CN108160043A - A kind of preparation method of antibiont support type collagen fiber adsorption material - Google Patents
A kind of preparation method of antibiont support type collagen fiber adsorption material Download PDFInfo
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- CN108160043A CN108160043A CN201711363771.7A CN201711363771A CN108160043A CN 108160043 A CN108160043 A CN 108160043A CN 201711363771 A CN201711363771 A CN 201711363771A CN 108160043 A CN108160043 A CN 108160043A
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28059—Surface area, e.g. B.E.T specific surface area being less than 100 m2/g
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/28085—Pore diameter being more than 50 nm, i.e. macropores
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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
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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Abstract
The present invention relates to a kind of preparation methods of antibiont support type collagen fiber adsorption material, belong to sorbing material technical field.The present invention to Chinese prickly ash albumen by carrying out enzymolysis processing, extract antibacterial peptide, it is coated by antibacterial peptide to collagenous fibres surface, by antibacterial peptide under potassium peroxydisulfate hydrolysis, cross-linked graft and coating modification, load of the bacterium on collagenous fibres surface is effectively prevent by antibacterial peptide, improves the antibiont load performance of collagenous fibres;And the present invention hydrolyzed by potassium peroxydisulfate after form sulfonic acid group, collagenous fiber material surface is modified, enhance modified collagenous fibres degree of scatter, improve adsorption capacity of the sorbing material to adsorbate simultaneously, and make to form cross-linked network inside collagenous fibres, the absorption property of material is effectively improved by the cross-linked structure of formation, so as to effectively improve the absorption property of collagen-based materials.
Description
Technical field
The present invention relates to a kind of preparation methods of antibiont support type collagen fiber adsorption material, belong to sorbing material technology
Field.
Background technology
Collagenous fibres are the linear chain structure albumen of a kind of appearance white, transparent natural fiber, are largely present in lactation
The skin histology of class animal is tied in hoof tissue and bone tissue, and content accounts for about 25%~33% left side of animal vivo protein total amount
The right side is the most protein of animal in-vivo content, has very important effect to protection body, support organ.According to collagen
Fiber to the difference of animal body concrete function, can generally be classified as basement membrane collagen, non-dimension collagen, anchoring collagen, cross-film collagen,
Fento collagen, the netted collagen in six sides and collagenous fibres with other special roles etc..In α-peptide chain of collagenous fibres molecule
Containing a large amount of acid and alkaline amino acid residue, all there are carboxyl and amino in every peptide chain both ends, therefore collagenous fibres have
Certain isoelectric point is a kind of amphiprotic substance.In addition, also containing a large amount of-COOH ,-NH in collagenous fibres molecular side chain2、-
NH-CO- ,-OH isoreactivity group have very high chemism in aqueous solution, can be combined with water molecules hydrogen bond, hydrophilic insoluble
Yu Shui, in water in solvent swelling state, therefore the water absorbing capacity of collagenous fibres is very strong.In addition, peptide is existed simultaneously between collagenous fibres
Ionic bond, hydrogen bond, Van der Waals force, hydrophobic bond and intermolecular Aldehyde-ammonia Condensation, aldol condensation and aldehyde alcohol histidine between chain
The effects that power so that being completely embedded between tropocollagen molecule, the comprehensive strength for leading to collagenous fibres are higher.These knots of collagenous fibres
Structure feature determines the good characteristics such as its good mechanical strength and stronger biocompatibility, increasingly causes researcher's
Extensive concern.
Collagenous fibres are emerging with the research that its unique structure and biology performance increasingly cause absorption both at home and abroad to learn expert
Interest, and its application in Industrial Wastewater Treatment is also increasingly extensive, cannot be only used for the metal ions waste water such as Cr, Cu, Fe
Adsorption treatment, it may also be used for the substances such as the removing of tannin and Wastewater Dyes, enzyme, microorganism and protein in Chinese medicine preparation
Removal.In addition, pretreatment, chemistry are passed it through containing a large amount of collagenous fibres in the solid waste generated in leather making process
Industrial wastewater is handled as sorbing material after the processes such as modified, efficiently using for Leather Solid Waste can be not only realized, subtract
Few environmental pollution, and the processing cost of industrial wastewater can be also reduced, enhance economic benefit, there is higher researching value.But
Be existing collagenous fibres sorbent material due to being collagen-based materials, easily by microorganism and bacterial load, block absorption hole, lead
Sorbent material absorption property is caused to lower, absorption is invalid, so prepare a kind of sorbent material of effective antibiont load has very much
It is necessary.
Invention content
The technical problems to be solved by the invention:For Heat Conduction Material in use, long-time heat conduction processing makes it
The problem of changing with volume stability easily is expanded, provides a kind of preparation side of low expansion high heat conduction carbon composite
Method.
In order to solve the above technical problems, the technical solution adopted by the present invention is:
(1)It takes fresh Chinese prickly ash seed and crushes, dry Chinese prickly ash seed powder, in mass ratio 1:25, by Chinese prickly ash seed powder
It is stirred, is heated to reflux with ethylene glycol, standing is cooled to room temperature, and filters to obtain filter cake, in mass ratio 1:10, by filter cake and quality
A concentration of 10% hydrochloric acid solution is stirred, and is centrifuged and is collected lower sediment, washing, dry desiccation protein;
(2)In mass ratio 1:5, desiccation protein and deionized water are stirred, pH to 6.0~6.5 is adjusted, obtains mixed liquor, it will
Pepsin is added in mixed liquor, and after heat preservation enzymolysis, heating is boiled, and standing is cooled to room temperature, and obtains enzymolysis liquid;
(3)It takes pig bone and crushes, vacuum freeze drying must dry skeletal grain, in mass ratio 1:10, by dry skeletal grain and in mass ratio
1:10, dry skeletal grain is added in glacial acetic acid, heating water bath, after being rinsed 3~5 times with deionized water, vacuum freeze drying is simultaneously
Collagenous fibres must be dried;
(4)It counts in parts by weight, weighs 45~50 parts of enzymolysis liquids, 15~20 parts of dry collagenous fibres, 6~8 parts of persulfuric acid respectively
Potassium and 2~3 parts of glyoxalic acids are placed in three-necked flask, adjust pH to 7.0, and heating water bath, standing is cooled to room temperature and filter residue,
Washing, drying can be prepared into a kind of antibiont support type collagen fiber adsorption material.
Step(1)The temperature that is heated to reflux is 55~60 DEG C.
Step(2)The pepsin additive amount is 50U/g.
Step(4)The adjusting pH is using 5% sodium hydroxide of mass fraction.
Compared with other methods, advantageous effects are the present invention:
(1)The present invention extracts antibacterial peptide, is coated by antibacterial peptide to collagenous fibres table by carrying out enzymolysis processing to Chinese prickly ash albumen
Face, by antibacterial peptide under potassium peroxydisulfate hydrolysis, cross-linked graft and coating modification effectively prevent bacterium to exist by antibacterial peptide
The load on collagenous fibres surface improves the antibiont load performance of collagenous fibres;
(2)The present invention forms sulfonic acid group after being hydrolyzed by potassium peroxydisulfate, and collagenous fiber material surface is modified, makes modification
Collagenous fibres degree of scatter enhances afterwards, while improves adsorption capacity of the sorbing material to adsorbate, and makes shape inside collagenous fibres
Cross-linked structure is reticulated, the absorption property of material is effectively improved by the cross-linked structure of formation, so as to effectively improve collagen-based materials
Absorption property.
Specific embodiment
It takes fresh Chinese prickly ash seed and crushes, dry Chinese prickly ash seed powder, then in mass ratio 1:25, by Chinese prickly ash seed
Powder is stirred with ethylene glycol, and 4~5h is heated to reflux at 55~60 DEG C, and standing is cooled to room temperature, and filter cake is filtered to obtain, by matter
Measure ratio 1:10, filter cake is stirred, then the centrifugation point under 1200~1300r/min with mass concentration for 10% hydrochloric acid solution
From and collect lower sediment, be washed with distilled water 3~5 times, be dried in vacuo to obtain desiccation protein, then in mass ratio 1:5, by dry egg
It is stirred in vain with deionized water, with the salt acid for adjusting pH that mass concentration is 10% to 6.0~6.5, obtains mixed liquor, then press stomach egg
White enzyme additive amount 50U/g, pepsin is added in mixed liquor, and 3~5h of heat preservation enzymolysis, heats and boil 10 at 30~35 DEG C
~15min, standing are cooled to room temperature, and obtain enzymolysis liquid;It takes pig bone and crushes, vacuum freeze drying must dry skeletal grain, in mass ratio
1:10, by dry skeletal grain and in mass ratio 1:10, dry skeletal grain is added in glacial acetic acid, the heating water bath 2 at 45~50 DEG C
After~3h, and with after deionized water flushing 3~5 times, vacuum freeze drying simultaneously must dry collagenous fibres and count in parts by weight, point
It also known as measures 45~50 parts of enzymolysis liquids, 15~20 parts of dry collagenous fibres, 6~8 parts of potassium peroxydisulfates and 2~3 parts of glyoxalic acids and is placed in three
In mouth flask, pH to 7.0,2~3h of heating water bath at 75~80 DEG C are adjusted with 5% sodium hydroxide of mass fraction, stands cooling
To room temperature and filter residue, after being rinsed 3~5 times with deionized water, vacuum freeze drying can be prepared into a kind of antibiont load
Type collagen fiber sorbing material.
Example 1
It takes fresh Chinese prickly ash seed and crushes, dry Chinese prickly ash seed powder, then in mass ratio 1:25, by Chinese prickly ash seed powder
It is stirred with ethylene glycol, 4h is heated to reflux at 55 DEG C, standing is cooled to room temperature, and filters to obtain filter cake, in mass ratio 1:10, it will
Filter cake is stirred, then centrifuged under 1200r/min and collect lower sediment with the hydrochloric acid solution that mass concentration is 10%,
It is washed with distilled water 3 times, is dried in vacuo to obtain desiccation protein, then in mass ratio 1:5, desiccation protein and deionized water are stirred mixed
It closes, with the salt acid for adjusting pH that mass concentration is 10% to 6.0, mixed liquor is obtained, then by pepsin additive amount 50U/g, by stomach cardia
Enzyme is added in mixed liquor, and heat preservation enzymolysis 3h, heats and boil 10min, standing is cooled to room temperature, and obtains enzymolysis liquid at 30 DEG C;It takes
Pig bone simultaneously crushes, and vacuum freeze drying must dry skeletal grain, in mass ratio 1:10, by dry skeletal grain and in mass ratio 1:10, it will be dry
Dry skeletal grain be added to glacial acetic acid in, at 45 DEG C after heating water bath 2h, and with deionized water rinse 3 times after, vacuum freeze drying
And collagenous fibres must be dried and counted in parts by weight, 45 parts of enzymolysis liquids, 15 parts of dry collagenous fibres, 6 parts of persulfuric acid are weighed respectively
Potassium and 2 parts of glyoxalic acids are placed in three-necked flask, and pH to 7.0, the heating water bath at 75 DEG C are adjusted with 5% sodium hydroxide of mass fraction
2h, standing is cooled to room temperature and filter residue, and after being rinsed 3 times with deionized water, vacuum freeze drying can be prepared into a kind of anti-
Biological load type collagen fiber sorbing material.
Example 2
It takes fresh Chinese prickly ash seed and crushes, dry Chinese prickly ash seed powder, then in mass ratio 1:25, by Chinese prickly ash seed powder
It is stirred with ethylene glycol, 4h is heated to reflux at 57 DEG C, standing is cooled to room temperature, and filters to obtain filter cake, in mass ratio 1:10, it will
Filter cake is stirred, then centrifuged under 1250r/min and collect lower sediment with the hydrochloric acid solution that mass concentration is 10%,
It is washed with distilled water 4 times, is dried in vacuo to obtain desiccation protein, then in mass ratio 1:5, desiccation protein and deionized water are stirred mixed
It closes, with the salt acid for adjusting pH that mass concentration is 10% to 6.2, mixed liquor is obtained, then by pepsin additive amount 50U/g, by stomach cardia
Enzyme is added in mixed liquor, and heat preservation enzymolysis 4h, heats and boil 12min, standing is cooled to room temperature, and obtains enzymolysis liquid at 32 DEG C;It takes
Pig bone simultaneously crushes, and vacuum freeze drying must dry skeletal grain, in mass ratio 1:10, by dry skeletal grain and in mass ratio 1:10, it will be dry
Dry skeletal grain be added to glacial acetic acid in, at 47 DEG C after heating water bath 2h, and with deionized water rinse 4 times after, vacuum freeze drying
And collagenous fibres must be dried and counted in parts by weight, 47 parts of enzymolysis liquids, 17 parts of dry collagenous fibres, 7 parts of persulfuric acid are weighed respectively
Potassium and 2 parts of glyoxalic acids are placed in three-necked flask, and pH to 7.0, the heating water bath at 77 DEG C are adjusted with 5% sodium hydroxide of mass fraction
2h, standing is cooled to room temperature and filter residue, and after being rinsed 4 times with deionized water, vacuum freeze drying can be prepared into a kind of anti-
Biological load type collagen fiber sorbing material.
Example 3
It takes fresh Chinese prickly ash seed and crushes, dry Chinese prickly ash seed powder, then in mass ratio 1:25, by Chinese prickly ash seed powder
It is stirred with ethylene glycol, 5h is heated to reflux at 60 DEG C, standing is cooled to room temperature, and filters to obtain filter cake, in mass ratio 1:10, it will
Filter cake is stirred, then centrifuged under 1300r/min and collect lower sediment with the hydrochloric acid solution that mass concentration is 10%,
It is washed with distilled water 5 times, is dried in vacuo to obtain desiccation protein, then in mass ratio 1:5, desiccation protein and deionized water are stirred mixed
It closes, with the salt acid for adjusting pH that mass concentration is 10% to 6.5, mixed liquor is obtained, then by pepsin additive amount 50U/g, by stomach cardia
Enzyme is added in mixed liquor, and heat preservation enzymolysis 5h, heats and boil 12min, standing is cooled to room temperature, and obtains enzymolysis liquid at 35 DEG C;It takes
Pig bone simultaneously crushes, and vacuum freeze drying must dry skeletal grain, in mass ratio 1:10, by dry skeletal grain and in mass ratio 1:10, it will be dry
Dry skeletal grain be added to glacial acetic acid in, at 50 DEG C after heating water bath 3h, and with deionized water rinse 5 times after, vacuum freeze drying
And collagenous fibres must be dried and counted in parts by weight, 50 parts of enzymolysis liquids, 20 parts of dry collagenous fibres, 8 parts of persulfuric acid are weighed respectively
Potassium and 3 parts of glyoxalic acids are placed in three-necked flask, and pH to 7.0, the heating water bath at 80 DEG C are adjusted with 5% sodium hydroxide of mass fraction
3h, standing is cooled to room temperature and filter residue, and after being rinsed 5 times with deionized water, vacuum freeze drying can be prepared into a kind of anti-
Biological load type collagen fiber sorbing material.
Example 1,2,3 prepared by the present invention is tested for the property, minimal inhibitory concentration≤4mgAg/L.Simultaneously
For the present invention by repeated using still having higher antibacterial activity after 5 times to this sorbing material, specific surface area is reachable
5.6398m2/ g, average adsorption aperture position 152.
Claims (4)
1. a kind of preparation method of antibiont support type collagen fiber adsorption material, it is characterised in that specifically preparation process is:
(1)It takes fresh Chinese prickly ash seed and crushes, dry Chinese prickly ash seed powder, in mass ratio 1:25, by Chinese prickly ash seed powder
It is stirred, is heated to reflux with ethylene glycol, standing is cooled to room temperature, and filters to obtain filter cake, in mass ratio 1:10, by filter cake and quality
A concentration of 10% hydrochloric acid solution is stirred, and is centrifuged and is collected lower sediment, washing, dry desiccation protein;
(2)In mass ratio 1:5, desiccation protein and deionized water are stirred, pH to 6.0~6.5 is adjusted, obtains mixed liquor, it will
Pepsin is added in mixed liquor, and after heat preservation enzymolysis, heating is boiled, and standing is cooled to room temperature, and obtains enzymolysis liquid;
(3)It takes pig bone and crushes, vacuum freeze drying must dry skeletal grain, in mass ratio 1:10, by dry skeletal grain and in mass ratio
1:10, dry skeletal grain is added in glacial acetic acid, heating water bath, after being rinsed 3~5 times with deionized water, vacuum freeze drying is simultaneously
Collagenous fibres must be dried;
(4)It counts in parts by weight, weighs 45~50 parts of enzymolysis liquids, 15~20 parts of dry collagenous fibres, 6~8 parts of persulfuric acid respectively
Potassium and 2~3 parts of glyoxalic acids are placed in three-necked flask, adjust pH to 7.0, and heating water bath, standing is cooled to room temperature and filter residue,
Washing, drying can be prepared into a kind of antibiont support type collagen fiber adsorption material.
2. a kind of preparation method of antibiont support type collagen fiber adsorption material according to claim 1, feature exist
In:Step(1)The temperature that is heated to reflux is 55~60 DEG C.
3. a kind of preparation method of antibiont support type collagen fiber adsorption material according to claim 1, feature exist
In:Step(2)The pepsin additive amount is 50U/g.
4. a kind of preparation method of antibiont support type collagen fiber adsorption material according to claim 1, feature exist
In:Step(4)The adjusting pH is using 5% sodium hydroxide of mass fraction.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110820331A (en) * | 2019-11-25 | 2020-02-21 | 张威劲 | Preparation method of high-strength anti-wrinkle finishing agent material for natural fiber fabric |
CN115336620A (en) * | 2022-08-22 | 2022-11-15 | 山东海奥斯生物科技股份有限公司 | Process for preparing casing by utilizing collagen fibers recovered from waste water |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110820331A (en) * | 2019-11-25 | 2020-02-21 | 张威劲 | Preparation method of high-strength anti-wrinkle finishing agent material for natural fiber fabric |
CN115336620A (en) * | 2022-08-22 | 2022-11-15 | 山东海奥斯生物科技股份有限公司 | Process for preparing casing by utilizing collagen fibers recovered from waste water |
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