CN107880318A - Preparation method of hydrogen sulfide gas sensing material of biomass carrying inorganic particle and products thereof and application - Google Patents
Preparation method of hydrogen sulfide gas sensing material of biomass carrying inorganic particle and products thereof and application Download PDFInfo
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- CN107880318A CN107880318A CN201711087041.9A CN201711087041A CN107880318A CN 107880318 A CN107880318 A CN 107880318A CN 201711087041 A CN201711087041 A CN 201711087041A CN 107880318 A CN107880318 A CN 107880318A
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- hydrogen sulfide
- sulfide gas
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/30—Sulfur compounds
- B01D2257/304—Hydrogen sulfide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2303/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2303/02—Starch; Degradation products thereof, e.g. dextrin
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Abstract
The invention discloses a kind of preparation method of hydrogen sulfide gas sensing material of biomass carrying inorganic particle and products thereof and application, and using water miscible molysite and cobalt salt as presoma, addition contains OH‑Be used as precipitating reagent, spinel structure CoFe is collected by centrifugation2O4Inorganic nanoparticles.Biomass converted starch is soluble in water, film forming is mixed with inorganic particle, forms the organic film of inorganic particle insertion, its feature organic matter has loose structure, a large amount of captures of hydrogen sulfide gas can be achieved, then CoFe2O4Carry out the gas-sensitive reaction of adsorption/desorption.The present invention can make flexible air-sensitive film, and method is simple to operate, and controllability is strong, be detected for hydrogen sulfide gas.
Description
Technical field
The present invention relates to these hydrogen sulfide gas sensor, more particularly to a kind of stink damp of biomass carrying inorganic particle
Preparation method of body sensing material and products thereof and application, in particular to a kind of flexibility of inorganic nanoparticles insertion organic film
Sensing material.
Background technology
Development of modern industry causes serious air pollution, and great threat is all produced to human health and ecological environment.Sulphur
It is one of pollutant to change hydrogen, is mainly derived from oil/gas probing and refining, sewage disposal, papermaking and landfill etc..It is low
The hydrogen sulfide gas of concentration is with regard to entail dangers to health, therefore the detection of the ppm levels of working site particularly oil plant seems especially heavy
Will.
The method of testing of hydrogen sulfide has a variety of at present, and generally existing cost is high, and operating temperature height etc. can cause device in addition
Life-span is reduced.Organic conductive macromolecule film because low cost, the long-life, can on a large scale produce and cause common concern, in addition its
Flexible characteristic also allows for carrying.With AB2O4Structural inorganic nonmetallic materials turn into and ground due to showing good air-sensitive performance
The focus studied carefully, if reducing particle size to nanoscale lifting specific surface area increase activity.It is inorganic using organic flexible material as skeleton
Particle insertion is equivalent to ion conductor.Such structure has porous character, is advantageous to gas entrapment, reduces waving for inorganic particle
Hair, is advantageous to the raising of air-sensitive performance.
The content of the invention
For overcome the deficiencies in the prior art, present invention aims at：A kind of vulcanization of biomass carrying inorganic particle is provided
The preparation method of hydrogen sensing material.
Still a further object of the present invention is：Product prepared by the above method is provided.
Another object of the present invention is：The application of the said goods is provided.
The object of the invention is realized by following proposal：A kind of hydrogen sulfide gas sensing material of biomass carrying inorganic particle
Preparation method, comprise the following steps：
（1）The presoma of iron chloride and cobalt chloride is dissolved in magnetic agitation in deionized water and forms Fe3+And Co2+Homogeneous blend, obtain
To solution A；Sodium hydroxide is dissolved in stirring and dissolving in deionized water and obtains solution B；
（2）In step（1）In solution B be added dropwise in solution A, process do not stop stirring heating, obtain sediment centrifugation, cleaning
And collect dry after, in Muffle furnace biscuiting obtain CoFe2O4Nano-powder；
（3）Converted starch particle is dissolved in deionized water, glycerine is added after being completely dissolved and is continuously stirring to clearly, then adds step
Suddenly powder is well mixed after being dried in (2), then the film forming on spin coating instrument, and unnecessary moisture is 60~80oC is true, and evaporative air obtains
Obtain 100~200 μm of films.
The principle of the invention is：Biomass converted starch is soluble in water, film forming is mixed with inorganic particle, forms inorganic particle
Embedded organic film, its feature organic matter have loose structure, a large amount of captures of hydrogen sulfide gas can be achieved, then CoFe2O4
Carry out the gas-sensitive reaction of adsorption/desorption.The present invention can make flexible air-sensitive film, and method is simple to operate, and controllability is strong, for sulphur
Change hydrogen detection.
Wherein, step（1）It is described to be dissolved in water presoma and be replaced with ferric nitrate and cobalt nitrate, Fe3+Concentration be 0.5
~ 1.0 mol/l, Co:Fe=1:2；The concentration of sodium hydroxide is 2.0 mol/l.
Step（2）Described temperature is 90oC, reaction time 30min, mixing speed 300rpm, biscuiting are with 5oC/min
Programming rate is to 500oC, Temperature fall after being incubated 2~5 hours.
Step（3）Three kinds of described material mass ratios are converted starch：Glycerine：Nano-powder=（90~80）：5：（5~
15）.
The present invention provides a kind of hydrogen sulfide gas sensing material of biomass carrying inorganic particle, according to any of the above-described described
Method is prepared.
The present invention provides a kind of hydrogen sulfide gas sensing material of biomass carrying inorganic particle and detected in hydrogen sulfide gas
In application.
Obtained film is sticked on hexagonal earthenware air-sensitive testing element, using WS-30A type air-sensitive original paper test systems
Measure the response of gas.
The present invention is on the basis of being fully realized to gas sensing principle, it is proposed that is obtained using the technology with good
The film of good skeleton structure, and with the electric conductivity for keeping moisture to increase sensing powder, and then the sensitivity of gas sensitive is improved,
This method prepares that simple, controllability is strong, available for producing high-quality gas sensor.
Brief description of the drawings
Nano Co Fe prepared by Fig. 1 embodiments 12O4Stereoscan photograph；
The hydrogen sulfide air-sensitive performance of Fig. 2 embodiments 1.
Embodiment
Embodiment 1
Weigh respectively 0.05mol and 0.025mol iron chloride and cobalt chloride presoma be dissolved in 100ml deionized water with
300rpm is uniformly mixing to obtain solution A；The sodium hydroxide for continuing to weigh 0.2mol is dissolved in stirring and dissolving in 100ml deionized waters and obtained
To solution B;Solution B is added dropwise in solution A and does not stop to stir and be heated to 90oC reacts 30min, obtains CoFe2O4Precipitation
After thing is centrifuged, cleaned and collects drying, with 5oC/min is warming up to 500oC, the nano-powder of Temperature fall after 2h is incubated, sees Fig. 1
Nano Co Fe prepared by the present embodiment 12O4Stereoscan photograph.
Weigh 9g converted starch particles to be dissolved in deionized water, 0.5g glycerine added after being completely dissolved and is continuously stirring to clearly,
Add 0.5g CoFe2O4In organic solution, the then film forming on spin coating instrument, unnecessary moisture is 60oThe true evaporative airs of C
Obtain 100 μm of films.Obtained film is sticked on hexagonal earthenware air-sensitive testing element, surveyed using WS-30A type air-sensitives original paper
Test system measures the response of hydrogen sulfide gas, sees the hydrogen sulfide air-sensitive performance of Fig. 2 the present embodiment 1.
Embodiment 2
Weigh respectively 0.05mol and 0.025mol iron chloride and cobalt chloride presoma be dissolved in 100ml deionized water with
300rpm is uniformly mixing to obtain solution A；The sodium hydroxide for continuing to weigh 0.2mol is dissolved in stirring and dissolving in 100ml deionized waters and obtained
To solution B;Solution B is added dropwise in solution A and does not stop to stir and be heated to 90oC reacts 30min, obtains CoFe2O4Precipitation
After thing is centrifuged, cleaned and collects drying, with 5oC/min is warming up to 500oC, the nano-powder of Temperature fall after 5h is incubated, sees Fig. 1.
Weigh 9g converted starch particles to be dissolved in deionized water, 0.5g glycerine added after being completely dissolved and is continuously stirring to clearly,
Add 0.5g CoFe2O4In organic solution, the then film forming on spin coating instrument, unnecessary moisture is 80oThe true evaporative airs of C
Obtain 200 μm of films.Obtained film is sticked on hexagonal earthenware air-sensitive testing element, surveyed using WS-30A type air-sensitives original paper
Test system measures the response of hydrogen sulfide gas, and the material is 2.2 in the sensitivity of hydrogen sulfide gas.
Embodiment 3
Weigh respectively 0.1mol and 0.05mol iron chloride and cobalt chloride presoma be dissolved in 100ml deionized water with
300rpm is uniformly mixing to obtain solution A；The sodium hydroxide for continuing to weigh 0.45mol is dissolved in stirring and dissolving in 100ml deionized waters
Obtain solution B;Solution B is added dropwise in solution A and does not stop to stir and be heated to 90oC reacts 30min, obtains CoFe2O4It is heavy
After starch is centrifuged, cleaned and collects drying, with 5oC/min is warming up to 500oC, the nano-powder of Temperature fall after 3.5h is incubated, is seen
Fig. 1.
Weigh 8.5g converted starch particles to be dissolved in deionized water, 0.5g glycerine is added after being completely dissolved and is continuously stirring to
Clearly, 1g CoFe is added2O4In organic solution, the then film forming on spin coating instrument, unnecessary moisture is 70oThe true evaporative airs of C
Obtain 150 μm of films.Obtained film is sticked on hexagonal earthenware air-sensitive testing element, surveyed using WS-30A type air-sensitives original paper
Test system measures the response of hydrogen sulfide gas, and the material is 2.3 in the sensitivity of hydrogen sulfide gas.
Claims (6)
- A kind of 1. preparation method of the hydrogen sulfide gas sensing material of biomass carrying inorganic particle, it is characterised in that specific step It is rapid as follows：（1）The presoma of iron chloride and cobalt chloride is dissolved in magnetic agitation in deionized water and forms Fe3+And Co2+Homogeneous blend, obtain To solution A；Sodium hydroxide is dissolved in stirring and dissolving in deionized water and obtains solution B；（2）In step（1）In solution B be added dropwise in solution A, process do not stop stirring heating, obtain sediment centrifugation, cleaning And collect dry after, in Muffle furnace biscuiting obtain CoFe2O4Nano-powder；（3）Converted starch particle is dissolved in deionized water, glycerine is added after being completely dissolved and is continuously stirring to clearly, then adds step Suddenly powder is well mixed after being dried in (2), then the film forming on spin coating instrument, and unnecessary moisture is 60~80oC is true, and evaporative air obtains Obtain 100~200 μm of films.
- 2. the preparation method of the hydrogen sulfide gas sensing material of biomass carrying inorganic particle, its feature as described in claim 1 It is, step（1）It is described to be dissolved in water presoma and be replaced with ferric nitrate and cobalt nitrate, Fe3+Concentration be 0.5 ~ 1.0 Mol/l, Co:Fe=1:2；The concentration of sodium hydroxide is 2.0 mol/l.
- 3. the preparation method of the hydrogen sulfide gas sensing material of biomass carrying inorganic particle, its feature as described in claim 1 It is, step（2）Described temperature is 90oC, reaction time 30min, mixing speed 300rpm, biscuiting are with 5oC/min liters Temperature is to 500oC, it is incubated 2~5 hours Temperature falls.
- 4. the preparation method of the hydrogen sulfide gas sensing material of biomass carrying inorganic particle, its feature as described in claim 1 It is, step（3）Three kinds of described material mass ratios are converted starch：Glycerine：Nano-powder=（90~80）：5：（5~15）.
- 5. a kind of hydrogen sulfide gas sensing material of biomass carrying inorganic particle, it is characterised in that appointed according to claim 1-4 One methods described is prepared.
- 6. the hydrogen sulfide gas sensing material of biomass carrying inorganic particle detects in hydrogen sulfide gas according to claim 5 In application.
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| CN201711087041.9A CN107880318B (en) | 2017-11-07 | 2017-11-07 | Preparation method of biomass loaded inorganic particle hydrogen sulfide gas sensing material, product and application thereof |
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| CN201711087041.9A CN107880318B (en) | 2017-11-07 | 2017-11-07 | Preparation method of biomass loaded inorganic particle hydrogen sulfide gas sensing material, product and application thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104297318A (en) * | 2014-09-09 | 2015-01-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of network-structure nano-material for gas sensor |
| CN105985637A (en) * | 2015-02-09 | 2016-10-05 | 青岛蓝农谷农产品研究开发有限公司 | Manufacturing method of high-sensitivity stable gas sensitive sensor material |
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2017
- 2017-11-07 CN CN201711087041.9A patent/CN107880318B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104297318A (en) * | 2014-09-09 | 2015-01-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of network-structure nano-material for gas sensor |
| CN105985637A (en) * | 2015-02-09 | 2016-10-05 | 青岛蓝农谷农产品研究开发有限公司 | Manufacturing method of high-sensitivity stable gas sensitive sensor material |
Non-Patent Citations (3)
| Title |
|---|
| ANJALI B.BODADE等: "Conduction mechanism and gas sensing properties of CoFe2O4 nanocomposite thick films for H2S gas", 《TALANTA》 * |
| RAGHVENDRA SINGH YADAV等: "Structural, Cation Distribution, and Magnetic Properties of CoFe2O4 Spinel Ferrite Nanoparticles Synthesized Using a Starch-Assisted Sol–Gel Auto-Combustion Method", 《J SUPERCOND NOV MAGN》 * |
| 张小秋等: "基于纳米材料的气体传感器的研究进展", 《传感器与微系统》 * |
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