CN103149332B - Nano composite material for monitoring dimethyl ether - Google Patents
Nano composite material for monitoring dimethyl ether Download PDFInfo
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- CN103149332B CN103149332B CN201310067188.7A CN201310067188A CN103149332B CN 103149332 B CN103149332 B CN 103149332B CN 201310067188 A CN201310067188 A CN 201310067188A CN 103149332 B CN103149332 B CN 103149332B
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- yttrium
- dimethyl ether
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- hours
- salt
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Abstract
The invention relates to a nano composite material for monitoring dimethyl ether in air, which is a Y2O3-MnO2-Al2O3 nano powder prepared from yttrium salt, manganese salt and aluminum salt by a sol-gel technique. The nano powder comprises the following components in percentage by mass: 22-36% of Y2O3, 18-33% of MnO2 and 30-45% of Al2O3. The particle size of the nano powder is 20-45 nm. The dimethyl ether sensor prepared from the nano composite material provided by the invention has the advantages of wide linear range, favorable selectivity and high sensitivity, and can be used for monitoring the dimethyl ether content in air on line without being influenced by coexistent substances.
Description
Technical field
The present invention relates to a kind of nano composite material for monitoring dimethyl ether in air, especially by Y
2o
3, MnO
2and Al
2o
3the nano composite oxide sensitive material of composition.Belong to field of sensing technologies.
Background technology
Dimethyl ether (Dimethyl ether, DME) is a kind of colourless gas at normal temperatures and pressures, is the homolog of ether, there is slight ether fragrance, there is inhibiting effect to people's central nervous system, anesthesia and sensation of asphyxia can be caused after suction, to the irritant effect of skin.Dimethyl ether belongs to fire goods, produces explosive mixture (volumetric concentration is about 3%-17%) with air mixing energy, and chance naked light and high heat energy cause combustion explosion, and easily liquefy during dimethyl ether pressurization, the steam pressure under room temperature is about 0.5MPa.Dimethyl ether is considered to desirable Alternative Diesel Fuel and potential generating and domestic fuel, is a kind of important ultra-clean energy and environmental friendly product.When current oil fuel is in short supply; the oil replacement industries such as coal-based alcohol ether fuel such as develop actively dimethyl ether; be important measures of contradiction of alleviating rapidly that oil is in short supply, the production of dimethyl ether and application and development have extremely important meaning to development China's derived energy chemical and environmental protection.In order to the enforcement of advance oil substituted pesticides; in July, 2006; National Development and Reform Committee has held dimethyl ether industry development forum in Beijing; point out that dimethyl ether is the substitute energy product with better development prospect; it is the alternative fuel being suitable for China's energy structure; dimethyl ether industry will walk the road for development of scale, maximization, is specification dimethyl ether manufacture and usage, promptly should works out relevant criterion.Along with rising steadily of liquefied petroleum gas (LPG) price, dimethyl ether, separately as the domestic fuel of new cleaning fuel or be mixed into hybrid fuel with liquefied petroleum gas (LPG), comes into the market in a large number.But because the rubber seal of dimethyl ether to liquefied petroleum gas steel cylinder has swelling action, fill doping for a long time and may cause cylinder valve and kitchen range gas leakage, Long-Time Service easily sets off an explosion, and has had a strong impact on the person and the property safety of consumer.At present, in China's liquefied petroleum gas (LPG) national standard, not yet formulate index and the detection method of dimethyl ether content, therefore, set up dimethyl ether detection method in combination gas significant.
The assay method of dimethyl ether is a lot, and wherein vapor-phase chromatography precision is high, detection is accurate, and application at most.Such as, Zhao Li delivered and was entitled as the article of the mensuration of dimethyl ether content " in the liquefied petroleum gas (LPG) " in " industrial technology " in September, 2012, in June, 2012, a Lv Wen Ji delivered the article being entitled as " in capillary gas chromatography analytic liquid liquefied oil gas dimethyl ether content " on " Guangdong chemical industry ", in May, 2011, Li Dong just delivered the article being entitled as " in capillary gas chromatography analytic liquid liquefied oil gas dimethyl ether " in " chemical analysis metering ", more than in Dec, 2010, Deqing has been delivered and has been entitled as " in liquefied petroleum gas (LPG) the research of dimethyl ether detection method of content " on " printing during chemical industry ", etc..These methods are all based on gas chromatography, and major defect is that analytical procedure is complicated, length consuming time, and needs expensive instrument and equipment.
The fast development of gas sensing techniques is that the various pollutants detected fast in air provide possibility, especially be that the gas sensor of sensitive material is widely applied with metal oxide, report in document in a large number for detecting sensitive material of a lot of gas such as methane, ethane, propane, alcohol, formaldehyde, carbon monoxide, carbon dioxide, ethene, acetylene, styrene, acrylic acid and preparation method thereof, but then reported seldom for the sensitive material detecting dimethyl ether.
Summary of the invention
The object of this invention is to provide a kind of nano composite material for monitoring dimethyl ether in air and preparation method thereof.The sensor of dimethyl ether in the monitoring air made of this material, can micro-dimethyl ether at the scene fast, in Accurate Determining air and not by the impact of other common mutual interference material.
Nano composite material of the present invention is by Y
2o
3, MnO
2and Al
2o
3nano-powder forms, and adopt sol-gal process preparation, concrete grammar is:
By yttrium salt, manganese salt, aluminium salt and tartrate are dissolved in the aqueous solution of watery hydrochloric acid altogether, sonic oscillation is to clear, under high-speed stirred state, slowly drip weak aqua ammonia to solution ph is 3.5-4.2, continue stirring after 8 hours, still aging more than 12 hours, solution rotary evaporation at 74-78 DEG C is obtained gel, by gel infra-red drying 1-2 hour, after abundant grinding, 350 DEG C are warming up to the speed being no more than 7 DEG C per minute in high temperature box type resistance furnace, keep this temperature 2 hours, 480 DEG C are warming up to again with the speed being no more than 3 DEG C per minute, keep this temperature 2 hours, naturally cooling obtains Y
2o
3, MnO
2and Al
2o
3nano-powder.
Wherein, yttrium salt is acetic acid yttrium, yttrium oxalate, yttrium nitrate, yttrium sulfate, yttrium phosphate, the anhydride of yttrium chloride or the potpourri of one or more of hydrate, manganese salt is the anhydride of manganese acetate, manganese sulfate, manganese chloride, manganese nitrate and Manganese perchlorate or the potpourri of one or more of hydrate, and aluminium salt is aluminium nitrate, aluminium sulphate, aluminum perchlorate, aluminum phosphate, aluminum chloride, aluminum acetate, aluminium isopropoxide and the anhydride of aluminium secondary butylate or the potpourri of one or more of hydrate.
Obtained nano-powder transmissioning electric mirror test, when the particle size range of nano-powder is 20-45nm, and the mass percent of each component meets Y
2o
3(22-36%), MnO
2(18-33%) and Al
2o
3(30-45%) time, for there is very high sensitivity and selectivity as the sensitive material of dimethyl ether in monitoring air.
Tool of the present invention has the following advantages:
(1) preparation process is simple, reproducible;
(2) excitable material pellet growth evenly, particle size distribution range less (25 ~ 45nm);
(4) the dimethyl ether sensor made with prepared sensitive material is still very stable after using 80 hours continuously;
(5) sensitive material prepared by has good selectivity to dimethyl ether, the common concurrent not interference measurement in air.
Accompanying drawing explanation
Fig. 1 is a kind of Y
2o
3, MnO
2and Al
2o
3transmission electron microscope (TEM) figure of nano-powder.
Embodiment
Embodiment 1
By four water acetic acid yttriums, tetrahydrate manganese chloride, nine water aluminium nitrates and tartrate are dissolved in the aqueous solution of watery hydrochloric acid altogether, sonic oscillation is to clear, under high-speed stirred state, slowly drip weak aqua ammonia to solution ph is 3.55, continue stirring after 8 hours, still aging 15 hours, solution rotary evaporation at 74.5 DEG C is obtained gel, by gel infra-red drying 1 hour, after abundant grinding, 350 DEG C are warming up to the speed being no more than 7 DEG C per minute in high temperature box type resistance furnace, keep this temperature 2 hours, 480 DEG C are warming up to again with the speed being no more than 3 DEG C per minute, keep this temperature 2 hours, naturally cooling obtains Y
2o
3, MnO
2and Al
2o
3nano-powder.
Analyze: with this powder body material of transmissioning electric mirror test, its particle size range is 25-35nm, and mean grain size is about 30nm; Carry out constituent analysis to it, recording its composition (mass percent) is 25.5%Y
2o
3, 30.3%MnO
2and 44.2%Al
2o
3.
Application: measure the dimethyl ether in air using this powder body material as sensitive material, the range of linearity 5 ~ 68mg/m
3, detection limit can reach 2.8mg/m
3, concurrent does not disturb.
Embodiment 2
By yttrium phosphate, manganese sulfate, aluminium isopropoxide and tartrate are dissolved in the aqueous solution of watery hydrochloric acid altogether, sonic oscillation is to clear, under high-speed stirred state, slowly drip weak aqua ammonia to solution ph is 3.7, continue stirring after 8 hours, still aging 12 hours, solution rotary evaporation at 75 DEG C is obtained gel, by gel infra-red drying 1.5 hours, after abundant grinding, 350 DEG C are warming up to the speed being no more than 7 DEG C per minute in high temperature box type resistance furnace, keep this temperature 2 hours, 480 DEG C are warming up to again with the speed being no more than 3 DEG C per minute, keep this temperature 2 hours, naturally cooling obtains Y
2o
3, MnO
2and Al
2o
3nano-powder.Analyze: with this powder body material of transmissioning electric mirror test, its particle size range is 35-45nm, and mean grain size is about 40nm; Carry out constituent analysis to it, recording its composition (mass percent) is 29.8%Y
2o
3, 27.7%MnO
2and 42.5%Al
2o
3.
Application: measure the dimethyl ether in air using this powder body material as sensitive material, the range of linearity 4 ~ 70mg/m
3, detection limit can reach 2.5mg/m
3, concurrent does not disturb.
Embodiment 3
By nine water yttrium oxalate, six water yttrium nitrates, six water manganese nitrates, perchlorate hexahydrate's manganese, aluminum sulfate octadecahydrate, nine water aluminum perchlorates and tartrate are dissolved in the aqueous solution of watery hydrochloric acid altogether, sonic oscillation is to clear, under high-speed stirred state, slowly drip weak aqua ammonia to solution ph is 3.8, continue stirring after 8 hours, still aging 18 hours, solution rotary evaporation at 76 DEG C is obtained gel, by gel infra-red drying 2 hours, after abundant grinding, 350 DEG C are warming up to the speed being no more than 7 DEG C per minute in high temperature box type resistance furnace, keep this temperature 2 hours, 480 DEG C are warming up to again with the speed being no more than 3 DEG C per minute, keep this temperature 2 hours, naturally cooling obtains Y
2o
3, MnO
2and Al
2o
3nano-powder.
Analyze: with this powder body material of transmissioning electric mirror test, its particle size range is 25-35nm, and mean grain size is about 30nm; Carry out constituent analysis to it, recording its composition (mass percent) is 31.1%Y
2o
3, 30.0%MnO
2and 38.9%Al
2o
3.
Application: measure the dimethyl ether in air using this powder body material as sensitive material, the range of linearity 5 ~ 77mg/m
3, detection limit can reach 2.8mg/m
3, concurrent does not disturb.
Embodiment 4
By six water yttrium chlorides, acetate dihydrate manganese, Aluminum Chloride Hexahydrate, two hydration aluminum acetates, aluminium secondary butylate and tartrate are dissolved in the aqueous solution of watery hydrochloric acid altogether, sonic oscillation is to clear, under high-speed stirred state, slowly drip weak aqua ammonia to solution ph is 4.15, continue stirring after 8 hours, still aging 20 hours, solution rotary evaporation at 77 DEG C is obtained gel, by gel infra-red drying 1 hour, after abundant grinding, 350 DEG C are warming up to the speed being no more than 7 DEG C per minute in high temperature box type resistance furnace, keep this temperature 2 hours, 480 DEG C are warming up to again with the speed being no more than 3 DEG C per minute, keep this temperature 2 hours, naturally cooling obtains Y
2o
3, MnO
2and Al
2o
3nano-powder.
Analyze: with this powder body material of transmissioning electric mirror test, its particle size range is 25-45nm, and mean grain size is about 33nm; Carry out constituent analysis to it, recording its composition (mass percent) is 35.5%Y
2o
3, 31.8%MnO
2and 32.7%Al
2o
3.
Application: measure the dimethyl ether in air using this powder body material as sensitive material, the range of linearity 4 ~ 65mg/m
3, detection limit can reach 2.4mg/m
3, concurrent does not disturb.
Embodiment 5
By eight water yttrium sulfates, tetrahydrate manganese chloride, six water manganese nitrates, hypophosphite monohydrate aluminium, Aluminum Chloride Hexahydrate and tartrate are dissolved in the aqueous solution of watery hydrochloric acid altogether, sonic oscillation is to clear, under high-speed stirred state, slowly drip weak aqua ammonia to solution ph is 4.0, continue stirring after 8 hours, still aging 13 hours, solution rotary evaporation at 77.5 DEG C is obtained gel, by gel infra-red drying 1.5 hours, after abundant grinding, 350 DEG C are warming up to the speed being no more than 7 DEG C per minute in high temperature box type resistance furnace, keep this temperature 2 hours, 480 DEG C are warming up to again with the speed being no more than 3 DEG C per minute, keep this temperature 2 hours, naturally cooling obtains Y
2o
3, MnO
2and Al
2o
3nano-powder.
Analyze: with this powder body material of transmissioning electric mirror test, its particle size range is 30-40nm, and mean grain size is about 35nm; Carry out constituent analysis to it, recording its composition (mass percent) is 22.9%Y
2o
3, 32.8%MnO
2and 44.3%Al
2o
3.
Application: measure the dimethyl ether in air using this powder body material as sensitive material, the range of linearity 8 ~ 98mg/m
3, detection limit can reach 3.8mg/m
3, concurrent does not disturb.
Claims (2)
1., for monitoring a nano composite material for dimethyl ether, it is characterized in that by Y
2o
3, MnO
2and Al
2o
3nano-powder forms, and wherein the mass percent scope of each component is 22-36%Y
2o
3, 18-33%MnO
2and 30-45%Al
2o
3, its preparation method is: by yttrium salt, manganese salt, aluminium salt and tartrate are dissolved in the aqueous solution of watery hydrochloric acid altogether, sonic oscillation is to clear, under high-speed stirred state, slowly drip weak aqua ammonia to solution ph is 3.5-4.2, continue stirring after 8 hours, still aging more than 12 hours, solution rotary evaporation at 74-78 DEG C is obtained gel, by gel infra-red drying 1-2 hour, after abundant grinding, 350 DEG C are warming up to the speed being no more than 7 DEG C per minute in high temperature box type resistance furnace, keep this temperature 2 hours, 480 DEG C are warming up to again with the speed being no more than 3 DEG C per minute, keep this temperature 2 hours, naturally cooling obtains Y
2o
3, MnO
2and Al
2o
3nano-powder, the particle size range of nano-powder is 20-45nm.
2. a kind of nano composite material for monitoring dimethyl ether according to claim 1, it is characterized in that described yttrium salt is acetic acid yttrium, yttrium oxalate, yttrium nitrate, yttrium sulfate, yttrium phosphate, the anhydride of yttrium chloride or the potpourri of one or more of hydrate, manganese salt is manganese acetate, manganese sulfate, manganese chloride, the anhydride of manganese nitrate and Manganese perchlorate or the potpourri of one or more of hydrate, aluminium salt is aluminium nitrate, aluminium sulphate, aluminum perchlorate, aluminum phosphate, aluminum chloride, aluminum acetate, the anhydride of aluminium isopropoxide and aluminium secondary butylate or the potpourri of one or more of hydrate.
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|---|---|---|---|
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|---|---|---|---|
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101887057A (en) * | 2010-06-30 | 2010-11-17 | 北京联合大学生物化学工程学院 | Nano sensitive material of carbamic acid ester pesticides |
| CN102175815A (en) * | 2010-12-07 | 2011-09-07 | 北京联合大学生物化学工程学院 | Nano-sensitive material for monitoring sulfur dioxide |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2002952384A0 (en) * | 2002-10-31 | 2002-11-14 | Swinburne University Of Technology | Structures |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101887057A (en) * | 2010-06-30 | 2010-11-17 | 北京联合大学生物化学工程学院 | Nano sensitive material of carbamic acid ester pesticides |
| CN102175815A (en) * | 2010-12-07 | 2011-09-07 | 北京联合大学生物化学工程学院 | Nano-sensitive material for monitoring sulfur dioxide |
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