CN103833511B - The preparation method of 2,3,3,3-tetrafluoeopropene - Google Patents
The preparation method of 2,3,3,3-tetrafluoeopropene Download PDFInfo
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Abstract
The invention provides a kind of preparation method of 2,3,3,3-tetrafluoeopropene.The method with the difluorochloromethane of mol ratio 0.5-4:1 and monochloro methane for reaction raw materials, superheated vapour and reaction raw materials volume ratio are 1-20:1, superheated vapour temperature 900-1100 DEG C, mixes with superheated vapour after reaction raw materials preheating, and conversion zone temperature is at 600-1100 DEG C; Reactant is 0.01-1s in the conversion zone residence time; Product mixed flow obtains 2,3,3,3-tetrafluoeopropene through chilling, deacidification, drying, rectifying separation.Instant invention overcomes the defect that hollow tube Pintsch process easily ties carbon, side reaction complexity, reduce maintenance of equipment rate, extend reaction time simultaneously, improve utilization ratio of device.Method of the present invention has the features such as raw material is easy to get, reaction process is simple, and gained 2,3,3,3-tetrafluoeopropene has the advantage of zero odp, low GWP, as the substitute of car air conditioner refrigerant.
Description
Technical field
The present invention relates to a kind of preparation method of HF hydrocarbon, particularly relating to is the preparation method of 2,3,3,3-tetrafluoeopropene (HFO-1234yf).
Technical background
" Montreal Agreement book " has determined the superseded timetable of HCFCs, along with eliminating of HCFCs, the third generation is containing the substitute of fluorinated refrigerant HFCs as HCFCs, more and more paid close attention to by people, but in numerous HFCs substitute, depletion of the ozone layer is made to dive value (namely ODP is zero) although all have, destruction is not had to ozonosphere, but many HFCs have the latent value of higher Greenhouse effect, such as 1, 1, 1, 2-Tetrafluoroethane (HFC-134a) has zero odp, but its GWP is up to 1300, along with Greenhouse effect are more and more serious, people also pay attention to more to environmental problem, the GWP value of all new car refrigeration agents of its member states of European Union requirements can not more than 150, Given this Kyoto Protocol lists greenhouse gases, the novel refrigerant for automative air conditioning exploitation with slowing global warming phenomenon potential quality is quite concerned by people.2,3,3,3-tetrafluoeopropene (HFO-1234yf) not only has zero odp, and its GWP value only has 4, so become the focus that people pay close attention to, and becomes key point about 2,3,3,3-tetrafluoeopropenes (HFO-1234yf) preparation method.
The MarquisdavidM of Du Pont delivered 2 in 1964,3,3, preparation (the Preparationof2 of 3-tetrafluoeopropene, 3,3,3-tetrafluopropene [p]) CA690037.1964-07-07, U.S. Patent number is that the patent document of 2931840 is also openly about 2, the preparation method of 3,3,3-tetrafluoeopropene, what they all adopted is monochloro methane and tetrafluoroethylene or monochloro methane and difluorochloromethane are raw material, and under catalyst-free condition, Pintsch process prepares target product.Because the temperature of reaction of the method is up to more than 900 DEG C, so side reaction is more, and produce serious knot carbon phenomenon, so need regularly dredging reaction pipeline, with short production cycle, efficiency is low, and the productive rate of the method only has 13%, produce so be difficult to industrialization.Since entering 21 century, Du Pont and Honeywell affiliated company again with HFC-245eb, HFC-215cb, HFC-225cb, HFC-235cb, HFC-245cb etc. for HFC-1234yf(2 prepared by raw material, 3,3,3-tetrafluoeopropene), its weak point is that aftertreatment separating mixture is comparatively complicated.
Summary of the invention
For the deficiency existing for prior art Pintsch process, the invention provides that a kind of transformation efficiency is high, aftertreatment is easy, the preparation method of lower-cost 2,3,3,3-tetrafluoeopropenes.
Technical solution of the present invention is as follows:
A kind of preparation method of 2,3,3,3-tetrafluoeopropene, comprises step as follows:
(1) heat the temperature of reaction kettle filling water and make liquid water vaporizes to 100-200 DEG C, the water vapor after gasification enters into superheat section, makes vapor temperature rise to 900-1000 DEG C.The amount of steam is controlled by mass flowmeter.
(2) by difluorochloromethane: monochloro methane=0.5-4:1 mol ratio, in mixing vessel, filling reaction raw materials difluorochloromethane and monochloro methane, control the quality of charging feedstock by electronic scales.
(3) by the reaction raw materials preheating 200-400 DEG C of step (2), then reactor is entered into after mixing with step (1) superheated vapour, described superheated vapour and reaction raw materials volume ratio are 1-20:1, temperature of reaction controls at 600-1000 DEG C, and reactant reaction intraductal retention time is in the reactor 0.01-0.4s.
(4) the product mixed flow flowed out from reaction tubes is passed in the chilling chuck kettle device of circulating water condensing, and the product stream after chilling is passed into and fills in the deacidification device of alkali lye, then obtains dried product mixtures by drying installation.
(5) product mixtures of step (4) gained is passed in rectifying tower, is separated by prior art and obtains 2,3,3,3-tetrafluoeopropene.
According to the present invention, preferably, in step (1), heating fills the temperature of reaction kettle of water to 120-160 DEG C.Fill the preferred 1-5 kilogram of reactor pressure of water, further preferred 2-3 kilogram.The heating kettle be filled with water should be connected with pressure regulator.Water type of heating adopts heat-conducting oil heating mode.
According to the present invention, preferably, in step (1), the water vapor after gasification adopts diamond heating mode to obtain the superheated vapour of 900-1000 DEG C at superheat section.
Preferred according to the present invention, in step (2), two kinds of reaction raw materials difluorochloromethanes and monochloro methane mol ratio are 1 ~ 3:1, most preferably are 1 ~ 2:1.
According to the present invention, preferably, in step (3), described temperature of reaction is 700-900 DEG C.
According to the present invention, preferably, in step (3), reaction pressure is normal pressure or carries out slightly larger than under normal pressure, and reaction pressure is 0.1 ~ 0.5MPa preferably.The excessive easy generation autohemagglutination of pressure or mixed poly-.
According to the present invention, preferably, in step (3), the temperature survey of superheated vapour adopts thermocouple thermometer.
According to the present invention, preferably, in step (4), the alkali lye for deacidification device is the sodium hydroxide solution of massfraction 20%-60%.
According to the present invention, preferably, in step (4), the alkali lye device for deacidification device is secondary device, can realize the object of secondary alkali cleaning.
In above-mentioned steps of the present invention (4), mixture liquid samples after drying, adopts gc analysis mixture composition; Wherein the massfraction of 2,3,3,3-tetrafluoeopropenes (HFO-1234yf) is 25 ~ 55%.
The present invention's reaction raw materials used is commercial.Reaction unit is prior art.
The present invention's reaction unit material used is high corrosion resistance, and does not react with reaction raw materials difluorochloromethane or monochloro methane, is selected from palladium metal, silver or high-carbon steel material, in view of consideration cost, and the present invention's preferred SUS316 material tubular reactor.The stainless steel tubular reactor of described SUS316 is placed in vitrified pipe, looping resistance wire outside vitrified pipe, with the insulation of pure aluminium silicate insulating cotton, temperature required by being with the Resistant heating of temperature controller and thermopair to control reaction.
Technical characterstic of the present invention and excellent results:
1. the present invention's reaction raw materials used is all commercially available, and reaction raw materials cost is lower, concrete reaction mechanism is that difluorochloromethane pyrolysis obtains difluorocarbene, two molecule difluorocarbenes are combined into an one's share of expenses for a joint undertaking tetrafluoroethylene, monochloro methane cracking obtains Cabbeen, and reactive intermediate Cabbeen is combined with tetrafluoroethylene thus obtains target product 2,3,3,3-tetrafluoeopropene.
2. the present invention is raw materials used is the front mixture of reaction, and the two all exists with gas phase in the mixing container, ensure that the volume ratio of charging accurately controls.Two kinds of reaction raw materials difluorochloromethanes and monochloro methane amount are than being 0.5-4:1, and the excessive one side of difluorochloromethane amount causes the waste of reaction raw materials, and target product productive rate also decreases on the other hand.In the present invention, two kinds of reactant residence time in reaction pipeline are 0.01-1s, overstand, although two kinds of reaction-ure conversion-ages increase, but easily cause side reaction to occur, target product productive rate reduces, the residence time is too short, and two kinds of reactant collision probabilities reduce, and target product productive rate also can be caused to reduce.
3. the generation of superheated vapour of the present invention is the extremely boiling of first heating water, and enter into superheated vapour generation device in vapour form, this device type of heating is diamond heating, until temperature reaches 900-1000 DEG C, thus produces superheated vapour.
4. the present invention adopts steam dilution cracking, reduce the probability that side reaction occurs, namely the generation of highly toxic substance perfluoroisobutylene is avoided, and greatly suppress to finish carbon phenomenon, superheated vapour is as the carrier of heat simultaneously, transfer of heat is played the effect of heating two kinds of reaction raw materials difluorochloromethanes and monochloro methane to reactant.
5, reaction pressure of the present invention is carried out at normal pressure or slightly larger than under condition of normal pressure, the excessive generation impelling autohemagglutination or mixed poly-reaction of reaction pressure, thus can not get target product.
6, reaction of the present invention, by from reaction unit out after mixture of reaction products import in the chilling chuck kettle device of circulating water condensing at once, avoid the generation of secondary reaction, the quenching apparatus that the present invention preferably adopts is the chilling chuck still having circulating water condensing, product mixed flow after chilling enters into the deacidification device filling alkali lye, through secondary alkali cleaning, thus reach the object that deacidifies more thoroughly, then be passed in drying installation product mixtures is carried out drying treatment adopt gas-chromatography carry out analysis of mixtures composition, 2, 3, 3, 3-tetrafluoeopropene (HFO-1234yf) can pass through rectifier unit from the separation method mixture, thus by 2, 3, 3, 3-tetrafluoeopropene (HFO-1234yf) is isolated from mixture, obtain purity higher 2, 3, 3, 3-tetrafluoeopropene (HFO-1234yf) product.
Preparation method provided by the invention in reaction process without the need to catalyzer, adopt superheated vapour dilution cracking suppress to finish carbon phenomenon generation, avoid continuous seepage cycle short defect, thus decrease the maintenance of device, improve device service efficiency.In addition the present invention's reaction raw materials used is easy to get and commercially available price is lower, thus the cost also making this route prepare target product reduces greatly.Present invention optimizes the proportioning of raw material, steam dilution cracking, also reduce the probability that side reaction occurs, thus avoid the generation of highly toxic substance perfluoroisobutylene, avoid finishing the phenomenon that carbon easily causes device to block.
2,3,3,3-tetrafluoeopropenes obtained by the present invention have the advantage of zero odp, low GWP, can be used as whipping agent, heat-transfer medium, propelling agent etc., especially can be used as the ideal substitute of car air conditioner refrigerant.
Embodiment
Below in conjunction with embodiment, the present invention is described further, it should be noted that, following embodiment be only for illustration of, and not for limiting the present invention.The various changes that those skilled in the art's derivation according to the present invention is made all should within the protection domain required by the application's claim.In embodiment, reaction unit used is this area conventional equipment, and reaction raw materials used is commercial products.
Embodiment 1:
A kind of preparation method of 2,3,3,3-tetrafluoeopropene, with difluorochloromethane (R
22) and monochloro methane (methyl chloride) be raw material, under superheated vapour diluting condition, there is scission reaction obtain 2,3,3,3-tetrafluoeopropene.Chemical equation is as follows:
2CHClF
2+CH
3Cl→CF
3CF=CH
2+3HCl
Be be filled with 16.8g monochloro methane, 86.5g difluorochloromethane in the steel cylinder of 8L to volume
To being add pure water 6000g in the jacketed type reactor of 10L with thermometer, tensimeter, reducing valve volume, heat conduction silicone oil is housed in cutting ferrule, and be connected with circulating oil pump, arranging circulating oil pump temperature is 130 DEG C, make jacket reactor be connected thermometer registration produce water vapor be passed in tube furnace, wherein tube furnace temperature is set to 1000 DEG C, thus produces superheated vapour.
The steel cylinder holding two kinds of reaction raw materials connects preheating apparatus, and controlling pre-heating temperature is 350 DEG C, and two kinds of reaction raw materials after preheating enter into reaction unit with superheated vapour after mixing section mixes.
The reaction tubes of reaction unit is internal diameter is 4mm, the long stainless steel tubular reactor of SUS316 for 100cm, this tubular reactor is placed in vitrified pipe, looping resistance wire outside vitrified pipe, carry out boosting if desired, be incubated by pure aluminium silicate insulating cotton, by being with Resistant heating and the thermocouple measurement pipe reaction actuator temperature of temperature controller, control temperature is at 700 DEG C.
Reaction unit first passes into superheated vapour and preheats reaction tubes, reaction tubes connects thermometer registration when being stabilized in 700 DEG C, regulate the volumetric flow meter flow 235.2ml/s that water vapor pipeline connects, reaction raw materials connection traffic meter flow is regulated to be 15.7ml/s, reaction product mixed flow enters quenching apparatus, secondary alkaline cleaner, drying installation after reaction tubes flows out, and the amount for the water of product mixed flow chilling is enough.Collect dry rear products therefrom stream, in gas chromatographic analysis mix products, 2,3,3,3-tetrafluoeopropene massfractions are 38.5%.The mix products of gained is passed in rectifying tower, is separated by prior art and obtains 2,3,3,3-tetrafluoeopropene.
Embodiment 2: as described in Example 1, difference is:
Reaction unit first passes into superheated vapour and preheats reaction pipeline, reaction pipeline connects thermometer registration when being stabilized in 700 DEG C, regulate the volumetric flow meter flow 209.2ml/s that water vapor pipeline connects, reaction raw materials connection traffic meter flow is regulated to be 41.8ml/s, reaction product mixed flow enters quenching apparatus, secondary alkaline cleaner, drying installation after reaction tubes flows out, collect dry rear products therefrom stream, in gas chromatographic analysis mix products 2,3,3,3-tetrafluoeopropene massfraction is 42.5%.
Embodiment 3: as described in Example 1, difference is:
Reaction unit first passes into superheated vapour and preheats reaction pipeline, reaction pipeline connects thermometer registration when being stabilized in 700 DEG C, regulate the volumetric flow meter flow 225.9ml/s that water vapor pipeline connects, reaction raw materials connection traffic meter flow is regulated to be 25.1ml/s, reaction product mixed flow enters quenching apparatus, secondary alkaline cleaner, drying installation after reaction tubes flows out, collect dry rear products therefrom stream, in gas chromatographic analysis mix products 2,3,3,3-tetrafluoeopropene massfraction is 45.9%.
Embodiment 4: as described in Example 1, difference is:
Reaction unit first passes into superheated vapour and preheats reaction pipeline, reaction pipeline connects thermometer registration when being stabilized in 700 DEG C, regulate the volumetric flow meter flow 125.5ml/s that water vapor pipeline connects, reaction raw materials connection traffic meter flow is regulated to be 125.5ml/s, reaction product mixed flow enters quenching apparatus, secondary alkaline cleaner, drying installation after reaction tubes flows out, collect dry rear products therefrom stream, in gas chromatographic analysis mix products 2,3,3,3-tetrafluoeopropene massfraction is 25.9%.
Embodiment 5: as described in Example 1, difference is:
Reaction unit first passes into superheated vapour and preheats reaction pipeline, reaction pipeline connects thermometer registration when being stabilized in 700 DEG C, regulate the volumetric flow meter flow 52.3ml/s that water vapor pipeline connects, reaction raw materials connection traffic meter flow is regulated to be 10.5ml/s, reaction product mixed flow enters quenching apparatus, secondary alkaline cleaner, drying installation after reaction tubes flows out, collect dry rear products therefrom stream, in gas chromatographic analysis mix products 2,3,3,3-tetrafluoeopropene massfraction is 49.6%.
Embodiment 6: as described in Example 1, difference is:
Reaction unit first passes into superheated vapour and preheats reaction pipeline, reaction pipeline connects thermometer registration when being stabilized in 700 DEG C, regulate the volumetric flow meter flow 13.1ml/s that water vapor pipeline connects, reaction raw materials connection traffic meter flow is regulated to be 2.6ml/s, reaction product mixed flow enters quenching apparatus, secondary alkaline cleaner, drying installation after reaction tubes flows out, collect dry rear products therefrom stream, in gas chromatographic analysis mix products 2,3,3,3-tetrafluoeopropene massfraction is 41.3%.
Comprehensive Correlation embodiment 1,2,3,4 finds that water vapor ratio excessive target product productive rate is not high, and the dividing potential drop of water vapor increases on the one hand, and two kinds of reactant partial pressure are less, reactant molecule collision probability reduces, cause target product productive rate not high, on the other hand, too high water vapor ratio, the water vapor consumed is too much, uneconomical from cost consideration, steam dilution ratio is too small, and the probability that side reaction occurs increases, and have knot carbon phenomenon, thus cause target product productive rate not high.
Comprehensive Correlation embodiment 2,5,6, the difference of rate of flow of fluid i.e. the difference of the residence time in pipeline, also be influential to target product productive rate, steam and reaction raw materials flow velocity excessive namely reaction pipeline in the reaction times too short, between reactant molecule, collision probability is little, the amount of gained target product also reduces, otherwise, steam and the too small i.e. raw material of reaction raw materials flow velocity overstand in reaction pipeline, target product productive rate is caused to reduce, its reason is that the probability that overstand side reaction occurs increases, and autohemagglutination or mixed poly-phenomenon easily occur.
Embodiment 7: as described in Example 1, difference is:
Reaction unit first passes into superheated vapour and preheats reaction pipeline, reaction pipeline connects thermometer registration when being stabilized in 600 DEG C, regulate the volumetric flow meter flow 52.3ml/s that water vapor pipeline connects, reaction raw materials connection traffic meter flow is regulated to be 10.5ml/s, reaction product mixed flow enters quenching apparatus, secondary alkaline cleaner, drying installation after reaction tubes flows out, collect dry rear products therefrom stream, in gas chromatographic analysis mix products 2,3,3,3-tetrafluoeopropene massfraction is 45.3%.
Embodiment 8: as described in Example 1, difference is:
Reaction unit first passes into superheated vapour and preheats reaction pipeline, reaction pipeline connects thermometer registration when being stabilized in 800 DEG C, regulate the volumetric flow meter flow 52.3ml/s that water vapor pipeline connects, reaction raw materials connection traffic meter flow is regulated to be 10.5ml/s, reaction product mixed flow enters quenching apparatus, secondary alkaline cleaner, drying installation after reaction tubes flows out, collect dry rear products therefrom stream, in gas chromatographic analysis mix products 2,3,3,3-tetrafluoeopropene massfraction is 46.1%.
Comprehensive Correlation embodiment 5,7,8, the difference of reaction tubes temperature of reaction, slightly affects target product productive rate.
Embodiment 9: as described in Example 1, difference is:
Be be filled with 50.5g monochloro methane, 86.5g difluorochloromethane in the steel cylinder of 8L to volume.
Reaction unit first passes into superheated vapour and preheats reaction pipeline, reaction pipeline connects thermometer registration when being stabilized in 700 DEG C, regulate the volumetric flow meter flow 52.3ml/s that water vapor pipeline connects, reaction raw materials connection traffic meter flow is regulated to be 10.5ml/s, reaction product mixed flow enters quenching apparatus, secondary alkaline cleaner, drying installation after reaction tubes flows out, collect dry rear products therefrom stream, in gas chromatographic analysis mix products 2,3,3,3-tetrafluoeopropene massfraction is 54.3%.
Embodiment 10: as described in Example 1, difference is:
Be be filled with 50.5g monochloro methane, 43.25g difluorochloromethane in the steel cylinder of 8L to volume.
Reaction unit first passes into superheated vapour and preheats reaction pipeline, reaction pipeline connects thermometer registration when being stabilized in 700 DEG C, regulate the volumetric flow meter flow 52.3ml/s that water vapor pipeline connects, reaction raw materials connection traffic meter flow is regulated to be 10.5ml/s, reaction product mixed flow enters quenching apparatus, secondary alkaline cleaner, drying installation after reaction tubes flows out, collect dry rear products therefrom stream, in gas chromatographic analysis mix products 2,3,3,3-tetrafluoeopropene massfraction is 48.5%.
Comprehensive Correlation embodiment 5,9,10, the difference of reaction raw materials proportioning, has impact to target product productive rate.
Claims (11)
1. the preparation method of a tetrafluoeopropene, comprises step as follows:
(1) heat the temperature of reaction kettle filling water and make liquid water vaporizes to 100-200 DEG C, the water vapor after gasification enters into superheat section, adopts diamond heating mode to obtain the superheated vapour of 900-1000 DEG C;
(2) by difluorochloromethane: monochloro methane=0.5-4:1 mol ratio, filling reaction raw materials difluorochloromethane and monochloro methane in mixing vessel;
(3) by the reaction raw materials preheating 200-400 DEG C of step (2), then reactor is entered into after mixing with step (1) superheated vapour, described superheated vapour and reaction raw materials volume ratio are 1-20:1, temperature of reaction controls at 600-1000 DEG C, and reactant reaction intraductal retention time is in the reactor 0.01-0.4s;
(4) the product mixed flow flowed out from reaction tubes is passed in the chilling chuck kettle device of circulating water condensing, and the product stream after chilling is passed into and fills in the deacidification device of alkali lye, then obtains dried product mixtures by drying installation;
(5) product mixtures of step (4) gained is passed in rectifying tower, is separated and obtains 2,3,3,3-tetrafluoeopropene.
2. the preparation method of 2,3,3,3-tetrafluoeopropenes as claimed in claim 1, is characterized in that, in step (1), heating fills the temperature of reaction kettle of water to 120-160 DEG C.
3. the preparation method of 2,3,3,3-tetrafluoeopropenes as claimed in claim 1, is characterized in that, the reactor pressure filling water in step (1) is 1-5 kilogram.
4. the preparation method of 2,3,3,3-tetrafluoeopropenes as claimed in claim 1, is characterized in that, the reactor pressure filling water in step (1) is 2-3 kilogram.
5. the preparation method of 2,3,3,3-tetrafluoeopropenes as claimed in claim 1, is characterized in that, in step (2), reaction raw materials difluorochloromethane and monochloro methane mol ratio are 1 ~ 3:1.
6. the preparation method of 2,3,3,3-tetrafluoeopropenes as claimed in claim 1, is characterized in that, in step (2), reaction raw materials difluorochloromethane and monochloro methane mol ratio are 1 ~ 2:1.
7. the preparation method of 2,3,3,3-tetrafluoeopropenes as claimed in claim 1, is characterized in that, in step (3), described temperature of reaction controls at 700-900 DEG C.
8. the preparation method of 2,3,3,3-tetrafluoeopropenes as claimed in claim 1, is characterized in that, in step (3), reaction pressure is normal pressure or reaction pressure is 0.1 ~ 0.5MPa.
9. the preparation method of 2,3,3,3-tetrafluoeopropenes as claimed in claim 1, it is characterized in that, in step (4), dried product mixtures sampling, adopts gc analysis mixture composition, wherein the massfraction of 2,3,3,3-tetrafluoeopropenes is 25 ~ 55%.
10. the preparation method of 2,3,3,3-tetrafluoeopropenes as claimed in claim 1, is characterized in that, reactor used reaction pipeline is palladium metal, silver or high carbon steel are made.
The preparation method of 11. 2,3,3,3-tetrafluoeopropenes as claimed in claim 1, is characterized in that, reactor used is the tubular reactor of SUS316 stainless steel.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2931840A (en) * | 1958-11-25 | 1960-04-05 | Du Pont | Process for preparing 2, 3, 3, 3-tetrafluoropropene |
| CA690037A (en) * | 1964-07-07 | M. Marquis David | Preparation of 2,3,3,3,-tetrafluoropropene | |
| CN101913989A (en) * | 2010-09-07 | 2010-12-15 | 西安近代化学研究所 | Production method of 2,3,3,3-tetrafluoropropene |
| CN102675038A (en) * | 2012-04-23 | 2012-09-19 | 山东东岳高分子材料有限公司 | Preparation method of 2, 3, 3, 3-tetrafluoropropene |
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| JPS402132B1 (en) * | 1961-03-31 | 1965-02-04 |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA690037A (en) * | 1964-07-07 | M. Marquis David | Preparation of 2,3,3,3,-tetrafluoropropene | |
| US2931840A (en) * | 1958-11-25 | 1960-04-05 | Du Pont | Process for preparing 2, 3, 3, 3-tetrafluoropropene |
| CN101913989A (en) * | 2010-09-07 | 2010-12-15 | 西安近代化学研究所 | Production method of 2,3,3,3-tetrafluoropropene |
| CN102675038A (en) * | 2012-04-23 | 2012-09-19 | 山东东岳高分子材料有限公司 | Preparation method of 2, 3, 3, 3-tetrafluoropropene |
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