CN101274948A - D-aminoglucose and preparation thereof - Google Patents
D-aminoglucose and preparation thereof Download PDFInfo
- Publication number
- CN101274948A CN101274948A CNA200810016202XA CN200810016202A CN101274948A CN 101274948 A CN101274948 A CN 101274948A CN A200810016202X A CNA200810016202X A CN A200810016202XA CN 200810016202 A CN200810016202 A CN 200810016202A CN 101274948 A CN101274948 A CN 101274948A
- Authority
- CN
- China
- Prior art keywords
- glucosamine
- ion exchange
- exchange column
- ion
- high level
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention discloses a D-aminoglucose and a preparation method thereof, which can solve problems caused by acidity existing in the prior art. The method adopts the technical proposal that an ion exchange method is adopted to remove HCl in the hydrochloride molecular structure of the D-aminoglucose; the molecular structure formula of the D-aminoglucose is showed as the lower right formula. The product of the invention can replace the D-aminoglucose hydrochloride in the current market, does not pollute earth, realizes sustainable development in agriculture without pollution, poison and side effect, resists falling over, can increase crop output and has wider application.
Description
Technical field
The present invention relates to biological technical field, relate in particular to the D-glucosamine and the preparation method of chitin series.
Background technology
The D-glucosamine hydrochloride is arranged in the market as the raw material of chemosynthesis or be directly used in crop production.But owing to contain hydrochloric acid in the molecular structure, be acid, use to have limitation, in particular for the agriculture production aspect, the meeting contaminated soil is difficult to widespread use.
How solving the problem that prior art exists, then is the design problem that the present invention faces.
Summary of the invention
The invention provides a kind of D-glucosamine and preparation method, it can solve the acid problem of being brought of being of prior art existence.
In order to reach the purpose that solves the problems of the technologies described above, technical scheme of the present invention is,
A kind of D-glucosamine is characterized in that described D-glucosamine molecular structural formula is
In technique scheme of the present invention, also have following technical characterictic: described D-glucosamine exchange principle is as follows:
In the formula: R-OH is a D301 weakly alkaline anionic polystyrene exchange resin,
In technique scheme of the present invention, also have following technical characterictic: described D301 weakly alkaline anionic polystyrene exchange resin can be used U.S.'s product grade: Amberlite IRA-93/94 or DOWexMWA-1 replace.
A kind of method for preparing described D-glucosamine is characterized in that described method adopts preparation equipment, and its step is as follows:
1. smart the filtration: adopt the D-glucosamine hydrochloride, the solution that is made into 10～15% concentration with distilled water filters to remove impurity through plate-and-frame filter press;
2. ion-exchange: the solution after the filtration is squeezed into the stock liquid high level tank with pump, the D301 weakly alkaline anionic polystyrene exchange resin ion exchange column I in the described equipment that packs into, be that 1: 1.3～1.8 ratio pours into water in ion exchange column I according to the mass ratio of anionite-exchange resin and water then, the stock liquid high level tank of D-glucosamine hydrochloride solution from described equipment flows into the work in-process flow container after entering described ion exchange column I, the mass ratio of described anionite-exchange resin and D-glucosamine hydrochloride is 1: 0.6～0.8, and ion-exchange time is 20～30 minutes;
3. freeze concentration: with the solution freeze concentration in the described work in-process flow container to concentration is 8～10%, and freezing temp is-2 ℃～-8 ℃, removes ice cube, takes out spissated D-glucosamine.
In technique scheme of the present invention, also has following technical characterictic: after the raw material in the described stock liquid high level tank flows out from described ion exchange column I, after continuing to enter ion exchange column II, III and carrying out ion-exchange, flow into the work in-process flow container again.
In technique scheme of the present invention, also have following technical characterictic: the ion-exchange time among described ion exchange column II, the III is 20～30 minutes.
In technique scheme of the present invention, also have following technical characterictic: in D-glucosamine concentration described in the freeze concentration step is 8～10%.
In technique scheme of the present invention, also have following technical characterictic: the filter cloth in the described plate-and-frame filter press is a flannelette, and the order number is 200～300 orders.
In technique scheme of the present invention, also have following technical characterictic: the lower end of described ion exchange column I, II, III is provided with 150～300 purpose bolting silks.
The present invention has the following advantages and positively effect:
The product that employing the present invention produces is the acid ion that removes in the D-glucosamine hydrochloride, and only remaining amino, it is central better than present employed D-glucosamine hydrochloride to be used for agriculture production, nontoxic, have no side effect, and can contaminated soil, Sustainable development on agricultural.Also anti-volt falls, and can increase crop yield, and purposes is very extensive.
The increasing production of rice test
Be San Lian village, You Kou township, Nanchang County, Nanchang City, Jiangxi Province one of experimental field; Experimental field two are Yi Du villages, Liu Hu township, Xinjian County, Nanchang City, Jiangxi Province.Practice ground is in land for growing field crops central authorities and marks 0.07 hectare, so that unified management.
Test method all adopts seed soaking to germinate: be made into 10% DAS 400ml earlier, and on-the-spot then towards rare 100 times.20 kilograms of seed rice, identical with the used seed rice in land for growing field crops, be immersed in the solution, broadcast sowing in the rice seedling bed after the germination in 3-4 days.Seed-soaking liquid 1/4 after one week is uniformly unreasonable like a shrew in the rice seedling bed, and all the other seed-soaking liquids of 3/4 were sprayed on the blade face later in the rice growth in land for growing field crops in one month.All the other operations are all identical as rice transplanting, fertilising, weeding, irrigation etc. in addition.
Test-results: the preceding employing of harvesting is won each 100 ancient unit of weight, equal to 1/24 liang (arbitrarily respectively win 100 strains equably from Tanaka respectively by the peasant, threshing is dried) arbitrarily and is compared, and the result is as follows:
The dry weight of the 100 strain rice experimental field in San Lian village, You Kou township is 546 grams, and big Tanaka 100 strain rice are 475 grams, and both compare volume increase 15%.
The dry weight of the 100 strain rice in Yi Du village, Liu Hu township, Xinjian County is 510 grams, and big Tanaka 100 strain rice are 450 grams, and both compare volume increase 13.3%.
Description of drawings
Fig. 1 is that D-glucosamine of the present invention prepares apparatus embodiments 1 synoptic diagram;
Fig. 2 is that D-glucosamine of the present invention prepares apparatus embodiments 2 synoptic diagram;
1. stock liquid high level tank; 2. distilled water high level tank; 3.NaOH solution high level tank; 4. emptying valve; 5, ion exchange column; 5-1. ion exchange column I; 5-2. ion exchange column II; 5-3. ion exchange column III; 6. Stainless Steel Valve; 7. work in-process flow container; 8. treatment tank; 9. pipeline.
Embodiment
Gordian technique scheme of the present invention is that the employing ion exchange method is removed the HCL in the molecular structure, and its exchange principle is as follows:
In the formula: R-OH is a D301 weakly alkaline anionic polystyrene exchange resin, and the product grade that this product is corresponding with the U.S. is: Amberlite IRA-93/94; DOWexMWA-1.
R-OH also can adopt 717 strongly basic anion exchange resins in addition.
Referring to Fig. 1, D-glucosamine prepares device systems figure, ion exchange column 5 high 200cm, and diameter is 30cm, the lower end is provided with 200 purpose bolting silks.D-glucosamine prepares equipment and comprises ion exchange column 5, stock liquid high level tank 1, distilled water high level tank 2, NaOH solution high level tank 3, Stainless Steel Valve 6, work in-process flow container 7, treatment tank 8.Be connected with valve by pipeline 9 between ion exchange column 5 and stock liquid high level tank 1, distilled water high level tank 2, NaOH solution high level tank 3, work in-process flow container 7, the treatment tank 8.Wherein all valves are the stainless steel check valve.
Concrete ion-exchange step is as follows:
Load 100kg D301 weakly alkaline anionic polystyrene exchange resin in the ion exchange column 5, reinjecting adds 150 premium on currency, and water covers resin;
The solution that 80kg D-glucosamine hydrochloride is made into 12% concentration with distilled water filters to remove impurity through plate-and-frame filter press;
Solution after the filtration is squeezed into stock liquid high level tank 1 with pump, then by stock liquid high level tank 1 through stainless valve V
1Flow in the ion exchange column 5, D301 weakly alkaline anionic polystyrene exchange resin and D-glucosamine hydrochloride carry out ion-exchange in ion exchange column 5, and the flow velocity of controlled liq finishes through exchange in 20～30 minutes;
Resin regeneration
In order to make that resin can recycle, make resin regeneration with the resin reaction after NaOH solution and the exchange.
Close V
1, treat the stock liquid emptying in the ion exchange column 5 after, close V
8, open V
2-0, V
3-1, open V simultaneously
4Valve makes it directly logical atmosphere, and the water in the distilled water high level tank 2 injects ion exchange column 5 automatically, closes V
2-0, V
3-1Valve static 30 minutes, is opened V then
7, washing lotion is entered work in-process flow container 7.
Open V then
3-0And V
3-1, this moment V
8Close, regenerated liquid is a NaOH solution, flows into ion exchange column I from NaOH solution high level tank 3 immediately.When treating that NaOH solution did not have resin 5cm above, close V
3-0Static 30 minutes, open V
8, regenerated liquid flows in the treatment tank 8, evacuated ion exchange column I.
Close V then
8, open V
2-0, with the regenerated liquid of the distilled water wash ion exchange column 5 in the distilled water high level tank 2.When water to be distilled did not have resin 5cm above, close V
2-0, open V after 10 minutes
8, the washing water among the evacuated ion exchange column I are with V
8Effusive washing water do not become stream to be as the criterion.
Close V then
8, open V
2-0, when water to be distilled did not have resin 5cm above, close V
2-0, open V after 10 minutes
8, the emptying washing water.Detect washing water quality simultaneously, pH value should be between 7.0-7.5, otherwise washes once again.
And then carry out the exchange operations process again.
Referring to Fig. 2, D-glucosamine prepares device systems figure, in order to obtain the purity high product, adopts three ion exchange columns to carry out ion-exchange.The all high 200cm of ion exchange column I, II, III, diameter is 25cm, the lower end is provided with 250 purpose bolting silks.
D-glucosamine prepares equipment and comprises ion exchange column I5-1, ion exchange column II5-2 and ion exchange column III5-3, also comprises stock liquid high level tank 1, distilled water high level tank 2, NaOH solution high level tank 3, emptying valve 4, Stainless Steel Valve 6, work in-process flow container 7, treatment tank 8.Be connected with valve by pipeline 9 between ion exchange column I, II, III and stock liquid high level tank 1, distilled water high level tank 2, NaOH solution high level tank 3, work in-process flow container 7, the treatment tank 8.Wherein the emptying valve 4 of the upper end of ion exchange column connection is a 3-way valve, and what all the other positions connected is the stainless steel check valve.
Concrete ion-exchange step is as follows:
Load 100kg D301 weakly alkaline anionic polystyrene exchange resin among ion exchange column I5-1, ion exchange column II5-2 and the ion exchange column III5-3 respectively, add 150 premium on currency more respectively in each ion exchange column, water covers resin;
The solution that the 80kgD-glucosamine hydrochloride is made into 12% concentration with distilled water filters to remove impurity through plate-and-frame filter press;
Solution after the filtration is squeezed into stock liquid high level tank 1 with pump, then by stock liquid high level tank 1 through stainless valve V
1-1Flow among the ion exchange column I5-1, D301 weakly alkaline anionic polystyrene exchange resin and D-glucosamine hydrochloride carry out ion-exchange in ion exchange column I5-1, and the flow velocity of controlled liq finishes through exchange in 20～30 minutes;
For further carrying out ion-exchange, feed liquid enters among ion exchange column II5-2 and the ion exchange column III5-3 after exchanging from ion exchange column I5-1 and finishing again, opens stainless valve V this moment simultaneously
5-1 ', V
5-2, V
5-2 'And V
5-3, the open degree of by-pass valve control, be 20～30 minutes swap time, after V
7-3And V
7Flow in the work in-process flow container 7.This moment, all the other valves all were in closing condition.
Resin regeneration
The regeneration order is I, II, III circular order.In order to make that resin can recycle, make resin regeneration with the resin reaction after NaOH solution and the exchange.
Ion exchange column I regeneration:
Close V
1-1, at V
4-1Connect pressurized air (pressure is 0.025-0.03MPa) on the valve, treat to close V after the stock liquid emptying among the ion exchange column I5-1
5-1 'And V
5-2, open V
1-2, make ion exchange column II5-2 and ion exchange column III5-3 proceed ion-exchange.Then V
4-1T-valve is got to logical atmospheric condition.
Open V
2-0, V
3-1, the water in the distilled water high level tank 2 flows among the ion exchange column I5-1 automatically, closes V
2-0, static 30 minutes, open V then
7-1, washing lotion is entered work in-process flow container 7.
Close V
7-1, open V then
3-0And V
3-1, this moment V
8Close, regenerated liquid is a NaOH solution, flows into ion exchange column I from NaOH solution high level tank 3 immediately.When treating that NaOH solution did not have resin 5cm above, close V
3-0Static 30 minutes, open V
8, regenerated liquid flows in the treatment tank 8, evacuated ion exchange column I.
Close V then
8, open V
2-0, with the regenerated liquid of the water washing ion exchange column I in the distilled water high level tank 2.When water to be distilled did not have resin 5cm above, close V
2-0, open V after 10 minutes
8, the washing water among the evacuated ion exchange column I are with V
8Effusive washing water do not become stream to be as the criterion.
Close V then
8, open V
2-0, when water to be distilled did not have resin 5cm above, close V
2-0, open V after 10 minutes
8, the emptying washing water.Detect washing water quality simultaneously, pH value should be between 7.0-7.5, otherwise washes once again.
The access of regenerating resin:
Close V
7Valve is opened V
7-1Valve, solution among the ion exchange column III flows into ion exchange column I, when treating that liquid among the ion exchange column I did not have resin 5cm above, confirm the interior no bubble of ion exchange column I, closes V
7-3Valve.
Close V
4-1V left by valve
5-3 'And V
5-1V left simultaneously by valve
5-1 'And V
5-2Valve.Open V
7Valve normally carries out the exchange operations process.
Ion exchange column II, III regenerated principle are identical with ion exchange column I regenerative process.
The above only is preferred embodiment of the present invention, is not to be the restriction of the present invention being made other form, and any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the equivalent embodiment of equivalent variations.But every technical solution of the present invention content that do not break away to any simple modification, equivalent variations and remodeling that above embodiment did, still belongs to the protection domain of technical solution of the present invention according to technical spirit of the present invention.
Claims (9)
1. a D-glucosamine is characterized in that described D-glucosamine molecular structural formula is
2. D-glucosamine according to claim 1 is characterized in that described D-glucosamine exchange principle is as follows:
In the formula: R-OH is a D301 weakly alkaline anionic polystyrene exchange resin,
3. D-glucosamine according to claim 2 is characterized in that described D301 weakly alkaline anionic polystyrene exchange resin can use U.S.'s product grade: AmberliteIRA-93/94 or DOWexMWA-1 to replace.
4. a method for preparing the described D-glucosamine of claim 1 is characterized in that described method adopts preparation equipment, and its step is as follows:
1. smart the filtration: adopt the D-glucosamine hydrochloride, the solution that is made into 10～15% concentration with distilled water filters to remove impurity through plate-and-frame filter press;
2. ion-exchange: the solution after the filtration is squeezed into the stock liquid high level tank with pump, the D301 weakly alkaline anionic polystyrene exchange resin ion exchange column I in the described equipment that packs into, be that 1: 1.3～1.8 ratio pours into water in ion exchange column I according to the mass ratio of anionite-exchange resin and water then, the stock liquid high level tank of D-glucosamine hydrochloride solution from described equipment flows into the work in-process flow container after entering described ion exchange column I, the mass ratio of described anionite-exchange resin and D-glucosamine hydrochloride is 1: 0.6～0.8, and ion-exchange time is 20～30 minutes;
3. freeze concentration: with the solution freeze concentration in the described work in-process flow container to concentration is 8～10%, and freezing temp is-2 ℃～-8 ℃, removes ice cube, takes out spissated D-glucosamine.
5. according to the described method of claim 4, it is characterized in that raw material in the described stock liquid high level tank flows out from described ion exchange column I after, after continuing to enter ion exchange column II, III and carrying out ion-exchange, flow into the work in-process flow container again.
6. according to the described method of claim 5, it is characterized in that the ion-exchange time among described ion exchange column II, the III is 20～30 minutes.
7. according to the described method of claim 6, it is characterized in that in D-glucosamine concentration described in the freeze concentration step be 8～10%.
8. according to the described method of claim 4, it is characterized in that the filter cloth in the described plate-and-frame filter press is a flannelette, the order number is 200～300 orders.
9. according to claim 4 or 8 described methods, it is characterized in that the lower end of described ion exchange column I, II, III is provided with 150～300 purpose bolting silks.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810016202XA CN101274948A (en) | 2008-05-08 | 2008-05-08 | D-aminoglucose and preparation thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810016202XA CN101274948A (en) | 2008-05-08 | 2008-05-08 | D-aminoglucose and preparation thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101274948A true CN101274948A (en) | 2008-10-01 |
Family
ID=39994837
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA200810016202XA Pending CN101274948A (en) | 2008-05-08 | 2008-05-08 | D-aminoglucose and preparation thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101274948A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899071A (en) * | 2009-05-31 | 2010-12-01 | 欣凯医药化工中间体（上海）有限公司 | Method for preparing glucosamine monomer from glucosamine hydrochloride |
| CN103626809A (en) * | 2013-12-10 | 2014-03-12 | 安徽丰原发酵技术工程研究有限公司 | Method for purifying glucosamine hydrochloride mother liquid |
| CN104327263A (en) * | 2014-09-30 | 2015-02-04 | 严积芳 | Glucose resin preparation method |
-
2008
- 2008-05-08 CN CNA200810016202XA patent/CN101274948A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899071A (en) * | 2009-05-31 | 2010-12-01 | 欣凯医药化工中间体（上海）有限公司 | Method for preparing glucosamine monomer from glucosamine hydrochloride |
| CN103626809A (en) * | 2013-12-10 | 2014-03-12 | 安徽丰原发酵技术工程研究有限公司 | Method for purifying glucosamine hydrochloride mother liquid |
| CN103626809B (en) * | 2013-12-10 | 2016-01-20 | 安徽丰原发酵技术工程研究有限公司 | A kind of purification process of glucosamine hydrochloride mother liquid |
| CN104327263A (en) * | 2014-09-30 | 2015-02-04 | 严积芳 | Glucose resin preparation method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN204670029U (en) | A kind of saline land irrigation rig | |
| CN106305021A (en) | Method for treating desertification grassland | |
| CN105801259A (en) | Preparation method of liquid fertilizer for preventing and treating banana wilt | |
| CN101274948A (en) | D-aminoglucose and preparation thereof | |
| CN114667819B (en) | Improvement method for removing slurry of soda saline-alkali rice field and application thereof | |
| CN104628427A (en) | Preparation method of humic acid activator for organic fertilizer production | |
| CN105561943B (en) | A kind of preparation method and application of magnetic rape stalk sorbing material | |
| CN104996055A (en) | Plant nutritive water circulation use system | |
| CN107556141A (en) | A kind of soil conditioner and preparation method thereof | |
| CN106068732A (en) | A kind of contaminated land and alkaline land improving system and modification method | |
| CN209702352U (en) | A kind of integrated regulation device of industrialized agriculture liquid manure salt input | |
| CN205961804U (en) | Morning and evening tides formula irrigation system | |
| CN105379762B (en) | Cold-resistant agent for rice and its application of the Herba Equiseti Hiemalis extract as cold-resistant composition | |
| CN104150696A (en) | N and P recovery device and method in sewage | |
| CN104824621A (en) | Method for extracting low-potassium plant salts from sea asparagus planted in sulfate saline-alkali soil with medium-high alkalinity | |
| CN204860040U (en) | Plant nutrition water cyclic utilization system | |
| CN202035358U (en) | Drip irrigation header | |
| CN212064806U (en) | Beach saline and alkaline land soil improvement device | |
| CN108377773A (en) | A kind of grape cuttage cultivation Nutrition Soil and preparation method thereof | |
| CN108966846A (en) | Rice stubble wheatland rice straw ditch corruption returning to the field method and facility | |
| CN105418204A (en) | New applications of Rhizobium W33 strain | |
| US20140319060A1 (en) | Method for removing ammonium nitrogen from organic waste water | |
| CN211056982U (en) | Biogas slurry resource utilization system device | |
| CN106748236A (en) | A kind of Snakegourd Fruit foliar fertilizer | |
| CN109134117A (en) | A kind of high-activity humic acid fertilizer and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20081001 |