CN216584814U - Device for continuously and efficiently preparing monofluoromethane - Google Patents
Device for continuously and efficiently preparing monofluoromethane Download PDFInfo
- Publication number
- CN216584814U CN216584814U CN202123457327.6U CN202123457327U CN216584814U CN 216584814 U CN216584814 U CN 216584814U CN 202123457327 U CN202123457327 U CN 202123457327U CN 216584814 U CN216584814 U CN 216584814U
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- Prior art keywords
- reactor
- monofluoromethane
- evaporator
- continuously
- dimethyl carbonate
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- NBVXSUQYWXRMNV-UHFFFAOYSA-N monofluoromethane Natural products FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910001515 alkali metal fluoride Inorganic materials 0.000 claims abstract description 12
- 230000002572 peristaltic effect Effects 0.000 claims abstract description 11
- 150000004673 fluoride salts Chemical class 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- 238000003860 storage Methods 0.000 claims abstract description 6
- 239000010408 film Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000001179 sorption measurement Methods 0.000 claims description 4
- 239000003518 caustics Substances 0.000 claims description 2
- 239000011552 falling film Substances 0.000 claims description 2
- 238000009776 industrial production Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 17
- 239000000463 material Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 230000008016 vaporization Effects 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000003444 phase transfer catalyst Substances 0.000 description 2
- 239000003586 protic polar solvent Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- VAYGXNSJCAHWJZ-UHFFFAOYSA-N dimethyl sulfate Chemical compound COS(=O)(=O)OC VAYGXNSJCAHWJZ-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- -1 fluorine ions Chemical class 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910001512 metal fluoride Inorganic materials 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model discloses a device for continuously and efficiently preparing monofluoromethane, which is characterized in that a dimethyl carbonate storage tank (1), a peristaltic pump (2), an evaporator (3), a gas flowmeter (4), a reactor (5) and an alkaline washing tower (6) are connected in sequence; the peristaltic pump (2) and the gas flow meter (4) are both connected to the upper part of the evaporator (3); the gas flow meter (4) is connected with the upper part of the reactor (5), the alkaline washing tower (6) is connected with the lower part of the reactor (5), and the reactor is internally provided with a load type alkali metal fluoride salt catalyst. The device for preparing the monofluoromethane has the advantages of high conversion rate of the dimethyl carbonate, high yield of the monofluoromethane, safety, high efficiency and suitability for continuous industrial production.
Description
Technical Field
The utility model relates to a fluoromethane's preparation equipment especially relates to a device of continuous high-efficient preparation fluoromethane.
Background
Electronic gases are essential basic support source materials in the development of integrated circuits, optoelectronics, microelectronics, particularly very large scale integrated circuits, liquid crystal display devices, semiconductor light emitting devices, and semiconductor material fabrication processes, and are known as "blood" and "grain" in the electronics industry. The fluoromethane is a green and efficient electronic special gas, is used for etching semiconductors and electronic products, has good etching selectivity on silicide films, and can dissolve fluorine ions under a radio frequency field to carry out reactive ion etching. The monofluoromethane has the lowest C/F ratio (1: 1) in the mainstream etching gas, the selectivity is extremely high, and the compound growth rate can reach more than 15 percent in the future five years due to the development requirement of advanced processes.
The prior art method for preparing monofluoromethane is as follows: dimethyl sulfate or dimethyl carbonate is used as a raw material and reacts with alkali metal fluoride in an intermittent reaction kettle to prepare the metal fluoride, but the reaction activity of the fluoride in a liquid phase system is extremely poor, the conversion rate is less than 30 percent after about 48 hours of reaction, and a large amount of protic solvent is required to be added in the reaction to be used as a phase transfer catalyst to promote the reaction, so that a large amount of organic waste liquid is generated after the reaction, the solid-liquid reaction of the intermittent reaction kettle is long in time consumption, extremely low in conversion rate and yield, incapable of realizing continuous production, and low in actual industrial production value.
SUMMERY OF THE UTILITY MODEL
For overcoming the defect that prior art exists, the utility model aims at providing a device of continuous high-efficient preparation fluoromethane, through the device preparation fluoromethane, the dimethyl carbonate conversion rate is high, and a fluoromethane yield is high, and is safe, high-efficient, is suitable for serialization industrial production.
In order to overcome the defects of the prior art, the utility model provides a device for continuously and efficiently preparing monofluoromethane, which is characterized in that a dimethyl carbonate storage tank 1, a peristaltic pump 2, an evaporator 3, a gas flowmeter 4, a reactor 5 and an alkaline washing tower 6 are connected in sequence according to the trend of materials; the peristaltic pump 2 and the gas flow meter 4 are connected to the upper part of the evaporator 3; the gas flow meter 4 is connected with the upper part of the reactor 5, the alkaline washing tower 6 is connected with the lower part of the reactor 5, and the inside of the reactor is provided with a load type alkali metal fluoride salt catalyst. Further, the upper part of the alkaline tower 6 is connected with an adsorption rectification system 7.
Pumping dimethyl carbonate in a dimethyl carbonate storage tank into an evaporator for vaporization through a peristaltic pump, then feeding the dimethyl carbonate into a reactor after metering through a flowmeter to react with alkali metal fluoride salt to generate monofluoromethane, removing acid gas such as hydrogen fluoride and the like possibly generated in the reaction and residual dimethyl carbonate from reaction mixed gas discharged from the reactor through alkali washing, and feeding the reaction mixed gas into an adsorption rectification system for refining.
The evaporator is designed for the purpose of vaporizing dimethyl carbonate, and the caustic washing tower is designed for removing acid gas such as hydrogen fluoride and the like which may be generated in the reaction and residual dimethyl carbonate and the like.
The evaporator can be selected from reaction kettle, falling film evaporator, wiped film evaporator, molecular still, etc., preferably wiped film evaporator. The reactor can be selected from a tubular reactor, a fixed bed reactor, a fluidized bed reactor and the like, and is provided with a heating device for controlling the reaction temperature of the bed layer. The pressure and residence time in the reactor can be adjusted by adjusting the feed rate of the peristaltic pump.
The device can prepare high-purity electronic grade monofluoromethane gas continuously, safely and efficiently, and has the following beneficial effects:
(1) the device utilizes the evaporator to vaporize the reactant dimethyl carbonate, then flows through the bed layer of the reactor at a certain speed to react with the active component alkali metal fluoride salt, and compared with a liquid-solid reaction system which can only be carried out in a kettle type reactor (belonging to batch reaction), the device can realize continuous production more easily.
(2) The device adopts continuous flow feeding and discharging modes in the processes of evaporation and vaporization of the dimethyl carbonate and reaction with the alkali metal fluoride, and the retention time of materials in the evaporator and the reactor is shorter, so that instantaneous heating and few reaction materials can be ensured, and the reaction safety is higher.
(3) The reactor of the device is internally provided with the load type alkali metal fluoride catalyst, so that the alkali metal fluoride and the dimethyl carbonate have larger contact area on the microscopic level, and the conversion rate of a reaction system is favorably improved; compared with a liquid-solid phase reaction system, the alkali metal fluoride salt has extremely poor solubility in a liquid phase, and a large amount of protic solvent is required to be added as a phase transfer catalyst to promote the reaction, so that the device is more efficient, convenient and fast to prepare the monofluoromethane and has higher economy. The conversion rate of the dimethyl carbonate can reach more than 82 percent, and the yield of the monofluoromethane can reach more than 74 percent.
(4) The device is used for preparing the fluoromethane, a solvent is not needed to be used, no waste liquid is generated, a small amount of residual unreacted dimethyl carbonate steam in the reaction mixed gas can be absorbed by alkali liquor, no waste gas is generated, the supported alkali metal fluoride salt catalyst used in the reaction can be regenerated by hydrogen fluoride gas to realize cyclic utilization, no waste solid is generated, and green, pollution-free and zero emission is really realized.
Drawings
Fig. 1 is a schematic view of the device of the present invention.
Which comprises the following steps: dimethyl carbonate storage tank 1, peristaltic pump 2, evaporimeter 3, gas flowmeter 4, reactor 5, alkaline tower 6, absorption rectification system 7.
Detailed Description
The following describes in detail embodiments of the present invention with reference to examples.
A device for continuously and efficiently preparing monofluoromethane is characterized in that a dimethyl carbonate storage tank 1, a peristaltic pump 2, an evaporator 3, a gas flowmeter 4, a reactor 5 and an alkaline tower 6 are sequentially connected according to the material trend; the peristaltic pump 2 and the gas flow meter 4 are connected to the upper part of the evaporator 3; the gas flow meter 4 is connected with the upper part of the reactor 5, the alkaline tower 6 is connected with the lower part of the reactor 5, the load type alkali metal fluoride salt catalyst is arranged in the reactor, and the upper part of the alkaline tower 6 is connected with the adsorption rectification system 7. The evaporator is a wiped film evaporator, the reactor is a fixed bed reactor, and the reactor is provided with a heating device for controlling the reaction temperature of the bed layer.
Claims (5)
1. A device for continuously and efficiently preparing monofluoromethane is characterized in that a dimethyl carbonate storage tank (1), a peristaltic pump (2), an evaporator (3), a gas flowmeter (4), a reactor (5) and an alkaline washing tower (6) are sequentially connected; the peristaltic pump (2) and the gas flow meter (4) are both connected to the upper part of the evaporator (3); the gas flow meter (4) is connected with the upper part of the reactor (5), the alkaline washing tower (6) is connected with the lower part of the reactor (5), and the reactor is internally provided with a load type alkali metal fluoride salt catalyst.
2. The apparatus for continuously and efficiently producing monofluoromethane according to claim 1, wherein the upper part of the caustic tower (6) is connected to the adsorption rectification system (7).
3. The apparatus according to claim 1, wherein the evaporator is selected from a reaction vessel, a falling film evaporator, a wiped film evaporator or a molecular still.
4. The apparatus for continuously and efficiently producing monofluoromethane according to claim 1, wherein the reactor is a tubular reactor, a fixed bed reactor or a fluidized bed reactor.
5. An apparatus for continuously and efficiently producing monofluoromethane according to claim 1, wherein the reactor is equipped with a heating means.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202123457327.6U CN216584814U (en) | 2021-12-30 | 2021-12-30 | Device for continuously and efficiently preparing monofluoromethane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202123457327.6U CN216584814U (en) | 2021-12-30 | 2021-12-30 | Device for continuously and efficiently preparing monofluoromethane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN216584814U true CN216584814U (en) | 2022-05-24 |
Family
ID=81631438
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202123457327.6U Active CN216584814U (en) | 2021-12-30 | 2021-12-30 | Device for continuously and efficiently preparing monofluoromethane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN216584814U (en) |
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2021
- 2021-12-30 CN CN202123457327.6U patent/CN216584814U/en active Active
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