CN107474295A - A kind of preparation method of beta cyclodextrin Chitosan Composites - Google Patents

A kind of preparation method of beta cyclodextrin Chitosan Composites Download PDF

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Publication number
CN107474295A
CN107474295A CN201710878943.8A CN201710878943A CN107474295A CN 107474295 A CN107474295 A CN 107474295A CN 201710878943 A CN201710878943 A CN 201710878943A CN 107474295 A CN107474295 A CN 107474295A
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CN
China
Prior art keywords
beta cyclodextrin
preparation
chitosan
chitosan composites
temperature
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Pending
Application number
CN201710878943.8A
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Chinese (zh)
Inventor
周文婷
罗超
何运良
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Wuhan Qianruitai Environmental Science And Technology Co Ltd
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Wuhan Qianruitai Environmental Science And Technology Co Ltd
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Priority to CN201710878943.8A priority Critical patent/CN107474295A/en
Publication of CN107474295A publication Critical patent/CN107474295A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/286Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/12Chemical modification
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L5/00Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
    • C08L5/08Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L5/00Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
    • C08L5/16Cyclodextrin; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2305/00Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
    • C08J2305/16Cyclodextrin; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2405/00Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
    • C08J2405/08Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Analytical Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • General Chemical & Material Sciences (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

It is an object of the invention to provide a kind of compound material being prepared into of beta cyclodextrin chitosan, the composite of formation is cellular membrane material, the contact area of increase sewage and water purification composite, improves cleaning water.

Description

A kind of preparation method of beta cyclodextrin-Chitosan Composites
Technical field
The present invention relates to a kind of preparation method of beta cyclodextrin-Chitosan Composites, belongs to water pollution treatment technology neck Domain.
Background technology
Chitosan-phospholipid complex is all to have good flocculation, clarification.As the fining agent of beverage, suspension can be made Thing flocculates rapidly, natural sedimentation, improves the yield of stoste;In Chinese medicine extract, protein, tannic acid and the pectin of macromolecular, It can easily be removed with chitosan solution, refine out the higher effective components of Chinese medicinal of purity;Using the adsorptivity of chitosan, There is good effect in terms of purification of water quality.
Beta cyclodextrin molecule is the cyclic oligosaccharide being formed by connecting by 7 glucose monomers, and its example structure is in cylinder Shape.Because covering of the hydrogen atom to oxygen atom on C1 acts on C3 and C5, the inner chamber of cyclodextrin has stronger hydrophobicity, can be with Guest molecule is included using its hydrophobic cavity, forms inclusion.It can strengthen the tensile resistance of chitosan and anti-tear with beta cyclodextrin Fragility energy so that it forms cellular film, the preferably pollutant in absorption effluent with chitosan.
Therefore, a kind of compound material being prepared into of beta cyclodextrin-chitosan can be studied, the composite of formation is porous Shape membrane material, the contact area of increase sewage and water purification composite, improve cleaning water.
The content of the invention
It is an object of the invention to provide a kind of compound material being prepared into of beta cyclodextrin-chitosan, the composite of formation For cellular membrane material, the contact area of increase sewage and water purification composite, cleaning water is improved.
The present invention provides a kind of preparation method of beta cyclodextrin-Chitosan Composites, comprises the following steps (1) constant Under conditions of reaction temperature stirring, beta cyclodextrin, citric acid, PEG-400 are dissolved in water, form solution A;(2) in solution A Catalyst sodium dihydrogen phosphate dihydrate is added, reacts 4.5h at a constant temperature, is cooled down, is washed, is filtered, drying, obtains beta cyclodextrin polymerization Thing;(3) take chitosan to be dissolved in water, add acetic acid thereto, generate colloidal liquid, beta cyclodextrin is added in colloidal liquid and is gathered Compound, form blending liquid;(4) it is evenly laid out on a glass that liquid will be blended, dry, form just film;(5) first film is put into 3h is reacted in crosslinking agent, takes out, ethanol wash, dries to obtain beta cyclodextrin-Chitosan Composites.
Further improvement of the present invention, constant reaction temperature is 45~60 DEG C in step (1).
Further improvement of the present invention, the temperature of constant temperature is 120~150 DEG C in step (2).
Further improvement of the present invention, the mass ratio of middle chitosan and beta cyclodextrin is 1:20~60.
Further improvement of the present invention, it is 95% acetic acid to add 4~8ml mass concentrations per 100g chitosans in step (3).
Further improvement of the present invention, the temperature of step (3) is 60~80 DEG C.
Further improvement of the present invention, just the thickness of film is 1~1.5mm in step (4).
Further improvement of the present invention, crosslinking agent are the VTES of mass concentration 20%.
Compared with prior art, beneficial effects of the present invention:
1st, preparation method low in raw material price of the invention, is readily obtained, and technique is simple, can save production cost, is adapted to The purification run of industrial wastewater, and prepare composite good film-forming property, easily recycle, recycling material it is net Water effect reduces without obvious.
2nd, the present invention prepares the tensile resistance and tear resistance that can strengthen chitosan using beta cyclodextrin in composite Can so that it forms cellular film with chitosan, the contact area of increase sewage and water purification composite, improves water purification effect Rate.
Embodiment
Embodiment 1:
The present invention provides a kind of preparation method of beta cyclodextrin-Chitosan Composites, comprises the following steps (1) constant Under conditions of reaction temperature stirring, beta cyclodextrin, citric acid, PEG-400 are dissolved in water, form solution A;(2) in solution A Catalyst sodium dihydrogen phosphate dihydrate is added, reacts 4.5h at a constant temperature, is cooled down, is washed, is filtered, drying, obtains beta cyclodextrin polymerization Thing;(3) take chitosan to be dissolved in water, add acetic acid thereto, generate colloidal liquid, beta cyclodextrin is added in colloidal liquid and is gathered Compound, form blending liquid;(4) it is evenly laid out on a glass that liquid will be blended, dry, form just film;(5) first film is put into 3h is reacted in crosslinking agent, takes out, ethanol wash, dries to obtain beta cyclodextrin-Chitosan Composites.
Further improvement of the present invention, constant reaction temperature is 45 DEG C in step (1).
Further improvement of the present invention, the temperature of constant temperature is 120 DEG C in step (2).
Further improvement of the present invention, the mass ratio of middle chitosan and beta cyclodextrin is 1:20.
Further improvement of the present invention, it is 95% acetic acid to add 4ml mass concentrations per 100g chitosans in step (3).
Further improvement of the present invention, the temperature of step (3) is 60 DEG C.
Further improvement of the present invention, just the thickness of film is 1mm in step (4).
Further improvement of the present invention, crosslinking agent are the VTES of mass concentration 20%.
Embodiment 2:
The present invention provides a kind of preparation method of beta cyclodextrin-Chitosan Composites, comprises the following steps (1) constant Under conditions of reaction temperature stirring, beta cyclodextrin, citric acid, PEG-400 are dissolved in water, form solution A;(2) in solution A Catalyst sodium dihydrogen phosphate dihydrate is added, reacts 4.5h at a constant temperature, is cooled down, is washed, is filtered, drying, obtains beta cyclodextrin polymerization Thing;(3) take chitosan to be dissolved in water, add acetic acid thereto, generate colloidal liquid, beta cyclodextrin is added in colloidal liquid and is gathered Compound, form blending liquid;(4) it is evenly laid out on a glass that liquid will be blended, dry, form just film;(5) first film is put into 3h is reacted in crosslinking agent, takes out, ethanol wash, dries to obtain beta cyclodextrin-Chitosan Composites.
Further improvement of the present invention, constant reaction temperature is 60 DEG C in step (1).
Further improvement of the present invention, the temperature of constant temperature is 150 DEG C in step (2).
Further improvement of the present invention, the mass ratio of middle chitosan and beta cyclodextrin is 1:60.
Further improvement of the present invention, it is 95% acetic acid to add 8ml mass concentrations per 100g chitosans in step (3).
Further improvement of the present invention, the temperature of step (3) is 80 DEG C.
Further improvement of the present invention, just the thickness of film is 1.5mm in step (4).
Further improvement of the present invention, crosslinking agent are the VTES of mass concentration 20%.
Embodiment 3:
The present invention provides a kind of preparation method of beta cyclodextrin-Chitosan Composites, comprises the following steps (1) constant Under conditions of reaction temperature stirring, beta cyclodextrin, citric acid, PEG-400 are dissolved in water, form solution A;(2) in solution A Catalyst sodium dihydrogen phosphate dihydrate is added, reacts 4.5h at a constant temperature, is cooled down, is washed, is filtered, drying, obtains beta cyclodextrin polymerization Thing;(3) take chitosan to be dissolved in water, add acetic acid thereto, generate colloidal liquid, beta cyclodextrin is added in colloidal liquid and is gathered Compound, form blending liquid;(4) it is evenly laid out on a glass that liquid will be blended, dry, form just film;(5) first film is put into 3h is reacted in crosslinking agent, takes out, ethanol wash, dries to obtain beta cyclodextrin-Chitosan Composites.
Further improvement of the present invention, constant reaction temperature is 50 DEG C in step (1).
Further improvement of the present invention, the temperature of constant temperature is 130 DEG C in step (2).
Further improvement of the present invention, the mass ratio of middle chitosan and beta cyclodextrin is 1:50.
Further improvement of the present invention, it is 95% acetic acid to add 6ml mass concentrations per 100g chitosans in step (3).
Further improvement of the present invention, the temperature of step (3) is 60~80 DEG C.
Further improvement of the present invention, just the thickness of film is 1.2mm in step (4).
Further improvement of the present invention, crosslinking agent are the VTES of mass concentration 20%.
Embodiment 4:
The present invention provides a kind of preparation method of beta cyclodextrin-Chitosan Composites, comprises the following steps (1) constant Under conditions of reaction temperature stirring, beta cyclodextrin, citric acid, PEG-400 are dissolved in water, form solution A;(2) in solution A Catalyst sodium dihydrogen phosphate dihydrate is added, reacts 4.5h at a constant temperature, is cooled down, is washed, is filtered, drying, obtains beta cyclodextrin polymerization Thing;(3) take chitosan to be dissolved in water, add acetic acid thereto, generate colloidal liquid, beta cyclodextrin is added in colloidal liquid and is gathered Compound, form blending liquid;(4) it is evenly laid out on a glass that liquid will be blended, dry, form just film;(5) first film is put into 3h is reacted in crosslinking agent, takes out, ethanol wash, dries to obtain beta cyclodextrin-Chitosan Composites.
Further improvement of the present invention, constant reaction temperature is 50 DEG C in step (1).
Further improvement of the present invention, the temperature of constant temperature is 140 DEG C in step (2).
Further improvement of the present invention, the mass ratio of middle chitosan and beta cyclodextrin is 1:35.
Further improvement of the present invention, it is 95% acetic acid to add 4ml mass concentrations per 100g chitosans in step (3).
Further improvement of the present invention, the temperature of step (3) is 60 DEG C.
Further improvement of the present invention, just the thickness of film is 1mm in step (4).
Further improvement of the present invention, crosslinking agent are the VTES of mass concentration 20%.

Claims (8)

  1. A kind of 1. preparation method of beta cyclodextrin-Chitosan Composites, it is characterised in that:Comprise the following steps (1) constant anti- Under conditions of answering temperature stirring, beta cyclodextrin, citric acid, PEG-400 are dissolved in water, form solution A;(2) add in solution A Enter catalyst sodium dihydrogen phosphate dihydrate, react 4.5h at a constant temperature, cool down, wash, filter, drying, obtain beta cyclodextrin polymerization Thing;(3) take chitosan to be dissolved in water, add acetic acid thereto, generate colloidal liquid, beta cyclodextrin is added in colloidal liquid and is gathered Compound, form blending liquid;(4) it is evenly laid out on a glass that liquid will be blended, dry, form just film;(5) first film is put into 3h is reacted in crosslinking agent, takes out, ethanol wash, dries to obtain beta cyclodextrin-Chitosan Composites.
  2. 2. the preparation method of beta cyclodextrin-Chitosan Composites according to claim 1, it is characterised in that:The step (1) constant reaction temperature is 45~60 DEG C in.
  3. 3. the preparation method of beta cyclodextrin-Chitosan Composites according to claim 1, it is characterised in that:The step (2) temperature of constant temperature is 120~150 DEG C in.
  4. 4. the preparation method of beta cyclodextrin-Chitosan Composites according to claim 1, it is characterised in that:The middle shell gathers The mass ratio of sugar and beta cyclodextrin is 1:20~60.
  5. 5. the preparation method of beta cyclodextrin-Chitosan Composites according to claim 1, it is characterised in that:The step (3) it is 95% acetic acid to add 4~8ml mass concentrations per 100g chitosans in.
  6. 6. the preparation method of beta cyclodextrin-Chitosan Composites according to claim 1, it is characterised in that:The step (3) temperature is 60~80 DEG C.
  7. 7. the preparation method of beta cyclodextrin-Chitosan Composites according to claim 1, it is characterised in that:The step (4) just the thickness of film is 1~1.5mm in.
  8. 8. the preparation method of beta cyclodextrin-Chitosan Composites according to claim 1, it is characterised in that:The crosslinking agent For the VTES of mass concentration 20%.
CN201710878943.8A 2017-09-26 2017-09-26 A kind of preparation method of beta cyclodextrin Chitosan Composites Pending CN107474295A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110407267A (en) * 2019-08-08 2019-11-05 中国石油集团渤海钻探工程有限公司 A kind of filters pressing liquid processing method
CN112844332A (en) * 2021-01-08 2021-05-28 温州大学 Preparation method and application of cyclodextrin-citric acid graft loaded ceramic ball
CN115887305A (en) * 2023-01-06 2023-04-04 同芙集团(中国)股份有限公司 Herbal skin care film powder for improving antioxidant activity and moisturizing property of skin
CN117531484A (en) * 2024-01-08 2024-02-09 成都达奇科技股份有限公司 Active carbon film material and preparation method and application thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110407267A (en) * 2019-08-08 2019-11-05 中国石油集团渤海钻探工程有限公司 A kind of filters pressing liquid processing method
CN112844332A (en) * 2021-01-08 2021-05-28 温州大学 Preparation method and application of cyclodextrin-citric acid graft loaded ceramic ball
CN115887305A (en) * 2023-01-06 2023-04-04 同芙集团(中国)股份有限公司 Herbal skin care film powder for improving antioxidant activity and moisturizing property of skin
CN117531484A (en) * 2024-01-08 2024-02-09 成都达奇科技股份有限公司 Active carbon film material and preparation method and application thereof

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Application publication date: 20171215

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