35 degrees Celsius hereinafter, there is a large amount of solid matter slowly to crystallize precipitation, filtering obtains Crude product;
6th step, washing and drying:
The volume ratio of ethanol washing by above-mentioned crude product with purity not less than 95%, ethyl alcohol and crude product is 1:1.5-3.0, is washed It washs three times, is centrifuged or filters and to obtain solid component, then drying obtains product.
Optionally, impurity treatment agent is barium hydroxide or barium chloride in the third step, and the amount of the impurity treatment agent is The 0.1%-0.5% of filtrate weight.
Optionally, resistance to sour solvent is acid and alkali-resistance glassed steel reaction vessels in the first step, and acid and alkali-resistance glassed steel reaction vessels are By the glass containing high silicon dioxide, serve as a contrast the inner surface in steel vessel, through high temperature sintering securely adherence on metal surface As composite product.
Optionally, it is the glass lined container of acid and alkali-resistance that acid-resistant container, which is inner wall, in the second step, the second step and the Acid-resistant container in three steps is two identical containers.
(3) beneficial effect
The ammonia sugar preparation method based on bioconversion fermentations that the present invention provides a kind of, have it is following the utility model has the advantages that
(1) it is somebody's turn to do the ammonia sugar preparation method based on bioconversion fermentations, is used to prepare ammonia sugar using citric acid waste residues, avoids Tradition prepares ammonia sugar bring chitin using crust substance, and the risk for reducing sufferer allergy can simultaneously be effectively inhibits Primary and secondary bone and joint diseases slow down the abrasion of articulating joint surface cartilage, hyperplasia, inhibition of pain by plant source ammonia sugar.
(2) it is somebody's turn to do the ammonia sugar preparation method based on bioconversion fermentations, the raw materials used in the present invention produces lemon from fermentation method Waste residue during lemon acid, resourceful, heavy metal, antibiotic content will not be exceeded, cheap and easy to get, effectively reducing life While producing cost, suitable processing approach is had found for environmental contaminants, is turned waste into wealth, also save and curb environmental pollution Expense, simple production process is easy, and product quality is secure, there is preferable market prospects.
Specific embodiment
Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without making creative work The every other embodiment obtained, shall fall within the protection scope of the present invention.
The present invention provides a kind of technical solution: a kind of ammonia sugar preparation method based on bioconversion fermentations, including following step Suddenly;
The first step, acidolysis:
In the closed acid-resistant container with agitating device, first puts into 800 to 1000 kilograms of fermentation methods and produce citric acid The waste residue generated in the process adds 900-1200 kilograms of hydrochloric acid that mass concentration is 30%-38%, opens stirring, temperature liter To 75-95 degree, insulation reaction 12-15 hours, resistance to sour solvent was acid and alkali-resistance glassed steel reaction vessels, acid and alkali-resistance enamel in the first step Reaction kettle is the glass that will contain high silicon dioxide, serve as a contrast steel vessel inner surface, through high temperature sintering securely adherence in gold Become composite product on metal surface;
Second step, cooling and filters pressing:
By the feed liquid cooling down after above-mentioned reaction to l degrees Celsius hereinafter, crystallization is precipitated from feed liquid, filtering is obtained slightly Product transfers them in another acid-resistant container, and 1200-1500 kilograms of deionized water is added, heats under stirring conditions, Dissolve crude product, then filters pressing, it is the glass lined container of acid and alkali-resistance that acid-resistant container, which is inner wall, in second step, the second step with Acid-resistant container in third step is two identical containers;
Third step, decoloration:
Filtrate after above-mentioned filters pressing is transferred in the acid-resistant container with stirring, impurity treatment agent is added, opens stirring, temperature 70-90 degrees Celsius is risen to, then heat preservation decoloration 2 to 3 hours filters, collects filtrate, impurity treatment agent is hydroxide in third step Barium or barium chloride, the amount of the impurity treatment agent are the 0.1%-0.5% of filtrate weight;
4th step, distillation and concentration:
Above-mentioned filtrate is transferred in the closed container of vacuum-pumping, vacuum distillation, keeping distillation vacuum degree is 0.06- 0.09MPa stops distillation, obtains concentrate when steaming the 70-80% that material liquid volume is former filtrate volume;
5th step, crystallization:
Above-mentioned concentrate is cooled to 35 degrees Celsius hereinafter, there is a large amount of solid matter slowly to crystallize precipitation, filtering obtains Crude product;
6th step, washing and drying:
The volume ratio of ethanol washing by above-mentioned crude product with purity not less than 95%, ethyl alcohol and crude product is 1:1.5-3.0, is washed It washs three times, is centrifuged or filters and to obtain solid component, then drying obtains product.
Embodiment 1:
A kind of ammonia sugar preparation method based on bioconversion fermentations, includes the following steps;
The first step, acidolysis:
In the closed acid-resistant container with agitating device, first puts into 800 to 1000 kilograms of fermentation methods and produce citric acid The waste residue generated in the process adds 900-1200 kilograms of hydrochloric acid that mass concentration is 30%-38%, opens stirring, temperature liter To 75-95 degree, insulation reaction 8-10 hours;
Second step, cooling and filters pressing:
By the feed liquid cooling down after above-mentioned reaction to l degrees Celsius hereinafter, crystallization is precipitated from feed liquid, filtering is obtained slightly Product transfers them in another acid-resistant container, and 1200-1500 kilograms of deionized water is added, heats under stirring conditions, Dissolve crude product, then filters pressing;
Third step, decoloration:
Filtrate after above-mentioned filters pressing is transferred in the acid-resistant container with stirring, impurity treatment agent is added, opens stirring, temperature 70-90 degrees Celsius is risen to, then heat preservation decoloration 2 to 3 hours filters, collects filtrate;
4th step, distillation and concentration:
Above-mentioned filtrate is transferred in the closed container of vacuum-pumping, vacuum distillation, keeping distillation vacuum degree is 0.06- 0.09MPa stops distillation, obtains concentrate when steaming the 70-80% that material liquid volume is former filtrate volume;
5th step, crystallization:
Above-mentioned concentrate is cooled to 35 degrees Celsius hereinafter, there is a large amount of solid matter slowly to crystallize precipitation, filtering obtains Crude product;
6th step, washing and drying:
The volume ratio of ethanol washing by above-mentioned crude product with purity not less than 95%, ethyl alcohol and crude product is 1:1.5-3.0, is washed It washs three times, is centrifuged or filters and to obtain solid component, then drying obtains product.
Embodiment 2:
A kind of ammonia sugar preparation method based on bioconversion fermentations, includes the following steps;
The first step, acidolysis:
In the closed acid-resistant container with agitating device, first puts into 800 to 1000 kilograms of fermentation methods and produce citric acid The waste residue generated in the process adds 900-1200 kilograms of hydrochloric acid that mass concentration is 20%-30%, opens stirring, temperature liter To 75-95 degree, insulation reaction 12-15 hours;
Second step, cooling and filters pressing:
By the feed liquid cooling down after above-mentioned reaction to l degrees Celsius hereinafter, crystallization is precipitated from feed liquid, filtering is obtained slightly Product transfers them in another acid-resistant container, and 1200-1500 kilograms of deionized water is added, heats under stirring conditions, Dissolve crude product, then filters pressing;
Third step, decoloration:
Filtrate after above-mentioned filters pressing is transferred in the acid-resistant container with stirring, impurity treatment agent is added, opens stirring, temperature 70-90 degrees Celsius is risen to, then heat preservation decoloration 2 to 3 hours filters, collects filtrate;
4th step, distillation and concentration:
Above-mentioned filtrate is transferred in the closed container of vacuum-pumping, vacuum distillation, keeping distillation vacuum degree is 0.06- 0.09MPa stops distillation, obtains concentrate when steaming the 70-80% that material liquid volume is former filtrate volume;
5th step, crystallization:
Above-mentioned concentrate is cooled to 35 degrees Celsius hereinafter, there is a large amount of solid matter slowly to crystallize precipitation, filtering obtains Crude product;
6th step, washing and drying:
The volume ratio of ethanol washing by above-mentioned crude product with purity not less than 95%, ethyl alcohol and crude product is 1:1.5-3.0, is washed It washs three times, is centrifuged or filters and to obtain solid component, then drying obtains product.
Embodiment 3:
A kind of ammonia sugar preparation method based on bioconversion fermentations, includes the following steps;
The first step, acidolysis:
In the closed acid-resistant container with agitating device, first puts into 800 to 1000 kilograms of fermentation methods and produce citric acid The waste residue generated in the process adds 900-1200 kilograms of hydrochloric acid that mass concentration is 30%-38%, opens stirring, temperature liter To 75-95 degree, insulation reaction 12-15 hours;
Second step, cooling and filters pressing:
By the feed liquid cooling down after above-mentioned reaction to l degrees Celsius hereinafter, crystallization is precipitated from feed liquid, filtering is obtained slightly Product transfers them in another acid-resistant container, and 1200-1500 kilograms of deionized water is added, heats under stirring conditions, Dissolve crude product, then filters pressing;
Third step, decoloration:
Filtrate after above-mentioned filters pressing is transferred in the acid-resistant container with stirring, impurity treatment agent is added, opens stirring, temperature 70-90 degrees Celsius is risen to, then heat preservation decoloration 1 to 2 hours filters, collects filtrate;
4th step, distillation and concentration:
Above-mentioned filtrate is transferred in the closed container of vacuum-pumping, vacuum distillation, keeping distillation vacuum degree is 0.06- 0.09MPa stops distillation, obtains concentrate when steaming the 70-80% that material liquid volume is former filtrate volume;
5th step, crystallization:
Above-mentioned concentrate is cooled to 35 degrees Celsius hereinafter, there is a large amount of solid matter slowly to crystallize precipitation, filtering obtains Crude product;
6th step, washing and drying:
The volume ratio of ethanol washing by above-mentioned crude product with purity not less than 95%, ethyl alcohol and crude product is 1:1.5-3.0, is washed It washs three times, is centrifuged or filters and to obtain solid component, then drying obtains product.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment Intrinsic element.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding And modification, the scope of the present invention is defined by the appended.

Claims (4)

1. a kind of ammonia sugar preparation method based on bioconversion fermentations, it is characterised in that: include the following steps;
The first step, acidolysis:
In the closed acid-resistant container with agitating device, first puts into 800 to 1000 kilograms of fermentation methods and produce citric acid process The waste residue of middle generation adds 900-1200 kilograms of hydrochloric acid that mass concentration is 30%-38%, opens stirring, and temperature rises to 75- 95 degree, insulation reaction 12-15 hours;
Second step, cooling and filters pressing:
By the feed liquid cooling down after above-mentioned reaction to l degrees Celsius hereinafter, crystallization is precipitated from feed liquid, filtering obtains crude product, It transfers them in another acid-resistant container, 1200-1500 kilograms of deionized water is added, heats under stirring conditions, make thick Product dissolution, then filters pressing;
Third step, decoloration:
Filtrate after above-mentioned filters pressing is transferred in the acid-resistant container with stirring, impurity treatment agent is added, opens stirring, temperature rises to 70-90 degrees Celsius, then heat preservation decoloration 2 to 3 hours filters, collects filtrate;
4th step, distillation and concentration:
Above-mentioned filtrate is transferred in the closed container of vacuum-pumping, vacuum distillation, keeping distillation vacuum degree is 0.06-0.09MPa, When steaming the 70-80% that material liquid volume is former filtrate volume, stops distillation, obtain concentrate;
5th step, crystallization:
Above-mentioned concentrate is cooled to 35 degrees Celsius hereinafter, there is a large amount of solid matter slowly to crystallize precipitation, filtering obtains thick Product;
6th step, washing and drying:
The volume ratio of ethanol washing by above-mentioned crude product with purity not less than 95%, ethyl alcohol and crude product is 1:1.5-3.0, washing three It is secondary, it is centrifuged or filters and to obtain solid component, then drying obtains product.
2. a kind of ammonia sugar preparation method based on bioconversion fermentations according to claim 1, it is characterised in that: described Impurity treatment agent is barium hydroxide or barium chloride in three steps, and the amount of the impurity treatment agent is the 0.1%-0.5% of filtrate weight.
3. a kind of ammonia sugar preparation method based on bioconversion fermentations according to claim 1, it is characterised in that: described Resistance to sour solvent is acid and alkali-resistance glassed steel reaction vessels in one step, and acid and alkali-resistance glassed steel reaction vessels are the glass that will contain high silicon dioxide, Serve as a contrast steel vessel inner surface, through high temperature sintering securely adherence on metal surface become composite product.
4. a kind of ammonia sugar preparation method based on bioconversion fermentations according to claim 1, it is characterised in that: described It is the glass lined container of acid and alkali-resistance that acid-resistant container, which is inner wall, in two steps, and the acid-resistant container in the second step and third step is two Identical container.
CN201811381061.1A 2018-11-20 2018-11-20 A kind of ammonia sugar preparation method based on bioconversion fermentations Pending CN109504723A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101429221A (en) * 2008-12-19 2009-05-13 王纪杰 Method for producing D-glucosamine hydrochlorate
CN101503433A (en) * 2009-03-06 2009-08-12 石勇 Preparation of plant source glucosamine hydrochloride
CN101628921A (en) * 2009-07-30 2010-01-20 扬州日兴生物科技股份有限公司 Preparation method of plant source D-glucosamine hydrochloride

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101429221A (en) * 2008-12-19 2009-05-13 王纪杰 Method for producing D-glucosamine hydrochlorate
CN101503433A (en) * 2009-03-06 2009-08-12 石勇 Preparation of plant source glucosamine hydrochloride
CN101628921A (en) * 2009-07-30 2010-01-20 扬州日兴生物科技股份有限公司 Preparation method of plant source D-glucosamine hydrochloride

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Application publication date: 20190322