CN106540748A - The preparation method of polythiophene tin dioxide composite material - Google Patents
The preparation method of polythiophene tin dioxide composite material Download PDFInfo
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- CN106540748A CN106540748A CN201611052465.7A CN201611052465A CN106540748A CN 106540748 A CN106540748 A CN 106540748A CN 201611052465 A CN201611052465 A CN 201611052465A CN 106540748 A CN106540748 A CN 106540748A
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- polythiophene
- composite material
- dioxide composite
- tin dioxide
- preparation
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229920000123 polythiophene Polymers 0.000 title abstract 4
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001556 precipitation Methods 0.000 claims abstract description 13
- 238000005119 centrifugation Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- 239000002243 precursor Substances 0.000 claims abstract description 9
- 229910000375 tin(II) sulfate Inorganic materials 0.000 claims abstract description 9
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 8
- 229930192474 thiophene Natural products 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000000178 monomer Substances 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims abstract description 5
- 238000005286 illumination Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000006552 photochemical reaction Methods 0.000 claims description 4
- RCIVOBGSMSSVTR-UHFFFAOYSA-L stannous sulfate Chemical compound [SnH2+2].[O-]S([O-])(=O)=O RCIVOBGSMSSVTR-UHFFFAOYSA-L 0.000 claims description 4
- 238000003786 synthesis reaction Methods 0.000 claims description 4
- 238000002242 deionisation method Methods 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 5
- 230000001699 photocatalysis Effects 0.000 abstract description 5
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 238000006116 polymerization reaction Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 abstract description 2
- 230000004044 response Effects 0.000 abstract description 2
- 230000003595 spectral effect Effects 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 239000004020 conductor Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 241001597008 Nomeidae Species 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229920000547 conjugated polymer Polymers 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
Classifications
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/12—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing organo-metallic compounds or metal hydrides
- B01J31/123—Organometallic polymers, e.g. comprising C-Si bonds in the main chain or in subunits grafted to the main chain
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/345—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of ultraviolet wave energy
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Optics & Photonics (AREA)
- Health & Medical Sciences (AREA)
- Plasma & Fusion (AREA)
- Toxicology (AREA)
- Electromagnetism (AREA)
- Catalysts (AREA)
- Chemically Coating (AREA)
Abstract
The present invention discloses a kind of preparation method of polythiophene tin dioxide composite material, comprises the steps of：By SnSO4It is dissolved in the sulfuric acid solution of 0.2 mol/L, is made into precursor solution, be placed under the uviol lamp of 8W after irradiation 12h, collects precipitation, be washed with deionized to the pH=7 of filtrate, drying will be deposited in, SnO is obtained2Powder body, by SnO2During powder body and dehydrated alcohol add quartzy triangular flask, after ultrasonic disperse, thiophene monomer, stirring is added to be placed in illumination 24h under the uviol lamp of 2 8W, precipitation is collected in centrifugation, with absolute ethanol washing, is vacuum dried, is obtained polythiophene tin dioxide composite material.The present invention induces thiophene monomer to be prepared for polythiophene tin dioxide composite material in tin ash in situ Polymerization by photochemical method, and with wider spectral response range, the impurity for containing is few, and product purity is high, and photocatalysis performance is good.
Description
Technical field
The invention belongs to the preparation field of composite, and in particular to a kind of system of polythiophene-tin dioxide composite material
Preparation Method.
Background technology
Photocatalysis technology is environmental improvement and a kind of effective way for obtaining clean energy resource, in recent years high efficiency photocatalyst
Development causes common concern.Conductor oxidate is (such as TiO2、SnO2With ZnO etc.) it is conventional conductor photocatalysis material.But
Their Chang Yinwei have larger bandwidth, and application to a certain extent is restricted.Using conjugated polymer (as polyaniline,
Thiophene, polypyrrole and its derivant) composite sensitization is carried out to which, it is the effective way for improving one-component optical catalyst catalytic performance
One of.
The method for preparing conjugated polymers-conductor oxidate composite photocatalyst material at present mainly has oxidation reducing in-situ to gather
Close, heat treatment etc. is blended.In these methods, usually remove as other cationes for introducing are difficult, or polymer and quasiconductor it
Ask that interracial contact is insufficient etc., affect the photocatalysis performance of composite.
The content of the invention
The present invention provides a kind of method that photochemistry prepares polythiophene-tin dioxide composite material.
The present invention is achieved by the following technical solutions.
The preparation method of polythiophene-tin dioxide composite material, comprises the steps of：
（1）Weigh 2.68 g stannous sulfate SnSO4It is dissolved in the sulfuric acid solution of 250 mL, 0.2 mol/L, is made into 0.05
The precursor solution of mol/L；
（2）By step（1）The precursor solution for obtaining is placed under the uviol lamp of 8W after 12 h of irradiation, is collected precipitation, is used deionization
The pH=7 of water washing to filtrate, will be deposited at 120 DEG C and be dried 4 h, obtain the SnO of photochemical syntheses2Powder body；
（3）By 1g SnO2During powder body and 150 mL dehydrated alcohol add quartzy triangular flask, after ultrasonic disperse 30min, 1 mL is added
Thiophene monomer, stirring are placed on illumination 24h under the uviol lamp of 28 W, and precipitation, precipitation dehydrated alcohol are collected in centrifugation
Washing 5 times, is vacuum dried 10 h at 60 DEG C, obtains the polythiophene-tin dioxide composite material of photochemical reaction preparation.
Preferably, step（2）And step（3）In uviol lamp dominant wavelength be 254nm.
Preferably, step（3）The power of middle ultrasound is 150W.
Preferably, step（3）The condition of centrifugation is centrifugal rotational speed 1500rpm, and centrifugation time is 30min.
Advantages of the present invention：
The present invention induces thiophene monomer to be prepared for polythiophene-tin ash in tin ash in situ Polymerization by photochemical method
Composite, with wider spectral response range, the impurity for containing is few, and product purity is high, declines in uviol lamp and sunlight
The speed of solution methyl orange is high, and photocatalysis performance is good.
Specific embodiment
Embodiment 1
The preparation method of polythiophene-tin dioxide composite material, comprises the steps of：
（1）Weigh 2.68 g stannous sulfate SnSO4It is dissolved in the sulfuric acid solution of 250 mL, 0.2 mol/L, is made into 0.05
The precursor solution of mol/L；
（2）By step（1）The precursor solution for obtaining is placed under the uviol lamp of 8W after 12 h of irradiation, is collected precipitation, is used deionization
The pH=7 of water washing to filtrate, will be deposited at 120 DEG C and be dried 4 h, obtain the SnO of photochemical syntheses2Powder body；
（3）By 1g SnO2During powder body and 150 mL dehydrated alcohol add quartzy triangular flask, after ultrasonic disperse 30min, 1 mL is added
Thiophene monomer, stirring are placed on illumination 24h under the uviol lamp of 28 W, and precipitation, precipitation dehydrated alcohol are collected in centrifugation
Washing 5 times, is vacuum dried 10 h at 60 DEG C, obtains the polythiophene-tin dioxide composite material of photochemical reaction preparation.
Embodiment 2
The preparation method of polythiophene-tin dioxide composite material, comprises the steps of：
（1）Weigh 2.68 g stannous sulfate SnSO4It is dissolved in the sulfuric acid solution of 250 mL, 0.2 mol/L, is made into 0.05
The precursor solution of mol/L；
（2）By step（1）The precursor solution for obtaining is placed under the uviol lamp of 8W after 12 h of irradiation, wherein, the main ripple of uviol lamp
A length of 254nm, collects precipitation, is washed with deionized to the pH=7 of filtrate, will be deposited at 120 DEG C and be dried 4 h, and obtain photochemical
Learn the SnO of synthesis2Powder body；
（3）By 1g SnO2During powder body and 150 mL dehydrated alcohol add quartzy triangular flask, after ultrasonic disperse 30min, the work(of ultrasound
Rate is 150W, adds 1 mL thiophene monomers, stirring to be placed on illumination 24h under the uviol lamp of 28 W, wherein, uviol lamp
Dominant wavelength is 254nm, and precipitation is collected in centrifugation, and the condition of centrifugation is centrifugal rotational speed 1500rpm, and centrifugation time is 30min, is sunk
Forming sediment with absolute ethanol washing 5 times, 10 h being vacuum dried at 60 DEG C, the polythiophene-tin ash for obtaining photochemical reaction preparation is multiple
Condensation material.
Claims (4)
1. the preparation method of polythiophene-tin dioxide composite material, it is characterised in that：Comprise the steps of：
（1）Weigh 2.68 g stannous sulfate SnSO4It is dissolved in the sulfuric acid solution of 250 mL, 0.2 mol/L, is made into 0.05
The precursor solution of mol/L；
（2）By step（1）The precursor solution for obtaining is placed under the uviol lamp of 8W after 12 h of irradiation, is collected precipitation, is used deionization
The pH=7 of water washing to filtrate, will be deposited at 120 DEG C and be dried 4 h, obtain the SnO of photochemical syntheses2Powder body；
（3）By 1g SnO2During powder body and 150 mL dehydrated alcohol add quartzy triangular flask, after ultrasonic disperse 30min, 1 mL is added
Thiophene monomer, stirring are placed on illumination 24h under the uviol lamp of 28 W, and precipitation, precipitation dehydrated alcohol are collected in centrifugation
Washing 5 times, is vacuum dried 10 h at 60 DEG C, obtains the polythiophene-tin dioxide composite material of photochemical reaction preparation.
2. the preparation method of the polythiophene-tin dioxide composite material for being prepared according to claim 1, it is characterised in that：Step（2）
And step（3）In uviol lamp dominant wavelength be 254nm.
3. the preparation method of the polythiophene-tin dioxide composite material for being prepared according to claim 1, it is characterised in that：Step（3）
The power of middle ultrasound is 150W.
4. the preparation method of the polythiophene-tin dioxide composite material for being prepared according to claim 1, it is characterised in that：Step（3）
The condition of centrifugation is centrifugal rotational speed 1500rpm, and centrifugation time is 30min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611052465.7A CN106540748A (en) | 2016-11-25 | 2016-11-25 | The preparation method of polythiophene tin dioxide composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611052465.7A CN106540748A (en) | 2016-11-25 | 2016-11-25 | The preparation method of polythiophene tin dioxide composite material |
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| Publication Number | Publication Date |
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| CN106540748A true CN106540748A (en) | 2017-03-29 |
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| CN201611052465.7A Pending CN106540748A (en) | 2016-11-25 | 2016-11-25 | The preparation method of polythiophene tin dioxide composite material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111450882A (en) * | 2020-04-16 | 2020-07-28 | 华南师范大学 | Photochemical induction synthesized polythiophene microsphere photocatalyst and preparation method thereof |
| CN114669327A (en) * | 2022-04-02 | 2022-06-28 | 扬州大学 | Tin sulfide/polypyrrole composite material and preparation method and application thereof |
| CN115340131A (en) * | 2022-08-31 | 2022-11-15 | 盐城工学院 | Preparation method of cobalt disulfide-polythiophene wave-absorbing material |
-
2016
- 2016-11-25 CN CN201611052465.7A patent/CN106540748A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111450882A (en) * | 2020-04-16 | 2020-07-28 | 华南师范大学 | Photochemical induction synthesized polythiophene microsphere photocatalyst and preparation method thereof |
| CN111450882B (en) * | 2020-04-16 | 2022-10-14 | 华南师范大学 | Photochemical induction synthesized polythiophene microsphere photocatalyst and preparation method thereof |
| CN114669327A (en) * | 2022-04-02 | 2022-06-28 | 扬州大学 | Tin sulfide/polypyrrole composite material and preparation method and application thereof |
| CN115340131A (en) * | 2022-08-31 | 2022-11-15 | 盐城工学院 | Preparation method of cobalt disulfide-polythiophene wave-absorbing material |
| CN115340131B (en) * | 2022-08-31 | 2023-06-02 | 盐城工学院 | Preparation method of cobalt disulfide-polythiophene wave-absorbing material |
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Application publication date: 20170329 |
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| WD01 | Invention patent application deemed withdrawn after publication |