CN108855007A - A kind of preparation method of black-koji mould filament-chitosan - Google Patents
A kind of preparation method of black-koji mould filament-chitosan Download PDFInfo
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- CN108855007A CN108855007A CN201810733157.3A CN201810733157A CN108855007A CN 108855007 A CN108855007 A CN 108855007A CN 201810733157 A CN201810733157 A CN 201810733157A CN 108855007 A CN108855007 A CN 108855007A
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- chitosan
- black
- koji mould
- preparation
- solution
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
- B01J20/267—Cross-linked polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4868—Cells, spores, bacteria
Abstract
The present invention provides a kind of preparation method of black-koji mould filament-chitosan, belongs to chitin modified technical field, which includes following preparation step：1) chitosan and glacial acetic acid aqueous solution are heated and is stirred evenly, form chitosan mixed solution；2) chitosan mixed solution and epoxychloropropane are formed into complex colloid after mixing；3) by the complex colloid in step 2), continue heating reaction；4) the black-koji mould filament after pulverizing and sieving is added into step 3), is handed over.5) sodium tripolyphosphate solution is added toward the mixed solution of step 4), the rear agitating and heating that continues is fixed.6) solution in step 5) is filtered, takes filter residue, vacuum drying is ground, and is saved backup.Obtain black-koji mould filament-chitosan.Preparation method simple process and low cost of the invention.
Description
Technical field
The present invention relates to chitin modified technical fields, more particularly to a kind of preparation of black-koji mould filament-chitosan
Method.
Background technique
Chitosan is the edibility animal origin of the uniquely alkaline kation containing free amine group in nature, is a kind of
It is fit similar to six carbon polies of fiber, there is the following characteristic：Biodegradability：Chitosan can be slowly catalyzed by biological enzyme
It is hydrolyzed to oligosaccharide, long-term place can hydrolyze in water, glucose ring open loop；Biocompatibility：Chitosan in vivo may be used
Lower-molecular substance is generated by lysozyme hydrolysis, to be absorbed by the body；Chelating：The ortho position of chitosan free amine group is hydroxyl,
There is chelating metal ion, is high performance metallic ion trapping agent；Enzyme immobilization effect：The free amine group of chitosan,
It can be used as the fixation support of the physiological activators such as enzyme, antigen, antibody；Hygroscopicity：The hydroscopicity of chitin is at most reachable
400%~500%, it is cellulose more than twice, the hygroscopicity of chitosan is more stronger than chitin；Antibiotic property：To various bacteria and
The growth of fungi has apparent inhibiting effect, and (Liu Xiaofei etc., the progress of Natural Chitosan/Viscoce Rayon with Antimicrobial Activity are changed
Work progress, 1999, (1)：32-34).Allan etc. just made systematic research to the antibiotic property of chitosan early in 1979, he mentions
Chitosan is gone out with broad spectrum antibacterial since chitosan has good physics, chemistry and biological property, intramolecular contains ammonia
Base and hydroxyl, it is good to organic solvent stability, be easy secondary operation, make chitosan weaving, printing and dyeing, papermaking, food, medicine,
Environmental protection, water process, heavy metal recovery etc., the broad application prospect with unique.
Aspergillus niger (Aspergillus niger) is common in some by-products in the fields such as fermentation industry and food processing
Object can survive extensively in the natural environment, and the black-koji mould filament stabilization from a wealth of sources of industrial waste and cheap,
The functional groups such as amino, carboxyl and hydroxyl are contained on surface, are a kind of economic and environment-friendly efficient biological adsorption agents.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to and a kind of preparation method of mycelium-chitosan is provided,
The preparation method in acid condition, is crosslinked chitosan and black-koji mould filament, is prepared into composite efficient adsorbent,
Greatly save the cost improves adsorption efficiency, and preparation process is environmentally protective, meets the requirement of modernization green production.
The present invention solves the above problems by the following technical programs：
A kind of preparation method of black-koji mould filament-chitosan, includes the following steps：
Step 1：By chitosan:0.5g-3g is dissolved in the glacial acetic acid aqueous solution of 25mL-150mL 2%, solution is heated
And stir evenly, form chitosan solution；
Step 2：Epoxychloropropane 2mL-4mL is added to chitosan solution, forms complex colloid after mixing；
Step 3：Complex colloid in step 2 is stirred 4h-6h and carry out heating reaction in 20 DEG C of -40 DEG C of conditions；
Step 4：The black-koji mould filament 0.5g-1.5g after pulverizing and sieving is added into step 3, is crosslinked 20min-40min；
Step 5：50mL2.5% (g/L) sodium tripolyphosphate solution is added in mixed solution toward step 4, under the conditions of 40 DEG C,
Fixed 9.0h；
Step 6：Solution in step 5 is filtered, filter residue is taken, 60 DEG C of vacuum dryings grind, save backup, that is, make
Obtain black-koji mould filament-chitosan.
The step 1 be specially：The chitosan for being 90%-99.9% by 0.5-5g deacetylation, stirring are sufficiently dissolved
Form chitosan mixed solution.
In the step 1 be specially：Chitosan is not soluble in water, need to be dissolved in the glacial acetic acid aqueous solution of 50mL2%.
Black-koji mould filament is 1g in the step 4, and the ratio with chitosan need to be 1:1, it is crosslinked 30min.
Sodium tripolyphosphate is 50ml in the step 5.
Chitosan is 1g in the step 1, and glacial acetic acid aqueous solution is 50ml.
Epoxychloropropane 3mL in the step 2.
Temperature condition in the step 3 is 30 DEG C, mixing time 5h.
The volume ratio of chitosan and acetic acid mixed solution is 1 in the step 1：50.
The step 4 is specially：Black-koji mould filament is sufficiently crushed, after 60 DEG C of drying, black-koji mould filament is in temperature
For in 50 DEG C of -55 DEG C of addition steps 3.
Advantages of the present invention is with effect：
Black-koji mould filament-chitosan composite adsorbent prepared by the present invention remains original amino, and does not have
Additional group is added, waste utilization can be accomplished to discarded mycelium, materials are greatly reduced, anhydrous in whole preparation process,
Addition without catalyst, preparation process is environmentally protective, meets the requirement of modernization green production, and at low cost, has good
Application prospect.
Specific embodiment
The invention will be further described with reference to embodiments.
A kind of preparation method of black-koji mould filament-chitosan, includes the following steps：
1) it by chitosan 1g, is dissolved in the glacial acetic acid aqueous solution of 50mL 2%, solution is heated and stirred evenly, form shell
Glycan solution.The volume ratio of chitosan and acetic acid mixed solution is 1：50.The chitosan for being 90%-99.9% by 1g deacetylation
It crushes, is reused after 50 DEG C of drying.
2) epoxychloropropane 3mL is added to chitosan solution, forms complex colloid after mixing.
3) complex colloid in step 2) is stirred 5h and carries out heating reaction in 30 DEG C of conditions.
4) the black-koji mould filament 1g after pulverizing and sieving is added into step 3), is crosslinked 30min.Black-koji mould filament is filled
Divide and crush, after 60 DEG C of drying, is added in step 3) while hot.
5) 50mL2.5% (g/L) sodium tripolyphosphate solution is added toward the mixed solution of step 4), under the conditions of 40 DEG C, Gu
Determine 9.0h.
6) solution in step 5) is filtered, takes filter residue, 60 DEG C of vacuum dryings grind, save backup.It obtains black
Aspergillus filament-chitosan.
The preferred embodiment of the present invention has been described in detail above, but the present invention is not limited to embodiment,
Those skilled in the art can also make on the premise of not violating the inventive spirit of the present invention various equivalent modification or
Replacement, these equivalent variation or replacement are all contained in scope of the present application.
Claims (10)
1. a kind of preparation method of black-koji mould filament-chitosan, it is characterised in that：Include the following steps：
Step 1：By chitosan:0.5g-3g, is dissolved in the glacial acetic acid aqueous solution of 25mL-150mL 2%, and solution is heated and stirred
It mixes uniformly, forms chitosan solution；
Step 2：Epoxychloropropane 2mL-4mL is added to chitosan solution, forms complex colloid after mixing；
Step 3：Complex colloid in step 2 is stirred 4h-6h and carry out heating reaction in 20 DEG C of -40 DEG C of conditions；
Step 4：The black-koji mould filament 0.5g-1.5g after pulverizing and sieving is added into step 3, is crosslinked 20min-40min；
Step 5：50mL2.5% (g/L) sodium tripolyphosphate solution is added in mixed solution toward step 4, fixed under the conditions of 40 DEG C
9.0h；
Step 6：Solution in step 5 is filtered, filter residue is taken, 60 DEG C of vacuum dryings grind, save backup, obtain black
Aspergillus filament-chitosan.
2. a kind of preparation method of black-koji mould filament-chitosan according to claim 1, it is characterised in that：The step
Rapid 1 be specially：The chitosan for being 90%-99.9% by 0.5-5g deacetylation, stirring, sufficiently dissolution form chitosan mixing
Solution.
3. a kind of preparation method of black-koji mould filament-chitosan according to claim 1, it is characterised in that：The step
In rapid 1 be specially：Chitosan is not soluble in water, need to be dissolved in the glacial acetic acid aqueous solution of 50mL2%.
4. a kind of preparation method of black-koji mould filament-chitosan according to claim 1, it is characterised in that：The step
Black-koji mould filament is 1g in rapid 4, and the ratio with chitosan need to be 1:1, it is crosslinked 30min.
5. a kind of preparation method of black-koji mould filament-chitosan according to claim 1, it is characterised in that：The step
Sodium tripolyphosphate is 50ml in rapid 5.
6. a kind of preparation method of black-koji mould filament-chitosan according to claim 1, it is characterised in that：The step
Chitosan is 1g in rapid 1, and glacial acetic acid aqueous solution is 50ml.
7. a kind of preparation method of black-koji mould filament-chitosan according to claim 1, it is characterised in that：The step
Epoxychloropropane 3mL in rapid 2.
8. a kind of preparation method of black-koji mould filament-chitosan according to claim 1, it is characterised in that：The step
Temperature condition in rapid 3 is 30 DEG C, mixing time 5h.
9. a kind of preparation method of black-koji mould filament-chitosan according to claim 1, it is characterised in that：The step
The volume ratio of chitosan and acetic acid mixed solution is 1 in rapid 1：50.
10. a kind of preparation method of black-koji mould filament-chitosan according to claim 1, it is characterised in that：The step
Rapid 4 are specially：Black-koji mould filament is sufficiently crushed, after 60 DEG C of drying, black-koji mould filament is 50 DEG C of -55 DEG C of additions in temperature
In step 3.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810733157.3A CN108855007A (en) | 2018-07-06 | 2018-07-06 | A kind of preparation method of black-koji mould filament-chitosan |
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| CN201810733157.3A CN108855007A (en) | 2018-07-06 | 2018-07-06 | A kind of preparation method of black-koji mould filament-chitosan |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401590A (en) * | 2002-09-26 | 2003-03-12 | 北京化工大学 | Mycelium surface coated biologic adsorbent and preparing process thereof |
| CN106190918A (en) * | 2016-07-28 | 2016-12-07 | 江苏科技大学 | One strain vesicle shortwave Zymomonas mobilis and the application in preparation immobilized microorganism adsorbent thereof |
| JP2017047136A (en) * | 2015-09-04 | 2017-03-09 | 株式会社スギノマシン | Environment cleaning agent, environment cleaning method, and production method for environment cleaning agent |
-
2018
- 2018-07-06 CN CN201810733157.3A patent/CN108855007A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401590A (en) * | 2002-09-26 | 2003-03-12 | 北京化工大学 | Mycelium surface coated biologic adsorbent and preparing process thereof |
| JP2017047136A (en) * | 2015-09-04 | 2017-03-09 | 株式会社スギノマシン | Environment cleaning agent, environment cleaning method, and production method for environment cleaning agent |
| CN106190918A (en) * | 2016-07-28 | 2016-12-07 | 江苏科技大学 | One strain vesicle shortwave Zymomonas mobilis and the application in preparation immobilized microorganism adsorbent thereof |
Non-Patent Citations (3)
| Title |
|---|
| 朱灵峰等: "《应用化学专业实验》", 31 August 2012, 哈尔滨：哈尔滨工业大学出版社 * |
| 李永峰等: "《环境生物技术：典型厌氧环境微生物过程》", 31 August 2014, 哈尔滨：哈尔滨工业大学出版社 * |
| 李琛: "天然有机吸附剂在重金属废水处理中的应用", 《化工技术与开发》 * |
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Application publication date: 20181123 |