CN111559954A - Preparation method of 2-chloro-3, 3, 3-trifluoropropene - Google Patents
Preparation method of 2-chloro-3, 3, 3-trifluoropropene Download PDFInfo
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- CN111559954A CN111559954A CN202010424484.8A CN202010424484A CN111559954A CN 111559954 A CN111559954 A CN 111559954A CN 202010424484 A CN202010424484 A CN 202010424484A CN 111559954 A CN111559954 A CN 111559954A
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Abstract
The invention discloses a preparation method of 2-chloro-3, 3, 3-trifluoropropene, which mainly comprises the following steps: (1) 3,3, 3-trifluoropropene and chlorine are led into a photochlorination reaction kettle containing 2, 3-dichloro-1, 1, 1-trifluoropropane according to a certain proportion; (2) continuously adding reactants in the photochlorination reaction kettle in the step (1) into a rectifying tower, and obtaining 2, 3-dichloro-1, 1, 1-trifluoropropane at the bottom of the rectifying tower; (3) adding the 2, 3-dichloro-1, 1, 1-trifluoropropane obtained in the step (2) into a gasifier by using a metering pump, gasifying the mixture, mixing the gasified mixture with oxygen-poor nitrogen, and feeding the mixture into a fixed bed reactor filled with a catalyst to perform gas-phase catalytic dehydrochlorination; (4) condensing the reaction gas from the fixed bed reactor in the step (3) by a primary cooler and a secondary cooler to obtain a material of crude 2-chloro-3, 3, 3-trifluoropropene, and rectifying and purifying the crude 2-chloro-3, 3, 3-trifluoropropene. The invention has the advantages of high product selectivity, simple process and easy industrialization.
Description
Technical Field
The invention relates to the technical field of synthesis of intermediates, in particular to a preparation method of 2-chloro-3, 3, 3-trifluoropropene.
Background
2-chloro-3, 3, 3-trifluoropropene (HCFO-1233 xf) is useful as an intermediate for the preparation of various fluorocarbons, such as for the synthesis of HFC-245fa, HFO-1234yf, and the like, and also as a monomer for the synthesis of various polymers.
HCFO-1233xf is produced in a number of ways, for example: CN109651077A uses a chromium-containing fluorination catalyst to catalyze the reaction of polyhalogenated propylene and HF to prepare HCFO-1233xf under the gas phase condition. WO2007079431 and WO2008054781 use 1,1,2, 3-tetrachloropropene as raw material, and synthesize HCFO-1233xf by gas phase fluorination under the action of chromium catalyst, the catalyst is easy to deactivate, and the selectivity of 2-chloro-3, 3, 3-trifluoropropene is gradually reduced along with the activity. US20090030247 uses 1,1,1,2, 3-pentachloropropane and 2,3,3, 3-tetrachloropropene as raw materials, and adds amines, hydroquinones or other stabilizers to perform catalytic fluorination to synthesize HCFO-1233xf, which has low product selectivity and can not achieve the purpose of inhibiting the deactivation of the catalyst well. Therefore, it is urgently needed to develop a method for continuously preparing 2-chloro-3, 3, 3-trifluoropropene with high yield, which has simple process and low cost.
Disclosure of Invention
The invention aims to provide a preparation method of 2-chloro-3, 3, 3-trifluoropropene, which has high product selectivity, simple process and easy industrialization.
The technical purpose of the invention is realized by the following technical scheme:
a preparation method of 2-chloro-3, 3, 3-trifluoropropene is characterized by mainly comprising the following steps:
(1) 3,3, 3-trifluoropropene and chlorine are led into a photochlorination reaction kettle containing 2, 3-dichloro-1, 1, 1-trifluoropropane according to a certain proportion, so as to carry out photochlorination synthesis of the 2, 3-dichloro-1, 1, 1-trifluoropropane;
(2) continuously adding reactants in the photochlorination reaction kettle in the step (1) into a rectifying tower, absorbing gas-phase materials rich in 3,3, 3-trifluoropropene in the tower top by using 2, 3-dichloro-1, 1, 1-trifluoropropane in the rectifying tower, adding the gas-phase materials into the photochlorination reaction kettle, and obtaining 2, 3-dichloro-1, 1, 1-trifluoropropane in the tower kettle;
(3) adding the 2, 3-dichloro-1, 1, 1-trifluoropropane obtained in the step (2) into a gasifier by using a metering pump, gasifying the mixture, mixing the gasified mixture with oxygen-poor nitrogen, and feeding the mixture into a fixed bed reactor filled with a catalyst to perform gas-phase catalytic dehydrochlorination;
(4) condensing the reaction gas from the fixed bed reactor in the step (3) by a primary cooler, recovering unreacted 2, 3-dichloro-1, 1, 1-trifluoropropane, condensing the subsequent reaction gas by a secondary cooler to obtain a crude material of 2-chloro-3, 3, 3-trifluoropropene, absorbing and treating the non-condensable gas by using water, then evacuating, and rectifying and purifying the crude 2-chloro-3, 3, 3-trifluoropropene.
Preferably, the molar ratio of the 3,3, 3-trifluoropropene to the chlorine gas in the step (1) is 1-1.02: 1.
preferably, a light source is arranged in the photochlorination kettle, and the wavelength range of the light source is between the wavelength of visible light and the wavelength of ultraviolet light.
Preferably, in the step (1), the reaction temperature in the photochlorination reaction kettle is 15-85 ℃, and the reaction time is 0.5-5 h.
Preferably, the reaction temperature of the tower kettle of the rectifying tower in the step (2) is 77-85 ℃.
Preferably, the mass space velocity of the 2, 3-dichloro-1, 1, 1-trifluoropropane entering the gasifier in the step (3) is 0.75-3.8 h-1The volume space velocity of the oxygen-poor nitrogen is 100-500 h-1The oxygen content of the oxygen-deficient nitrogen is 0.05%~5%。
Preferably, the temperature of the gasifier is 180-200 ℃.
Preferably, the catalyst in the step (3) is ZnO-Bi2O3-ZrO2/Al-MCM-41。
Preferably, the gas phase catalytic reaction temperature in the step (3) is 230-350 ℃.
Preferably, the temperature of the primary cooler in the step (4) is 30-70 ℃, and the temperature of the secondary cooler is-15-10 ℃.
In conclusion, the invention has the following beneficial effects:
1. in the photochlorination reaction, excessive 3,3, 3-trifluoropropene added in the previous period is recycled, so that the effect of protecting 2, 3-dichloro-1, 1, 1-trifluoropropane can be achieved, and high boiling point generated by substitution is effectively reduced.
2. The gas-phase dehydrochlorination catalyst ZnO-Bi adopted by the invention2O3-ZrO2The specific surface area of the/Al-MCM-41 is large, and the catalytic activity loaded on the surface active sites of the carrier can be fully exerted. In addition, the pore diameter of the catalyst is larger, which is beneficial to product diffusion, thereby reducing product coking, improving product selectivity, and the catalyst is easy to regenerate, and the inactivated catalyst can be activated and regenerated by adopting a high-temperature roasting mode.
3. The invention uses oxygen-poor nitrogen as carrier gas, which can play the role of coking resistance of the catalyst.
4. The invention has the advantages of low cost of raw materials, simple process flow and easy industrialization.
Description of the drawings:
FIG. 1 is a schematic flow diagram of a process for the preparation of 2,3,3, 3-trifluoropropene according to the present invention;
the labels in the figures are: 1. the device comprises a photochlorination reaction kettle, 2, a rectifying tower, 3, a cracking raw material tank, 4, a fixed bed reactor, 5, a primary condenser, 6, a first gas-liquid separator, 7, a cracking raw material recovery tank, 8, a secondary condenser, 9, a second gas-liquid separator, 10 and a tail gas washing tower.
Detailed Description
The following further describes the embodiments of the present invention with reference to the drawings, and the present embodiment is not to be construed as limiting the invention.
As shown in FIG. 1, the detailed process flow of the invention is as follows:
3,3, 3-trifluoropropene and chlorine are introduced into a photochlorination reactor 1 containing 2, 3-dichloro-1, 1, 1-trifluoropropane according to a certain proportion for reaction, reaction liquid is continuously added into a rectifying tower 2, 3-dichloro-1, 1, 1-trifluoropropane obtained in the tower bottom is pumped into a cracking raw material tank 3, a gas phase material rich in 3,3, 3-trifluoropropene at the tower top of the rectifying tower 2 is absorbed by the 2, 3-dichloro-1, 1, 1-trifluoropropane and then is added into the photochlorination reactor 1, and part of the 2, 3-dichloro-1, 1, 1-trifluoropropane material in the cracking raw material tank 3 is returned to the photochlorination reactor 1 to be used as a solvent.
Adding the obtained 2, 3-dichloro-1, 1, 1-trifluoropropane and oxygen-deficient nitrogen into a fixed bed reactor 4 for gas-phase catalytic dehydrochlorination, condensing a mixed gas generated by the reaction through a primary cooler 5, separating the mixed gas through a first gas-liquid separator 6, recovering the unreacted 2, 3-dichloro-1, 1, 1-trifluoropropane to a cracking raw material recovery tank 7, the subsequent reaction gas is condensed in a secondary cooler 8, separated by a second gas-liquid separator 9, the liquid phase obtains a material of crude 2-chloro-3, 3, 3-trifluoropropene, the non-condensable gas is subjected to water absorption treatment in a tail gas water washing tower 10 to obtain acid liquid and exhaust gas, and the acid liquid and the tail gas are emptied, and the 2, 3-dichloro-1, 1, 1-trifluoropropane recovered from the cracking raw material recovery tank 7 can be continuously added into the fixed bed reactor 4 for reaction.
The volume of a photochlorination reaction kettle 1 is 5L, the photochlorination reaction kettle is connected with a rectifying tower 2 with the diameter of 50mm and the number of tower plates of 8, and a fixed bed reactor 4 filled with a catalyst has the diameter of 30 mm.
Example 1
The photochlorination reaction kettle is internally provided with a light source with a partial ultraviolet wavelength and 2, 3-dichloro-1, 1, 1-trifluoropropane. The feeding flow rate of the 2, 3-dichloro-1, 1, 1-trifluoropropane absorption liquid to the photo-chlorination reaction kettle at the top of the rectifying tower is 10mol/h, the feeding flow rate of the 3,3, 3-trifluoropropene to the photo-chlorination reaction kettle is 40.8mol/h, the feeding flow rate of chlorine to the photo-chlorination reaction kettle is 40mol/h, the reaction temperature is 45 ℃, and the reaction residence time is 0.5 h.
After the reaction is finished, the mole fraction of each component in the photo-chlorination reaction kettle is as follows: 0.997 percent of 2, 3-dichloro-1, 1, 1-trifluoropropane, 0.001 percent of 2,3, 3-trichloro-1, 1, 1-trifluoropropane, 0.002 percent of 3,3, 3-trifluoropropene, wherein the materials in the photochlorination reaction kettle are conveyed into a rectifying tower by a material pump at a liquid phase flow rate of 50.8mol/h, the feeding flow rate of the 3,3, 3-trifluoropropene to the photochlorination reaction kettle is adjusted to 40mol/h, the rectifying tower is operated at normal pressure, the yield at the bottom of the tower is 50mol/h, the top temperature of the rectifying tower is 35.2 ℃, and the temperature of the bottom of the tower is 83.1 ℃. The mole fraction of 2, 3-dichloro-1, 1, 1-trifluoropropane in the tower bottom material is 0.999, and the mole fraction of 2,3, 3-trichloro-1, 1, 1-trifluoropropane in the tower bottom material is 0.001, and the gas phase material rich in 3,3, 3-trifluoropropene in the tower top is absorbed by the 2, 3-dichloro-1, 1, 1-trifluoropropane and then is added into a photochlorination reaction kettle.
The mass airspeed of the material flowing out of the tower kettle of the rectifying tower is 2.0h by a metering pump-1After vaporization at 190 ℃, the air speed of the mixture is 350h-1Mixing oxygen-poor nitrogen with oxygen content of 1.2%, introducing the mixed gas into a reactor with diameter of 30mm, and filling with 50.1g mesoporous ZnO-Bi2O3-ZrO2Dehydrochlorination is carried out in a fixed bed reactor of an Al-MCM-41 catalyst at 240 ℃, and after sampling a mixed gas generated by the reaction, the conversion rate of 2, 3-dichloro-1, 1, 1-trifluoropropane is 89.4% and the selectivity of 2-chloro-3, 3, 3-trifluoropropene is 98.7% by gas chromatography analysis.
The mixed gas generated by the reaction is condensed by a primary condenser at 36.1 ℃ to recover unreacted 2, 3-dichloro-1, 1, 1-trifluoropropane, the subsequent mixed gas is condensed by a secondary condenser at-10.7 ℃ to obtain a crude material of crude 2-chloro-3, 3, 3-trifluoropropene, the crude material is rectified, separated and purified to obtain the 2-chloro-3, 3, 3-trifluoropropene with the purity of 99.9 percent, and the noncondensable gas discharged from the secondary condenser is washed by water and then is discharged.
Example 2
The photochlorination reaction kettle is internally provided with a light source with a partial ultraviolet wavelength and 2, 3-dichloro-1, 1, 1-trifluoropropane. The feeding flow rate of the 2, 3-dichloro-1, 1, 1-trifluoropropane absorption liquid to the photo-chlorination reaction kettle at the top of the rectifying tower is 10mol/h, the feeding flow rate of the 3,3, 3-trifluoropropene to the photo-chlorination reaction kettle is 40.8mol/h, the feeding flow rate of chlorine to the photo-chlorination reaction kettle is 40mol/h, the reaction temperature is 35 ℃, and the reaction residence time is 5 h.
After the reaction is finished, the mole fraction of each component in the chlorination reaction kettle is as follows: 0.995 percent of 2, 3-dichloro-1, 1, 1-trifluoropropane, 0.002 percent of 2,3, 3-trichloro-1, 1, 1-trifluoropropane and 0.003 percent of 3,3, 3-trifluoropropene, wherein the materials in the photochlorination reaction kettle are conveyed into a rectifying tower by a material pump at a liquid phase flow rate of 50.8mol/h, the feeding flow rate of the 3,3, 3-trifluoropropene to the photochlorination reaction kettle is adjusted to 40mol/h, the rectifying tower is operated at normal pressure, the yield at the bottom of the tower is 50mol/h, the top temperature of the rectifying tower is 36.4 ℃, and the temperature of the tower is 84.7 ℃. The mole fraction of 2, 3-dichloro-1, 1, 1-trifluoropropane in the tower bottom material is 0.998, and the mole fraction of 2,3, 3-trichloro-1, 1, 1-trifluoropropane in the tower bottom material is 0.002, and the gas phase material rich in 3,3, 3-trifluoropropene in the tower top is absorbed by the 2, 3-dichloro-1, 1, 1-trifluoropropane and then is added into a photochlorination reaction kettle.
The mass airspeed of the material flowing out of the tower kettle of the rectifying tower is 1.5h by a metering pump-1After vaporization at 200 ℃, the air speed is 120h-1Mixing oxygen-poor nitrogen with oxygen content of 0.5%, introducing the mixed gas into a reactor with diameter of 30mm, and filling with 50.0g of mesoporous ZnO-Bi2O3-ZrO2Dehydrochlorination is carried out in a fixed bed reactor of an Al-MCM-41 catalyst at 260 ℃, and after sampling a mixed gas generated by the reaction, the conversion rate of 2, 3-dichloro-1, 1, 1-trifluoropropane is 85.4 percent and the selectivity of 2-chloro-3, 3, 3-trifluoropropene is 98.9 percent by adopting gas chromatography analysis.
The mixed gas generated by the reaction is condensed by a primary condenser at 65.2 ℃ to recover unreacted 2, 3-dichloro-1, 1, 1-trifluoropropane, the subsequent mixed gas is condensed by a secondary condenser at 9.6 ℃ to obtain a crude material of crude 2-chloro-3, 3, 3-trifluoropropene, the crude material is separated and purified to obtain the 2-chloro-3, 3, 3-trifluoropropene with the purity of 99.9%, and the non-condensable gas discharged from the secondary condenser is washed by water and then is discharged.
Example 3
The photochlorination reaction kettle is internally provided with a light source with a partial ultraviolet wavelength and 2, 3-dichloro-1, 1, 1-trifluoropropane. The feeding flow rate of the 2, 3-dichloro-1, 1, 1-trifluoropropane absorption liquid to the photo-chlorination reaction kettle at the top of the rectifying tower is 10mol/h, the feeding flow rate of the 3,3, 3-trifluoropropene to the photo-chlorination reaction kettle is 40.8mol/h, the feeding flow rate of chlorine to the photo-chlorination reaction kettle is 40mol/h, the reaction temperature is 75 ℃, and the reaction residence time is 0.5 h.
After the reaction is finished, the mole fraction of each component in the chlorination reaction kettle is as follows: 0.996 percent of 2, 3-dichloro-1, 1, 1-trifluoropropane, 0.001 percent of 2,3, 3-trichloro-1, 1, 1-trifluoropropane, 0.003 percent of 3,3, 3-trifluoropropene, wherein a material pump is used for conveying materials in the photochlorination reaction kettle to a rectifying tower at a liquid phase flow rate of 50.8mol/h, the feeding flow rate of the 3,3, 3-trifluoropropene to the photochlorination reaction kettle is adjusted to 40mol/h, the rectifying tower is operated at normal pressure, the yield at the bottom of the tower is 50mol/h, the top temperature of the rectifying tower is 35.7 ℃, and the temperature of the bottom of the tower is 80.3 ℃. The mole fraction of 2, 3-dichloro-1, 1, 1-trifluoropropane in the tower bottom material is 0.999, and the mole fraction of 2,3, 3-trichloro-1, 1, 1-trifluoropropane in the tower bottom material is 0.001, and the gas phase material rich in 3,3, 3-trifluoropropene in the tower top is absorbed by the 2, 3-dichloro-1, 1, 1-trifluoropropane and then is added into a photochlorination reaction kettle.
The mass airspeed of the material flowing out of the tower kettle of the rectifying tower is 0.80h by a metering pump-1After vaporization at 190 ℃, the air speed of the mixture is 240h-1Mixing oxygen-poor nitrogen with oxygen content of 0.08%, introducing the mixed gas into a reactor with diameter of 30mm, and filling with 50.0g of mesoporous ZnO-Bi2O3-ZrO2Dehydrochlorination is carried out in a fixed bed reactor of an Al-MCM-41 catalyst at 320 ℃, and after sampling a mixed gas generated by the reaction, the conversion rate of 2, 3-dichloro-1, 1, 1-trifluoropropane is 88.3 percent and the selectivity of 2-chloro-3, 3, 3-trifluoropropene is 98.8 percent by adopting gas chromatography analysis.
The mixed gas generated by the reaction is condensed by a primary condenser at 45.7 ℃ to recycle the unreacted 2, 3-dichloro-1, 1, 1-trifluoropropane, the subsequent mixed gas is condensed by a secondary condenser at-8.4 ℃ to obtain a crude material of crude 2-chloro-3, 3, 3-trifluoropropene, the crude material is separated and purified to obtain the 2-chloro-3, 3, 3-trifluoropropene with the purity of 99.9%, and the non-condensable gas discharged from the secondary condenser is washed by water and then is discharged.
Example 4
The photochlorination reaction kettle is internally provided with a yellow light source and 2, 3-dichloro-1, 1, 1-trifluoropropane. The feeding flow rate of the 2, 3-dichloro-1, 1, 1-trifluoropropane absorption liquid to the photo-chlorination reaction kettle at the top of the rectifying tower is 10mol/h, the feeding flow rate of the 3,3, 3-trifluoropropene to the photo-chlorination reaction kettle is 40.8mol/h, the feeding flow rate of chlorine to the photo-chlorination reaction kettle is 40mol/h, the reaction temperature is 60 ℃, and the reaction residence time is 1.0 h.
After the reaction is finished, the mole fraction of each component in the chlorination reaction kettle is as follows: 0.995 percent of 2, 3-dichloro-1, 1, 1-trifluoropropane, 0.001 percent of 2,3, 3-trichloro-1, 1, 1-trifluoropropane, 0.004 percent of 3,3, 3-trifluoropropene, conveying the materials in the photochlorination reaction kettle to a rectifying tower by using a material pump at a liquid phase flow rate of 50.8mol/h, adjusting the feeding flow rate of the 3,3, 3-trifluoropropene to the photochlorination reaction kettle to 40mol/h, wherein the rectifying tower is operated at normal pressure, the yield at the bottom of the tower is 50mol/h, the top temperature of the rectifying tower is 35.7 ℃, and the temperature of the bottom of the tower is 80.3 ℃. The mole fraction of 2, 3-dichloro-1, 1, 1-trifluoropropane in the tower bottom material is 0.999, and the mole fraction of 2,3, 3-trichloro-1, 1, 1-trifluoropropane in the tower bottom material is 0.001, and the gas phase material rich in 3,3, 3-trifluoropropene in the tower top is absorbed by the 2, 3-dichloro-1, 1, 1-trifluoropropane and then is added into a photochlorination reaction kettle.
The material flowing out of the rectifying tower kettle passes through a metering pump at a mass airspeed of 3.5h-1After vaporization at 190 ℃, the air speed of the reactor is 480h-1Mixing oxygen-poor nitrogen with oxygen content of 4.5%, introducing the mixed gas into a reactor with diameter of 30mm, and filling with 50.0g of mesoporous ZnO-Bi2O3-ZrO2Dehydrochlorination is carried out in a fixed bed reactor of an Al-MCM-41 catalyst at 320 ℃, and after sampling a mixed gas generated by the reaction, the conversion rate of 2, 3-dichloro-1, 1, 1-trifluoropropane is 81.7 percent and the selectivity of 2-chloro-3, 3, 3-trifluoropropene is 99.1 percent by adopting gas chromatography analysis.
The mixed gas generated by the reaction is condensed by a primary condenser at 30.5 ℃ to recover unreacted 2, 3-dichloro-1, 1, 1-trifluoropropane, the subsequent mixed gas is condensed by a secondary condenser at-14.7 ℃ to obtain a crude material of crude 2-chloro-3, 3, 3-trifluoropropene, the crude material is rectified, separated and purified to obtain the 2-chloro-3, 3, 3-trifluoropropene with the purity of 99.9%, and the non-condensable gas discharged from the secondary condenser is washed by water and then is discharged.
According to the invention, excessive 3,3, 3-trifluoropropene is added in the early stage of the photochlorination, and a small amount of unreacted 3,3, 3-trifluoropropene is absorbed by 2, 3-dichloro-1, 1, 1-trifluoropropane and then is recycled in the device, so that the generation of photochlorination substitution products is reduced. In addition, the gas-phase dehydrochlorination catalyst is a porous mesoporous material, so that the escape of a product is facilitated, the product coking is reduced, and the oxygen-poor nitrogen is used as a carrier gas, so that the anti-coking effect of the catalyst can be achieved.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention.
Claims (10)
1. A preparation method of 2-chloro-3, 3, 3-trifluoropropene is characterized by mainly comprising the following steps:
(1) 3,3, 3-trifluoropropene and chlorine are led into a photochlorination reaction kettle containing 2, 3-dichloro-1, 1, 1-trifluoropropane according to a certain proportion, so as to carry out photochlorination synthesis of the 2, 3-dichloro-1, 1, 1-trifluoropropane;
(2) continuously adding reactants in the photochlorination reaction kettle in the step (1) into a rectifying tower, absorbing gas-phase materials rich in 3,3, 3-trifluoropropene in the tower top by using 2, 3-dichloro-1, 1, 1-trifluoropropane in the rectifying tower, adding the gas-phase materials into the photochlorination reaction kettle, and obtaining 2, 3-dichloro-1, 1, 1-trifluoropropane in the tower kettle;
(3) adding the 2, 3-dichloro-1, 1, 1-trifluoropropane obtained in the step (2) into a gasifier by using a metering pump, gasifying the mixture, mixing the gasified mixture with oxygen-poor nitrogen, and feeding the mixture into a fixed bed reactor filled with a catalyst to perform gas-phase catalytic dehydrochlorination;
(4) condensing the reaction gas from the fixed bed reactor in the step (3) by a primary cooler, recovering unreacted 2, 3-dichloro-1, 1, 1-trifluoropropane, condensing the subsequent reaction gas by a secondary cooler to obtain a crude material of 2-chloro-3, 3, 3-trifluoropropene, absorbing and treating the non-condensable gas by using water, then evacuating, and rectifying and purifying the crude 2-chloro-3, 3, 3-trifluoropropene.
2. The process according to claim 1 for producing 2-chloro-3, 3, 3-trifluoropropene, which comprises: the mol ratio of the 3,3, 3-trifluoropropene to the chlorine in the step (1) is 1-1.02: 1.
3. the process according to claim 1 for producing 2-chloro-3, 3, 3-trifluoropropene, which comprises: and a light source is arranged in the photo-chlorination reaction kettle, and the wavelength range of the light source is between the wavelength of visible light and the wavelength of ultraviolet light.
4. The process according to claim 1 for producing 2-chloro-3, 3, 3-trifluoropropene, which comprises: in the step (1), the reaction temperature in the photochlorination reaction kettle is 15-85 ℃, and the reaction time is 0.5-5 h.
5. The process according to claim 1 for producing 2-chloro-3, 3, 3-trifluoropropene, which comprises: and (3) in the step (2), the reaction temperature of the tower kettle of the rectifying tower is 77-85 ℃.
6. The process according to claim 1 for producing 2-chloro-3, 3, 3-trifluoropropene, which comprises: the mass space velocity of the 2, 3-dichloro-1, 1, 1-trifluoropropane entering the gasifier in the step (3) is 0.75-3.8 h-1The volume space velocity of the oxygen-poor nitrogen is 100-500 h-1The oxygen content of the oxygen-poor nitrogen is 0.05-5%.
7. The process according to claim 1 for producing 2-chloro-3, 3, 3-trifluoropropene, which comprises: the gasifier temperature is 180-200 ℃.
8. The process according to claim 1 for producing 2-chloro-3, 3, 3-trifluoropropene, which comprises: the catalyst in the step (3) is ZnO-Bi2O3-ZrO2/Al-MCM-41。
9. The process according to claim 1 for producing 2-chloro-3, 3, 3-trifluoropropene, which comprises: and (3) the gas-phase catalytic reaction temperature in the step (3) is 230-350 ℃.
10. The process according to claim 1 for producing 2-chloro-3, 3, 3-trifluoropropene, which comprises: the temperature of the primary cooler in the step (4) is 30-70 ℃, and the temperature of the secondary cooler is-15-10 ℃.
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| CN112537997A (en) * | 2020-12-09 | 2021-03-23 | 威海新元化工有限公司 | Method and device for co-production of 3,3, 3-trifluoropropene and 2-chloro-3, 3, 3-trifluoropropene |
| CN115160104A (en) * | 2022-08-15 | 2022-10-11 | 中盐常州化工股份有限公司 | Production method of pesticide grade 1,2, 3-tetrachloropropene |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103449958A (en) * | 2013-08-15 | 2013-12-18 | 巨化集团技术中心 | Synthesis method of 2-chloro-3,3,3-trifluoropropene |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103449958A (en) * | 2013-08-15 | 2013-12-18 | 巨化集团技术中心 | Synthesis method of 2-chloro-3,3,3-trifluoropropene |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112537997A (en) * | 2020-12-09 | 2021-03-23 | 威海新元化工有限公司 | Method and device for co-production of 3,3, 3-trifluoropropene and 2-chloro-3, 3, 3-trifluoropropene |
| CN112537997B (en) * | 2020-12-09 | 2021-06-29 | 威海新元化工有限公司 | Method and device for co-production of 3,3, 3-trifluoropropene and 2-chloro-3, 3, 3-trifluoropropene |
| CN115160104A (en) * | 2022-08-15 | 2022-10-11 | 中盐常州化工股份有限公司 | Production method of pesticide grade 1,2, 3-tetrachloropropene |
| CN115160104B (en) * | 2022-08-15 | 2023-12-22 | 中盐常州化工股份有限公司 | Production method of pesticide grade 1,2, 3-tetrachloropropene |
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