CN104927097B - A kind of method that microwave-hydrothermal method prepares nano titanium oxide/Chitosan Composites - Google Patents
A kind of method that microwave-hydrothermal method prepares nano titanium oxide/Chitosan Composites Download PDFInfo
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- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 22
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229920001661 Chitosan Polymers 0.000 claims abstract description 37
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 239000002243 precursor Substances 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 13
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000004044 response Effects 0.000 claims abstract description 9
- 239000012065 filter cake Substances 0.000 claims abstract description 8
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 238000012805 post-processing Methods 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 7
- 239000005416 organic matter Substances 0.000 abstract description 4
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- 239000004753 textile Substances 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract 1
- 238000012986 modification Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 23
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 14
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 12
- 239000002245 particle Substances 0.000 description 8
- 235000011121 sodium hydroxide Nutrition 0.000 description 7
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000003618 dip coating Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000004224 protection Effects 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 239000013066 combination product Substances 0.000 description 1
- 229940127555 combination product Drugs 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- -1 has sol-gel process Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Abstract
The invention discloses a kind of method that microwave-hydrothermal method prepares nano titanium oxide/Chitosan Composites, chitosan is dissolved in acetic acid solution and is configured to chitosan solution, under 50 DEG C~60 DEG C constant temperatures, it is slowly added into 25% glutaraldehyde and butyl titanate, and it is stirred continuously, then sodium hydroxide solution regulation pH value is added, continues to stir, obtains the precursor liquid of microwave hydrothermal reaction；Above-mentioned gained precursor liquid is moved into the reactor of polytetrafluoroethyllining lining, then reactor is put into microwave hydrothermal reaction and carries out hydro-thermal reaction；Question response is finished, and reactor is taken out, and is filtered, and after gained Washing of Filter Cake, is dried under 40 DEG C of constant temperatures, nano titanium oxide/chitosan complexes are made.Obtain product in this way all has superior performance in absorption degradation organic matter, textile material modification, fresh keeping property etc., and technique is simple, the reaction time is short, reaction temperature is low, energy consumption is small.
Description
Technical field
The present invention relates to a kind of method that microwave-hydrothermal method prepares nano titanium oxide/Chitosan Composites.
Background technology
Chitosan is a kind of natural macromolecule flocculating agent, is widely present in nature, and chitosan has good flocculation
And chelation, there are good biocompatibility, biological degradability, adsorptivity etc., in food, environmental protection, medicine and water process
Exploitation and application are obtained in field.Nano titanium oxide has that particle diameter is small, specific surface area is big, surface-active is high, bio-compatibility
It is good and absorb the performance that UV resistance waits by force uniqueness, in environmental protection, fine ceramics, catalysis material, sewage disposal and hospitality industry
Extensive use is able to, there is chemical property stabilization, indissoluble, nontoxic, inexpensive.But single nano titanium oxide or
All also there is certain weak point in chitosan, the advantageous property of two kinds of materials is combined into composite is in above-mentioned field
It is a kind of preferably to solve method.Nano titanium oxide/Chitosan Composites have the advantages of organic matter and inorganic matter concurrently, are preparing
Biology sensor material, absorption degradation organic matter, sewage disposal and medical material etc. all have superior performance.
At present, the preparation method of nano titanium oxide/Chitosan Composites mainly has sol-gel process, blended cross linking
The methods of method, hydro-thermal method, dip coating.Cost of material used in sol-gel process costly, generally whole colloidal sol-solidifying
It is longer the time required to glue process, a few days or a few weeks are often needed, a large amount of micropores in gel be present, will be escaped again in the drying process
Many gases and organic matter, and the defects of produce contraction, Chinese patent 200710168966.6 is exactly to use sol-gel process；
Blended cross linking method is to prepare the simplest method of nano titanium oxide/Chitosan Composites, first dissolves the chitosan in acetic acid
In solution, crosslinking agent and nano-titanium dioxide powder are then added, nanometer titanium dioxide is made using mechanical agitation and Ultrasonic Radiation
Titanium is dispersed, deaeration, and the method particle is easily reunited, and causes to be separated；Dip coating method prepares nano titanium oxide/shell and gathered
Sugared composite first has to prepare TiO 2 sol and chitosan solution, then carrier is successively immersed in TiO 2 sol and
In chitosan so that nano titanium oxide and chitosan form composite in carrier surface, because carrier is typically porous
Material, so, metal skewness inside and outside porous material duct after dipping, and it is time-consuming longer；Hydro-thermal method refers to special
Closed reactor（Autoclave）In, using the aqueous solution as reaction system, by heating, pressurizeing to reaction system（It is or spontaneous
Vapour pressure）, create a relatively-high temperature, the reaction environment of high pressure so that reaction substrate interpenetrates, and accelerates reaction rate, passes
The hydrothermal synthesis method operating condition of system is complicated and more harsh, and hydro-thermal method prepares nano titanium oxide/Chitosan Composites,
Using nano titanium dioxide particles and chitosan as raw material, the soda lye of strong basicity is solvent, in certain temperature and
The composite prepared under pressure.The change of its reaction condition can produce the combination product of different structure, or even can not answer at all
Have to carry out at high temperature under high pressure when closing, and reacting, consersion unit requires high, and technical difficulty is big.
Microwave is a kind of special mode of heating, and microwave-hydrothermal method has incomparable excellent of other conventional synthesis technologies
Point, such as reaction speed are fast, generated time is short, reaction efficiency is high, therefore are suitable for being generalized in large-scale industrial production,
Good development momentum and wide application prospect are shown in liquid phase synthesis reaction field, various countries has been subjected to and has weighed extensively
Depending on.By the use of microwave-hydrothermal method i.e. using microwave as mode of heating, nano titanium oxide/chitosan is prepared with reference to traditional hydro-thermal method
Composite is a kind of new method, can solve problems and shortcomings existing for prior art.
The content of the invention
It is an object of the invention to provide the side that a kind of microwave-hydrothermal method prepares nano titanium oxide/Chitosan Composites
Method.The method is simple to operate, and the reaction time is short, and reaction temperature is low, and energy consumption is small, and nano titanium oxide/chitosan of gained is multiple
Condensation material well-crystallized, particle size dispersion is uniform, and pattern is complete, and repeatability is high.
In order to solve the above problems, technical scheme comprises the following steps：
1st, precursor liquid is prepared
Chitosan is dissolved in acetic acid solution and is configured to chitosan solution, is placed in three-necked flask reactor, 50
DEG C~60 DEG C of constant temperatures under, be slowly added into glutaraldehyde and butyl titanate, and be stirred continuously, then add sodium hydroxide solution
PH value is adjusted, continues to stir, obtains the precursor liquid of microwave hydrothermal reaction.
2nd, microwave hydrothermal reacts
Above-mentioned gained precursor liquid is moved into the reactor of polytetrafluoroethyllining lining, then that reactor is put into microwave hydrothermal is anti-
Ying Yizhong carries out hydro-thermal reaction.
3rd, the post processing of reaction solution
Question response is finished, and reactor is taken out, and is filtered, and after gained Washing of Filter Cake, is done under 40 DEG C of constant temperatures
It is dry, nano titanium oxide/chitosan complexes are made.
A kind of preferred scheme, it is described to prepare in precursor liquid step, chitosan is dissolved in acetic acid solution and is configured to concentration
10mg/L~20mg/L chitosan solution.
A kind of preferred scheme, it is described to prepare in precursor liquid step, control the mol ratio of chitosan structure unit and glutaraldehyde
For 1: 1~6；The mass ratio of chitosan and nano titanium oxide is 1: 6~12.
A kind of preferred scheme, described to prepare in precursor liquid step, pH values are 6~7.
A kind of preferred scheme, in the microwave hydrothermal reactions steps, reactor range of reaction temperature is 150~200 DEG C,
Soaking time is 50~90 minutes.
The innovation of the present invention is at home first using microwave-hydrothermal method at a temperature of 150~200 DEG C
A diameter of 20~90 nm well-crystallized, the uniform nano titanium oxide/Chitosan Composites of particle diameter distribution are prepared, are being inhaled
Attached degradation of organic substances, textile material are modified, fresh keeping property etc. all has superior performance, and technique is simple, when reacting
Between it is short, reaction temperature is low, energy consumption is small.
Brief description of the drawings
Fig. 1 is the TEM figures of nano titanium oxide/chitosan complexes sample prepared by the present invention, as can be seen from the figure
Sample crystallization is good, particle diameter distribution is uniform, and particle diameter is smaller in 20nm or so, the reunion degree of particle.
With reference to embodiment, the present invention is described in further detail.
Embodiment
Embodiment 1
Chitosan is dissolved in acetic acid solution to be configured to concentration be 10mg/L chitosan solution 300ml, is placed on three mouthfuls
In flask reactor, under 50 DEG C~60 DEG C constant temperatures, 1.86g glutaraldehydes and 90ml butyl titanates are slowly added into, not
PH value is adjusted to 7 by disconnected stirring, the sodium hydroxide solution for then adding 0.4mol/L, continues stirring 10 minutes, it is anti-to obtain microwave hydrothermal
The precursor liquid answered；Precursor liquid is moved into the reactor of polytetrafluoroethyllining lining, then reactor is put into microwave hydrothermal reaction
In, stop reaction after being incubated 70 minutes at being 160 DEG C in temperature；After question response temperature is down to room temperature, reactor is taken out, carried out
Filter, gained filter cake is washed with deionized after being dried under 40 DEG C of constant temperatures, it is multiple that nano titanium oxide/chitosan is made
Compound.
Embodiment 2
Chitosan is dissolved in acetic acid solution to be configured to concentration be 15mg/L chitosan solution 200ml, is placed on three mouthfuls
In flask reactor, under 50 DEG C~60 DEG C constant temperatures, 5.58g glutaraldehydes and 120ml butyl titanates are slowly added into, not
PH value is adjusted to 6~7 by disconnected stirring, the sodium hydroxide solution for then adding 0.4mol/L, is continued stirring 10 minutes, is obtained Microwave Water
The precursor liquid of thermal response；Precursor liquid is moved into the reactor of polytetrafluoroethyllining lining, then that reactor is put into microwave hydrothermal is anti-
Ying Yizhong, stop reaction after being incubated 70 minutes at being 160 DEG C in temperature；After question response temperature is down to room temperature, reactor is taken out,
Filtered, gained filter cake is washed with deionized after being dried under 40 DEG C of constant temperatures, nano titanium oxide/shell is made and gathers
Saccharide complex.
Embodiment 3
Chitosan is dissolved in acetic acid solution to be configured to concentration be 15mg/L chitosan solution 200ml, is placed on three mouthfuls
In flask reactor, under 50 DEG C~60 DEG C constant temperatures, 9.3g glutaraldehydes and 150ml butyl titanates are slowly added into, not
PH value is adjusted to 7 by disconnected stirring, the sodium hydroxide solution for then adding 0.4mol/L, continues stirring 10 minutes, it is anti-to obtain microwave hydrothermal
The precursor liquid answered；Precursor liquid is moved into the reactor of polytetrafluoroethyllining lining, then reactor is put into microwave hydrothermal reaction
In, stop reaction after being incubated 60 minutes at being 180 DEG C in temperature；After question response temperature is down to room temperature, reactor is taken out, carried out
Filter, gained filter cake is washed with deionized after being dried under 40 DEG C of constant temperatures, it is multiple that nano titanium oxide/chitosan is made
Compound.
Embodiment 4
Chitosan is dissolved in acetic acid solution to be configured to concentration be 20mg/L chitosan solution 150ml, is placed on three mouthfuls
In flask reactor, under 50 DEG C~60 DEG C constant temperatures, 4.96g glutaraldehydes and 100ml butyl titanates are slowly added into, not
PH value is adjusted to 7 by disconnected stirring, the sodium hydroxide solution for then adding 0.4mol/L, continues stirring 10 minutes, it is anti-to obtain microwave hydrothermal
The precursor liquid answered；Precursor liquid is moved into the reactor of polytetrafluoroethyllining lining, then reactor is put into microwave hydrothermal reaction
In, stop reaction after being incubated 50 minutes at being 190 DEG C in temperature；After question response temperature is down to room temperature, reactor is taken out, carried out
Filter, gained filter cake is washed with deionized after being dried under 40 DEG C of constant temperatures, it is multiple that nano titanium oxide/chitosan is made
Compound.
Embodiment 5
Chitosan is dissolved in acetic acid solution to be configured to concentration be 20mg/L chitosan solution 150ml, is placed on three mouthfuls
In flask reactor, under 50 DEG C~60 DEG C constant temperatures, 2.4g glutaraldehydes and 120ml butyl titanates are slowly added into, not
PH value is adjusted to 7 by disconnected stirring, the sodium hydroxide solution for then adding 0.4mol/L, continues stirring 10 minutes, it is anti-to obtain microwave hydrothermal
The precursor liquid answered；Precursor liquid is moved into the reactor of polytetrafluoroethyllining lining, then reactor is put into microwave hydrothermal reaction
In, stop reaction after being incubated 60 minutes at being 170 DEG C in temperature；After question response temperature is down to room temperature, reactor is taken out, carried out
Filter, gained filter cake is washed with deionized after being dried under 40 DEG C of constant temperatures, it is multiple that nano titanium oxide/chitosan is made
Compound.
Claims (4)
1. a kind of method that microwave-hydrothermal method prepares nano titanium oxide/Chitosan Composites, it is characterised in that including as follows
Step：
（1）Prepare precursor liquid
Chitosan is dissolved in acetic acid solution and is configured to chitosan solution, is placed in three-necked flask reactor, 50 DEG C~
Under 60 DEG C of constant temperatures, glutaraldehyde and butyl titanate are slowly added into, and is stirred continuously, then adds sodium hydroxide solution
PH value is adjusted, continues to stir, obtains the precursor liquid of microwave hydrothermal reaction；
Described to prepare in precursor liquid step, it is 1: 1~6 to control the mol ratio of chitosan structure unit and glutaraldehyde；
（2）Microwave hydrothermal reacts
Above-mentioned gained precursor liquid is moved into the reactor of polytetrafluoroethyllining lining, then reactor is put into microwave hydrothermal reaction
Middle carry out hydro-thermal reaction；
（3）The post processing of reaction solution
Question response is finished, and reactor is taken out, and is filtered, and after gained Washing of Filter Cake, is dried under 40 DEG C of constant temperatures, system
Obtain nano titanium oxide/chitosan complexes.
2. the method that microwave-hydrothermal method prepares nano titanium oxide/Chitosan Composites according to claim 1, its feature
It is：It is described to prepare in precursor liquid step, chitosan is dissolved in concentration is configured in acetic acid solution as 10mg/L~20mg/L's
Chitosan solution.
3. the method that microwave-hydrothermal method prepares nano titanium oxide/Chitosan Composites according to claim 1, its feature
It is：Described to prepare in precursor liquid step, pH value is 6~7.
4. the method that microwave-hydrothermal method prepares nano titanium oxide/Chitosan Composites according to claim 1, its feature
It is：In the microwave hydrothermal reactions steps, range of reaction temperature is 150~200 DEG C, and soaking time is 50~90 minutes.
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| CN106268968A (en) * | 2016-09-28 | 2017-01-04 | 中南林业科技大学 | A kind of preparation method and application of chitosan loaded composite titania material |
| CN108217868B (en) * | 2017-12-07 | 2020-12-01 | 广州市弗雷德环保科技有限公司 | Preparation method of composite algaecide with high algae removal rate |
| CN109135474A (en) * | 2018-08-02 | 2019-01-04 | 佛山市高明区爪和新材料科技有限公司 | A kind of cation acrylic -ol acid resin water paint |
| CN108914388B (en) * | 2018-08-15 | 2020-06-23 | 安徽利通达纤维新材料有限公司 | High-strength composite non-woven fabric with antibacterial effect |
| CN110616031A (en) * | 2019-09-17 | 2019-12-27 | 湖州市南浔联谊喷涂厂 | Heat insulation coating with super-strong weather resistance and preparation method thereof |
| CN113230746B (en) * | 2021-06-07 | 2022-12-02 | 温州大学激光与光电智能制造研究院 | Preparation method of filtering membrane |
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| CN101210081A (en) * | 2007-12-20 | 2008-07-02 | 江汉大学 | Preparation for chitosan/titanium dioxide composite material |
| CN103586002A (en) * | 2013-10-30 | 2014-02-19 | 合肥学院 | Preparation method of hybrid film adsorbent for removing heavy metal ions in water |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101210081A (en) * | 2007-12-20 | 2008-07-02 | 江汉大学 | Preparation for chitosan/titanium dioxide composite material |
| CN103586002A (en) * | 2013-10-30 | 2014-02-19 | 合肥学院 | Preparation method of hybrid film adsorbent for removing heavy metal ions in water |
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