CN215540754U - Reaction device for high-purity chlorine trifluoride - Google Patents
Reaction device for high-purity chlorine trifluoride Download PDFInfo
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Abstract
The utility model provides a reaction device for high-purity chlorine trifluoride, and relates to the technical field of chemical industry. This reaction unit of high-purity level chlorine trifluoride includes casing and level set up in baffle in the casing, the baffle will separate charging chamber and the reaction chamber for the intercommunication from top to bottom for the casing, casing outer wall cover is equipped with the heating member, be provided with fluorine gas feed inlet and chlorine gas feed inlet on the wall of charging chamber, the reaction chamber is provided with the chlorine trifluoride gas outlet. The reaction device has the advantages that the heating element is additionally arranged on the shell, and the inside of the reaction device is divided into the feeding chamber and the reaction chamber by the partition plate, so that the reaction efficiency of chlorine trifluoride can be effectively improved, the utilization rate of chlorine gas is improved, and the purity of chlorine trifluoride is further improved.
Description
Technical Field
The utility model relates to the technical field of chemical production, in particular to a reaction device for high-purity chlorine trifluoride.
Background
Chlorine trifluoride isThe strong oxidant has high chemical reaction activity and inflammable characteristic, can perform explosive reaction with water and organic compounds, and is mainly used for uranium concentration and military in the electronic industry and nuclear industry. The high-purity chlorine trifluoride is mainly applied to cleaning of CVD chambers and pipelines thereof in the fields of semiconductors, liquid crystals, solar energy, LEDs and the like, and has obvious advantages in the aspects of cleaning quality, efficiency and greenhouse effect reduction. Unlike other fluorine-containing gases used for cleaning (e.g., NF)3、C2F6And CF4) Chlorine trifluoride can react with a semiconductor material at room temperature without heating a cleaning part, and therefore, the use of chlorine trifluoride can eliminate a heating part and a heating step, and can clean a CVD chamber at room temperature directly with chlorine trifluoride without using a process equipment for dissociating fluorine gas containing fluorine gas by plasma or the like. In addition, chlorine trifluoride is used for cleaning, a high-energy ion bombardment process like plasma does not exist in the chemical etching process, ion bombardment is avoided, and damage to equipment can be reduced to the minimum. Meanwhile, chlorine trifluoride cleaning belongs to a cleaning process in situ, equipment does not need to be disassembled so as to clean dead angles of the equipment and a pipeline, the equipment downtime can be reduced, the quantity of particle impurities can be reduced, and the exposure time of operators is reduced. High purity chlorine trifluoride is used as a CVD chamber cleaning gas, which has significant advantages in cleaning quality, efficiency and reduction of greenhouse effect.
The chlorine trifluoride has active chemical property, strong oxidability and high chemical reaction activity, and has strict requirements on production process condition control and equipment materials, so that the large-scale production and application of the chlorine trifluoride are limited. The purification method of chlorine trifluoride was originally proposed in 1930 by Ruff (Ruff) and kruk (Krug), in which fluorine gas and chlorine gas react to generate chlorine monofluoride first, and chlorine monofluoride further reacts with fluorine gas to generate chlorine trifluoride, and the reaction is carried out in two steps, which require two purification and separation processes. When the method is used for synthesizing the chlorine trifluoride, the reaction efficiency is low, and the method is not suitable for industrial production.
In the prior art, methods for purifying chlorine trifluoride are mainly classified into the following categories:
1. with solid metal chloride (NaCl or Ca)Cl2) The raw material reacts with fluorine gas to generate chlorine gas and chlorine monofluoride, and the chlorine monofluoride further reacts with the fluorine gas to generate chlorine trifluoride. The method has the advantages of easily obtained raw materials and complex process operation, and has the disadvantages of gas-solid reaction, complex reactor structure, low raw material conversion rate, two-step reaction, two-time separation and purification process and complex process operation.
2. Fluorine gas is introduced into liquid carbon tetrachloride or silicon tetrachloride to react to generate chlorine gas, and then the fluorine gas and the chlorine gas are further reacted to generate chlorine trifluoride. The method has the disadvantages that raw materials are not easy to obtain, the reaction needs to be carried out in two steps, two reactors for gas-liquid and gas-gas reactions are involved, the process operation is complex, impurities in the crude product are too much, the purification is not favorable, and the industrial large-scale production is difficult.
3. Chlorine gas, fluorine gas and a diluent gas are mixed and introduced into a reactor containing a catalyst, and chlorine trifluoride is purified at 100 to 400 ℃ using nickel fluoride or the like as the catalyst. The method has the advantages that the reaction is one-step catalytic synthesis, and has the disadvantages that the reaction needs to be added with a catalyst and the reaction pressure is higher.
In summary, there are many methods for purifying chlorine trifluoride, but methods which are developed for industrial production are essentially only those in which elemental fluorine reacts directly with chlorine. The main reaction equation is as follows:
F2+Cl2→2ClF3F2+CL2→2ClF3
the method can produce chlorine trifluoride with high impurity content, and contains more byproduct impurities ClF and ClO2F、F2And HF and the like. Because HF impurities in fluorine gas are high, the concentration of fluorine gas is low, generated ClF impurities are high, the yield of chlorine trifluoride products is influenced, particularly, HF is difficult to deeply process, after chlorine trifluoride gas is rectified, the content of HF is 500-700 PPm at present, the concentration of chlorine trifluoride is only 99.9%, the high-purity quality requirement of the current microelectronic industry development cannot be met, and the technical index of high-purity chlorine trifluoride on HF cannot be met.
The 3N chlorine trifluoride product also newly increases metal ion solid residues when cleaning the PECVD and LPCVD (cold wall) process chambers, and secondarily pollutes the CVD process chambers. The chlorine trifluoride gas used for etching and cleaning very large scale integrated circuit features high purity and ultracleanliness, especially the content of hydrogen fluoride must be less than or equal to 300 PPm. The demand for high purity grade chlorine trifluoride is currently primarily dependent on importation in the United states and Japan.
There are also some methods of purifying chlorine trifluoride in the current patent art, such as:
"a chlorine trifluoride purification method (CN 104477849A)" discloses a method for purifying chlorine trifluoride and provides a production apparatus, in which an inert gas is used to dilute fluorine gas and a mixed gas of chloride and fluorine gas is used to prepare the chlorine trifluoride, in the technique, the utilization rate of fluorine gas is 90%, the content of hydrogen fluoride is 600PPm, and chlorine trifluoride product can only meet 99.9%, and the index requirement of high purity level is not met.
"A chlorine trifluoride purification method (CN 104555927A)" discloses a method for purifying chlorine trifluoride and provides an adsorption apparatus. The absorption of hydrogen fluoride is improved, but there is no mention of the adsorption of fluorine systems, and there are disadvantages of low chlorine trifluoride yield and low gas purity.
"a method and a system for purifying chlorine trifluoride" (CN112390230A) discloses a method and a system for purifying chlorine trifluoride and provides an adsorption and rectification apparatus. The absorption rate of the chlorine trifluoride gas to the hydrogen fluoride is improved, but the defect of low purity of the chlorine trifluoride gas can only meet the quality index of 99.9 percent.
"a method for purifying chlorine trifluoride" (CN112723313A) discloses a method for purifying chlorine trifluoride, which only provides a production method, but the adsorption system does not have, although there is a rectification device, but the final quality index can only reach 99.1%. The method has simpler process, but the product quality can not meet the index requirement of high-purity chlorine trifluoride.
Therefore, it is urgently needed to develop a new chlorine trifluoride purification method, which can effectively overcome various defects in the prior art and realize industrial production on the premise of ensuring the quality of purified chlorine trifluoride.
SUMMERY OF THE UTILITY MODEL
The utility model provides a high-purity chlorine trifluoride reaction device, which is characterized in that a heating element is additionally arranged on a shell, and the interior of the reaction device is divided into a feeding chamber and a reaction chamber by using a partition plate, so that the reaction efficiency of chlorine trifluoride can be effectively improved, the utilization rate of chlorine gas is improved, and the purity of chlorine trifluoride is further improved.
The technical problem to be solved by the utility model is realized by adopting the following technical scheme.
The embodiment of the application provides a high-purity chlorine trifluoride's reaction unit, including casing and level set up in baffle in the casing, the baffle will separate charging chamber and the reaction chamber for the intercommunication from top to bottom for the casing, the casing outer wall cover is equipped with the heating member, be provided with fluorine gas feed inlet and chlorine gas feed inlet on the wall of charging chamber, the reaction chamber is provided with chlorine trifluoride gas outlet.
Compared with the prior art, the embodiment of the utility model has at least the following advantages or beneficial effects:
according to the high-purity chlorine trifluoride reaction device, the heating element is additionally arranged on the shell, and the inside of the reaction device is divided into the feeding chamber and the reaction chamber by the partition plate, so that the reaction efficiency of chlorine trifluoride can be effectively improved, the utilization rate of chlorine is improved, and the purity of chlorine trifluoride is further improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a flow diagram of the present invention FIG. 1 is a process for the preparation of high purity grade chlorine trifluoride provided by the present invention;
FIG. 2 is a schematic diagram of a reaction apparatus used in the present invention.
Icon: 1-chlorine gas dust remover; 2-hydrogen fluoride condenser; 3-a hydrogen fluoride adsorption column; 4-fluorine gas buffer tank; 5-a reactor; 51-fluorine gas feed inlet; 5100-a loading chamber; 5101-a reaction chamber; 52-chlorine feed inlet; 53-chlorine trifluoride gas outlet; 54-an electrical heating blanket; 55-a housing; 56-thermometer; 57-a separator; 6-a condenser; 7-recovery vaporizer; 8-an adsorption column; 9-a precision filter; 10-a rectification column; 11-a storage tank; 12-metering pump.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to specific examples.
The embodiment of the application provides a high-purity chlorine trifluoride's reaction unit, including casing and level set up in baffle in the casing, the baffle will separate charging chamber and the reaction chamber for the intercommunication from top to bottom for the casing, the casing outer wall cover is equipped with the heating member, be provided with fluorine gas feed inlet and chlorine gas feed inlet on the wall of charging chamber, the reaction chamber is provided with chlorine trifluoride gas outlet.
In some embodiments of the present invention, the partition plate is horizontally disposed at an upper middle portion of the reactor.
In some embodiments of the present invention, the partition plate of the reaction apparatus for high-purity chlorine trifluoride is provided with through holes.
In some embodiments of the present invention, in the above reaction apparatus for high-purity chlorine trifluoride, the area of the through-hole is half of the cross-section of the housing.
In some embodiments of the present invention, the heating element of the reaction apparatus for high-purity chlorine trifluoride is an electric heating blanket.
In some embodiments of the present invention, the electric heating blanket is disposed on the entire outer wall of the housing.
In some embodiments of the present invention, the reaction apparatus for high purity grade chlorine trifluoride further comprises a thermometer penetrating the wall of the reaction chamber and disposed in the middle of the housing.
In some embodiments of the present invention, in the reaction apparatus for high-purity chlorine trifluoride, the fluorine gas inlet is disposed through a side wall of the feeding chamber, the fluorine gas inlet extends into a middle portion of the feeding chamber, and a gas outlet end of the fluorine gas inlet is provided with a shower head.
In some embodiments of the present invention, in the reaction apparatus for high-purity chlorine trifluoride, one end of the chlorine gas inlet extends into the chamber from the top wall of the chamber and extends downward by 200mm, and the gas outlet end of the chlorine gas inlet is provided with a spray nozzle.
In some embodiments of the present invention, in the apparatus for reacting high-purity chlorine trifluoride, the outlet of the chlorine trifluoride gas is disposed at the bottom of the reaction chamber.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The purpose of this example is to provide a reactor 5 for high purity chlorine trifluoride, comprising the following structure:
the reactor 5 for high-purity chlorine trifluoride comprises a shell 55, wherein a partition plate 57 is arranged in the shell 55, the partition plate 57 is specifically horizontally arranged at the middle upper part of the reactor 5, the environment in the shell 55 is divided into an upper area and a lower area, a feeding chamber 5100 is arranged at the upper part, a reaction chamber 5101 is arranged at the lower part, the height of the feeding chamber 5100 at the upper part is preferably smaller than that of the reaction chamber 5101 at the lower part, and the feeding chamber 5100 is used as an automatic fluorine gas and chlorine gas mixing temporary storage area; the loading chamber 5100 and the reaction chamber 5101 are communicated with each other through a through hole in the partition plate 57.
An electric heating blanket 54 is sleeved on the outer wall of the reactor 5 and used for heating the charging chamber 5100 and the reaction chamber 5101 to provide a continuous heat source; the electric heating blanket 54 is arranged within a range to cover the outside of the reactor 5 completely to the optimum (without the top and bottom walls). Instead of using an electric heating blanket 54, other heating assemblies may be used as long as uniform heating is achieved in both the loading chamber 5100 and the reaction chamber 5101.
In order to further monitor the reaction in the reactor 5, a thermometer 56 (located in the reaction chamber 5101) is provided at a central position of the housing 55.
Specifically, a fluorine gas feed inlet 51 is formed in the side wall of the feeding chamber 5100, the fluorine gas feed inlet 51 extends into the middle of the feeding chamber 5100, and a nozzle is arranged at the gas outlet end; the top of the shell 55 is provided with a chlorine gas feed inlet 52; one end of the chlorine gas inlet 52 extends into the 200mm position of the charging chamber 5100, and the gas outlet end is provided with a spray head. In addition, the bottom of the reactor 5 is provided with a chlorine trifluoride gas outlet 53;
preferably, the partition 57 is uniformly provided with through holes having an area half of the inner diameter of the reactor 5, and the through holes are used to communicate the loading chamber 5100 and the reaction chamber 5101.
Example 2
The present embodiment aims to provide a method for purifying high-purity chlorine trifluoride, which comprises the following steps:
s1, condensation: introducing the produced chlorine trifluoride mixed gas into a condenser 6 for condensation, controlling the temperature of the condenser at-25 ℃ and the pressure at-0.03 Mpa, wherein the liquid obtained by condensation is a crude product of chlorine trifluoride, and the non-condensable gas and the unreacted fluorine gas are discharged after being treated by a tail gas purification system;
s2, recovery vaporization: the chlorine trifluoride gas purified in the step S3 passes through a recovery vaporizer 7, the temperature of the recovery vaporizer is controlled at 35 ℃, the pressure is-0.02 Mpa, a trace amount of unreacted fluorine gas and non-condensable gas are further removed, the concentration of chlorine trifluoride is controlled at 96-99%, the recovery vaporizer is heated and vaporized to provide pressure for a low-pressure adsorption tower 8 and a precision filter 9, and the pressure is controlled at the gauge pressure of 0.3 Mpa;
s3, low-pressure adsorption: chlorine trifluoride gas at the outlet of the top of the recovery vaporizer 7 passes through a low-pressure adsorption tower 8 to further adsorb and remove acid substances such as trace hydrogen fluoride impurities, and the content of hydrogen fluoride in a crude product is less than 50PPm after low-pressure adsorption;
s4, filtering: chlorine trifluoride gas from the low-pressure adsorption tower 8 enters a precision filter 9 for filtering solid particles and metal ions, so that solid impurities such as trace solid particles and metal ions are removed, and the contents of the solid particles and the metal ions in a crude product after precision filtration are less than 1 PPm;
s5, rectification: chlorine trifluoride gas from the precision filter 9 enters a 2-stage rectifying tower 10 from the middle part for rectification; controlling the temperature of the first-stage rectifying tower to be 9 ℃, removing heavy component impurities, and controlling the temperature of tower top gas entering the second-stage rectifying tower to be 5 ℃ to remove light component impurities;
the content of chlorine trifluoride in gas at the tower bottom of the secondary rectifying tower can reach more than 99.995 percent through detection, and compared with the rectification in other modes (such as primary rectification, the product purity is 99.9 percent, and the chlorine trifluoride product with higher purity can be provided more effectively.
S6, filling: qualified chlorine trifluoride liquid from the bottom of the rectifying tower 10 is stored in a storage tank 11, is pressurized by a metering pump 12, and is filled into a steel cylinder. In addition, a precision filter is arranged on the metering pump pipeline to remove solid particle impurities possibly existing in the gas pipeline.
Example 3
The present embodiment aims to provide a method for purifying high-purity chlorine trifluoride, which comprises the following steps:
s1, condensation: introducing the produced chlorine trifluoride mixed gas into a condenser 6 for condensation, controlling the temperature of the condenser at minus 40 ℃ and the pressure at 0Mpa, wherein the liquid obtained by condensation is a crude product of chlorine trifluoride, and the non-condensable gas and the unreacted fluorine gas are discharged after being treated by a tail gas purification system;
s2, recovery vaporization: the chlorine trifluoride gas purified in the step S3 passes through a recovery vaporizer 7, the temperature of the recovery vaporizer is controlled at 43 ℃, the pressure is 0.3Mpa, a trace amount of unreacted fluorine gas and non-condensable gas are further removed, the concentration of chlorine trifluoride is controlled at 96 to 99%, the recovery vaporizer is heated and vaporized to provide pressure for a low-pressure adsorption tower 8 and a precision filter 9, and the pressure is controlled at the gauge pressure of 0.4 Mpa;
s3, low-pressure adsorption: chlorine trifluoride gas at the outlet of the top of the recovery vaporizer 7 passes through a low-pressure adsorption tower 8 to further adsorb and remove acid substances such as trace hydrogen fluoride impurities, and the content of hydrogen fluoride in a crude product is less than 50PPm after low-pressure adsorption;
s4, filtering: chlorine trifluoride gas from the low-pressure adsorption tower 8 enters a precision filter 9 for filtering solid particles and metal ions, so that solid impurities such as trace solid particles and metal ions are removed, and the contents of the solid particles and the metal ions in a crude product after precision filtration are less than 1 PPm;
s5, rectification: chlorine trifluoride gas from the precision filter 9 enters a 2-stage rectifying tower 10 from the middle part for rectification; controlling the temperature of the first-stage rectifying tower to be 11 ℃, removing heavy component impurities, controlling the temperature of tower top gas entering the second-stage rectifying tower to be 7 ℃, and removing light component impurities;
the content of chlorine trifluoride in gas at the tower bottom of the secondary rectifying tower can reach more than 99.995 percent through detection, and compared with the rectification in other modes (such as primary rectification, the product purity is 99.9 percent, and the chlorine trifluoride product with higher purity can be provided more effectively.
S6, filling: qualified chlorine trifluoride liquid from the bottom of the rectifying tower 10 is stored in a storage tank 11, is pressurized by a metering pump 12, and is filled into a steel cylinder. In addition, a precision filter is arranged on the metering pump pipeline to remove solid particle impurities possibly existing in the gas pipeline.
Example 4
The present embodiment aims to provide a method for purifying high-purity chlorine trifluoride, which comprises the following steps:
s1, condensation: introducing the produced chlorine trifluoride mixed gas into a condenser 6 for condensation, controlling the temperature of the condenser at minus 50 ℃ and the pressure at 0.01Mpa, wherein the liquid obtained by condensation is a crude product of chlorine trifluoride, and the non-condensable gas and the unreacted fluorine gas are discharged after being treated by a tail gas purification system;
s2, recovery vaporization: the chlorine trifluoride gas purified in the step S3 passes through a recovery vaporizer 7, the temperature of the recovery vaporizer is controlled at 50 ℃, the pressure is 0.5Mpa, a trace amount of unreacted fluorine gas and non-condensable gas are further removed, the concentration of chlorine trifluoride is controlled at 96 to 99%, the recovery vaporizer is heated and vaporized to provide pressure for a low-pressure adsorption tower 8 and a precision filter 9, and the pressure is controlled at the gauge pressure of 0.5 Mpa;
s3, low-pressure adsorption: chlorine trifluoride gas at the outlet of the top of the recovery vaporizer 7 passes through a low-pressure adsorption tower 8 to further adsorb and remove acid substances such as trace hydrogen fluoride impurities, and the content of hydrogen fluoride in a crude product is less than 50PPm after low-pressure adsorption;
s4, filtering: chlorine trifluoride gas from the low-pressure adsorption tower 8 enters a precision filter 9 for filtering solid particles and metal ions, so that solid impurities such as trace solid particles and metal ions are removed, and the contents of the solid particles and the metal ions in a crude product after precision filtration are less than 1 PPm;
s5, rectification: chlorine trifluoride gas from the precision filter 9 enters a 2-stage rectifying tower 10 from the middle part for rectification; controlling the temperature of the first-stage rectifying tower to be 14 ℃, removing heavy component impurities, and controlling the temperature of the overhead gas entering the second-stage rectifying tower to be 9 ℃, and removing light component impurities;
the content of chlorine trifluoride in gas at the tower bottom of the secondary rectifying tower can reach more than 99.995 percent through detection, and compared with the rectification in other modes (such as primary rectification, the product purity is 99.9 percent, and the chlorine trifluoride product with higher purity can be provided more effectively.
S6, filling: qualified chlorine trifluoride liquid from the bottom of the rectifying tower 10 is stored in a storage tank 11, is pressurized by a metering pump 12, and is filled into a steel cylinder. In addition, a precision filter is arranged on the metering pump pipeline to remove solid particle impurities possibly existing in the gas pipeline.
Example 5
The present embodiment aims to provide a method for preparing high-purity chlorine trifluoride, which comprises the following steps:
s1, preparation and purification of fluorine gas: the electrolytic bath is used for automatically producing fluorine gas, and the generated fluorine gas passes through a fluorine gas dust remover, a hydrogen fluoride condenser and a hydrogen fluoride adsorption tower and reaches a fluorine gas buffer tank;
specifically, the temperature of the electrolytic cell is controlled to be 80-85 ℃, the acidity is controlled to be 39%, hydrogen fluoride is automatically added in an interlocking manner by weight, the materials are uniformly added, and the excessive addition of the hydrogen fluoride is greatly reduced. Fluorine gas passes through a fluorine gas dust remover 1, the temperature of the dust remover is normal temperature, dust and electrolyte in the gas are removed, the fluorine gas enters a hydrogen fluoride condenser 2, the temperature of the condenser is controlled to be-70 ℃, a hydrogen fluoride discharging device is arranged at the bottom end of the condenser, automatic discharging can be realized, the hydrogen fluoride is recycled, the cost is greatly reduced, the fluorine gas after primary treatment enters a hydrogen fluoride adsorption tower 3 to further adsorb trace hydrogen fluoride, and the purity of the fluorine gas can be improved to more than 99%. The outlet of the adsorption tower is butted with the buffer tank 4.
S2, preparing and purifying chlorine trifluoride: the fluorine gas in the buffer tank enters a reactor (shown in example 1) with a novel structure, and is subjected to chemical combination reaction with high-purity chlorine gas;
wherein, the pressure of the fluorine gas buffer tank 4 is-0.02 Mpa; the fluorine gas conversion rate is higher than 99 percent; the ratio of fluorine to chlorine was about 2.98:1, and the chlorine concentration was 99.999%.
S3, condensation: condensing the chlorine trifluoride mixed gas prepared in the step S2 by using a condenser 6, controlling the temperature of the condenser to be-25 to-50 ℃, controlling the pressure to be-0.03 to 0.01Mpa, wherein the liquid obtained by condensation is a crude product of chlorine trifluoride, and the non-condensable gas and the unreacted fluorine gas are discharged after being treated by a tail gas purification system;
s4, recovery vaporization: the chlorine trifluoride gas purified in the step S3 passes through a recovery vaporizer 7, the temperature of the recovery vaporizer is controlled to 35 to 50 ℃, the pressure is-0.02 to 0.5Mpa, trace amounts of unreacted fluorine gas and non-condensable gas are further removed, the concentration of chlorine trifluoride is controlled to 96 to 99%, the recovery vaporizer is heated and vaporized to provide pressure to a low-pressure adsorption tower 8 and a precision filter 9, and the pressure is controlled to be 0.3 to 0.5 Mpa;
s5, low-pressure adsorption: chlorine trifluoride gas at the outlet of the top of the recovery vaporizer 7 passes through a low-pressure adsorption tower 8 to further adsorb and remove acid substances such as trace hydrogen fluoride impurities, and the content of hydrogen fluoride in a crude product is less than 50PPm after low-pressure adsorption;
s7, rectification: chlorine trifluoride gas from the precision filter 9 enters a 2-stage rectifying tower 10 from the middle part for rectification;
controlling the temperature of the first-stage rectifying tower to be 9-14 ℃, removing heavy component impurities, and controlling the temperature of tower top gas entering the second-stage rectifying tower to be 5-9 ℃, removing light component impurities;
the content of chlorine trifluoride in gas at the tower bottom of the secondary rectifying tower can reach more than 99.995 percent through detection, and compared with the rectification in other modes (such as primary rectification, the product purity is 99.9, and the chlorine trifluoride product with higher purity can be provided more effectively.
S8, filling: qualified chlorine trifluoride liquid from the bottom of the rectifying tower 10 is stored in a storage tank 11, is pressurized by a metering pump 12, and is filled into a steel cylinder.
In addition, a precision filter is arranged on the metering pump pipeline to remove solid particle impurities possibly existing in the gas pipeline.
Example 6
The present embodiment aims to provide a method for preparing high-purity chlorine trifluoride, which comprises the following steps:
s1, preparation and purification of fluorine gas: the electrolytic bath is used for automatically producing fluorine gas, and the generated fluorine gas passes through a fluorine gas dust remover, a hydrogen fluoride condenser and a hydrogen fluoride adsorption tower and reaches a fluorine gas buffer tank;
specifically, the temperature of the electrolytic cell is controlled to be 87-92 ℃, the acidity is controlled to be 40%, hydrogen fluoride is automatically added in an interlocking manner by weight, the materials are uniformly added, and the excessive addition of the hydrogen fluoride is greatly reduced. Fluorine gas passes through a fluorine gas dust remover 1, the temperature of the dust remover is normal temperature, dust and electrolyte in the gas are removed, the fluorine gas enters a hydrogen fluoride condenser 2, the temperature of the condenser is controlled to be-85 ℃, a hydrogen fluoride discharging device is arranged at the bottom end of the condenser, automatic discharging can be realized, the hydrogen fluoride is recycled, the cost is greatly reduced, the fluorine gas after primary treatment enters a hydrogen fluoride adsorption tower 3 to further adsorb trace hydrogen fluoride, and the purity of the fluorine gas can be improved to more than 99%. The outlet of the adsorption tower is butted with the buffer tank 4.
S2, preparing and purifying chlorine trifluoride: the fluorine gas in the buffer tank enters a reactor (shown in example 1) with a novel structure, and is subjected to chemical combination reaction with high-purity chlorine gas;
wherein, the pressure of the fluorine gas buffer tank 4 is 0 Mpa; the fluorine gas conversion rate is higher than 99 percent; the ratio of fluorine to chlorine is about 3:1, the chlorine concentration is 99.999 percent.
S3, condensation: condensing the chlorine trifluoride mixed gas prepared in the step S2 by using a condenser 6, controlling the temperature of the condenser to be-25 to-50 ℃, controlling the pressure to be-0.03 to 0.01Mpa, wherein the liquid obtained by condensation is a crude product of chlorine trifluoride, and the non-condensable gas and the unreacted fluorine gas are discharged after being treated by a tail gas purification system;
s4, recovery vaporization: the chlorine trifluoride gas purified in the step S3 passes through a recovery vaporizer 7, the temperature of the recovery vaporizer is controlled to 35 to 50 ℃, the pressure is-0.02 to 0.5Mpa, trace amounts of unreacted fluorine gas and non-condensable gas are further removed, the concentration of chlorine trifluoride is controlled to 96 to 99%, the recovery vaporizer is heated and vaporized to provide pressure to a low-pressure adsorption tower 8 and a precision filter 9, and the pressure is controlled to be 0.3 to 0.5 Mpa;
s5, low-pressure adsorption: chlorine trifluoride gas at the outlet of the top of the recovery vaporizer 7 passes through a low-pressure adsorption tower 8 to further adsorb and remove acid substances such as trace hydrogen fluoride impurities, and the content of hydrogen fluoride in a crude product is less than 50PPm after low-pressure adsorption;
s6, rectification: chlorine trifluoride gas from the precision filter 9 enters a 2-stage rectifying tower 10 from the middle part for rectification;
controlling the temperature of the first-stage rectifying tower to be 9-14 ℃, removing heavy component impurities, and controlling the temperature of tower top gas entering the second-stage rectifying tower to be 5-9 ℃, removing light component impurities;
the content of chlorine trifluoride in gas at the tower bottom of the secondary rectifying tower can reach more than 99.995 percent through detection, and compared with the rectification in other modes (such as primary rectification, the product purity is 99.9 percent, and the chlorine trifluoride product with higher purity can be provided more effectively.
S7, filling: qualified chlorine trifluoride liquid from the bottom of the rectifying tower 10 is stored in a storage tank 11, is pressurized by a metering pump 12, and is filled into a steel cylinder.
In addition, a precision filter is arranged on the metering pump pipeline to remove solid particle impurities possibly existing in the gas pipeline.
Example 7
The present embodiment aims to provide a method for preparing high-purity chlorine trifluoride, which comprises the following steps:
s1, preparation and purification of fluorine gas: the electrolytic bath is used for automatically producing fluorine gas, and the generated fluorine gas passes through a fluorine gas dust remover, a hydrogen fluoride condenser and a hydrogen fluoride adsorption tower and reaches a fluorine gas buffer tank;
specifically, the temperature of the electrolytic cell is controlled to be 95-100 ℃, the acidity is controlled to be 41%, hydrogen fluoride is automatically added in an interlocked manner by weight, the materials are uniformly added, and the excessive addition of the hydrogen fluoride is greatly reduced. Fluorine gas passes through a fluorine gas dust remover 1, the temperature of the dust remover is normal temperature, dust and electrolyte in the gas are removed, the fluorine gas enters a hydrogen fluoride condenser 2, the temperature of the condenser is controlled at-100 ℃, a hydrogen fluoride discharging device is arranged at the bottom end of the condenser, automatic discharging can be realized, the hydrogen fluoride is recycled, the cost is greatly reduced, the fluorine gas after primary treatment enters a hydrogen fluoride adsorption tower 3 to further adsorb trace hydrogen fluoride, and the purity of the fluorine gas can be improved to more than 99%. The outlet of the adsorption tower is butted with the buffer tank 4.
S2, preparing and purifying chlorine trifluoride: the fluorine gas in the buffer tank enters a reactor (shown in example 1) with a novel structure, and is subjected to chemical combination reaction with high-purity chlorine gas;
wherein, the pressure of the fluorine gas buffer tank 4 is 0.02 Mpa; the fluorine gas conversion rate is higher than 99 percent; fluorine to chlorine ratio of about 3.02: 1, the chlorine concentration is 99.999 percent.
S3, condensation: condensing the chlorine trifluoride mixed gas prepared in the step S2 by using a condenser 6, controlling the temperature of the condenser to be-25 to-50 ℃, controlling the pressure to be-0.03 to 0.01Mpa, wherein the liquid obtained by condensation is a crude product of chlorine trifluoride, and the non-condensable gas and the unreacted fluorine gas are discharged after being treated by a tail gas purification system;
s4, recovery vaporization: the chlorine trifluoride gas purified in the step S3 passes through a recovery vaporizer 7, the temperature of the recovery vaporizer is controlled to 35 to 50 ℃, the pressure is-0.02 to 0.5Mpa, trace amounts of unreacted fluorine gas and non-condensable gas are further removed, the concentration of chlorine trifluoride is controlled to 96 to 99%, the recovery vaporizer is heated and vaporized to provide pressure to a low-pressure adsorption tower 8 and a precision filter 9, and the pressure is controlled to be 0.3 to 0.5 Mpa;
s5, low-pressure adsorption: chlorine trifluoride gas at the outlet of the top of the recovery vaporizer 7 passes through a low-pressure adsorption tower 8 to further adsorb and remove acid substances such as trace hydrogen fluoride impurities, and the content of hydrogen fluoride in a crude product is less than 50PPm after low-pressure adsorption;
s6, rectification: chlorine trifluoride gas from the precision filter 9 enters a 2-stage rectifying tower 10 from the middle part for rectification;
controlling the temperature of the first-stage rectifying tower to be 9-14 ℃, removing heavy component impurities, and controlling the temperature of tower top gas entering the second-stage rectifying tower to be 5-9 ℃, removing light component impurities;
the content of chlorine trifluoride in gas at the tower bottom of the secondary rectifying tower can reach more than 99.995 percent through detection, and compared with the rectification in other modes (such as primary rectification, the product purity is 99.9 percent, and the chlorine trifluoride product with higher purity can be provided more effectively.
S7, filling: qualified chlorine trifluoride liquid from the bottom of the rectifying tower 10 is stored in a storage tank 11, is pressurized by a metering pump 12, and is filled into a steel cylinder.
In addition, a precision filter is arranged on the metering pump pipeline to remove solid particle impurities possibly existing in the gas pipeline.
The purity of fluorine gas in this application can influence the utilization ratio of fluorine gas and the purity of final product chlorine trifluoride, and the higher the purity of fluorine gas, its utilization ratio is higher, and chlorine trifluoride directly influences high-purity level chlorine trifluoride product quality especially in the index control of chlorine trifluoride in purification process, solid-state particulate matter and metal ion in the product gas.
Example 8
The purpose of this example is to provide a purification system suitable for use in examples 2, 3 and 4.
The purification system specifically comprises a condensation system, a recovery vaporization system, an adsorption system, a filtration system and a rectification system, and the five parts are connected in sequence. The condensing system comprises a condenser, in particular a condenser 6. The recovery vaporization system includes a recovery vaporizer, specifically a recovery vaporizer 7. The adsorption system comprises a low-pressure adsorption tower and a precision filter, and specifically comprises a low-pressure adsorption tower 8 and a precision filter 9 which are connected in sequence. The rectifying system comprises a rectifying tower 10, and further comprises a storage tank 11 and a metering pump 12 which are sequentially connected with the rectifying tower 10. Wherein, the condenser is provided with a tubular structure, and the recovery vaporizer is externally provided with a jacket.
Example 9
The purpose of this example was to provide a production system suitable for example 5, example 6 and example 7.
The preparation system comprises a fluorine gas system, a reaction device and a purification system, wherein the purification system comprises a fluorine gas system as shown in example 8, and the reaction device comprises a fluorine gas system as shown in example 1.
The fluorine gas system specifically comprises an electrolytic bath, a fluorine gas dust remover 1, a hydrogen fluoride condenser 2, a hydrogen fluoride adsorption tower 3 and a fluorine gas buffer tank 4. Wherein, the electrolytic cell is provided with an automatic system, and the feeding mode is weight interlocking automatic feeding. The bottom end of the hydrogen fluoride condenser is provided with a hydrogen fluoride discharging device, and the inside of the hydrogen fluoride absorption tower is provided with an adsorbent fluoride salt.
Comparative example 1
The difference between the comparative example and the example 1 is that whether a hydrogen fluoride adsorption system is arranged in the fluorine gas purification stage or not specifically comprises the following steps:
s1, preparation of fluorine gas: the electrolytic bath is used for automatically producing fluorine gas, and the generated fluorine gas passes through a fluorine gas dust remover and a hydrogen fluoride condenser and reaches a fluorine gas buffer tank; the temperature of the electrolytic cell is controlled to be 95-105 ℃, the acidity is controlled to be 41%, hydrogen fluoride is automatically added in an interlocking manner by weight, the materials are uniformly added, and the excessive addition of the hydrogen fluoride is greatly reduced. The gas passes through the dust remover 1, and the outlet of the hydrogen fluoride condenser 2 is butted with the buffer tank 4.
S2, preparing chlorine trifluoride: fluorine gas in the buffer tank enters a reactor with a novel structure to carry out chemical combination reaction with high-purity chlorine gas; the pressure of the fluorine gas buffer tank 4 is-0.02 Mpa; the fluorine gas conversion rate is higher than 99 percent; the ratio of fluorine to chlorine was about 3:1, and the chlorine concentration was 99.999%.
S3, condensation: condensing the chlorine trifluoride mixed gas by using a condenser 7, controlling the temperature of the condenser to be between 25 ℃ below zero and 50 ℃ below zero, controlling the pressure to be between 0.03MPa and 0.01MPa, wherein the liquid obtained by condensation is a crude product of chlorine trifluoride, and exhausting the non-condensable gas and unreacted fluorine gas after the non-condensable gas and the unreacted fluorine gas are treated by a tail gas purification system;
s4, recovery vaporization: the prepared chlorine trifluoride gas passes through a recovery vaporizer 7, the temperature of the recovery vaporizer is controlled to be 35-50 ℃, the pressure is-0.02-0.5 MPa, trace unreacted fluorine gas and non-condensable gas are further removed, the concentration of the chlorine trifluoride is controlled to be 99%, the recovery vaporizer is heated and vaporized to provide pressure for a low-pressure adsorption tower 8, and the pressure is controlled to be 0.3-0.5 MPa;
s5, low-pressure adsorption: chlorine trifluoride gas at the outlet of the top of the recovery vaporizer 7 passes through a low-pressure adsorption tower 8 to further adsorb and remove acid substances such as trace hydrogen fluoride impurities, and the content of hydrogen fluoride in a crude product is less than 300PPm after low-pressure adsorption;
s6, rectification: chlorine trifluoride gas from the low-pressure adsorption tower 8 enters a 2-stage rectifying tower 9 from the middle part for rectification;
controlling the temperature of the first-stage rectifying tower to be 9-14 ℃, removing heavy component impurities, and controlling the temperature of tower top gas entering the second-stage rectifying tower to be 5-9 ℃, removing light component impurities;
the content of chlorine trifluoride in gas at the tower bottom of the secondary rectifying tower can reach more than 99.995 percent through detection, and compared with the rectification in other modes (such as primary rectification, the product purity is 99.9 percent, and the chlorine trifluoride product with higher purity can be provided more effectively.
S7, filling: qualified chlorine trifluoride liquid from the tower bottom of the rectifying tower 9 is stored in a storage tank 10, then is pressurized by a metering pump 11, and then is filled into a steel cylinder.
Comparative example 2
The difference between the comparative example and the examples 1 and 2 lies in the difference of the temperature and acidity of the electrolytic bath and the existence of the hydrogen fluoride adsorption tower, and the method specifically comprises the following steps:
s1, preparation of fluorine gas: the electrolytic cell automatically produces fluorine gas. The fluorine gas passes through a fluorine gas dust remover and a hydrogen fluoride condenser and reaches a fluorine gas buffer tank;
the temperature of the electrolytic cell is controlled to be 105-110 ℃, the acidity is controlled to be 44%, hydrogen fluoride is automatically added in an interlocking manner by weight, the materials are uniformly added, and the excessive addition of the hydrogen fluoride is greatly reduced. Fluorine gas passes through a fluorine gas dust remover 1, the temperature of the dust remover is normal temperature, dust and electrolyte in the gas are removed, the gas enters a hydrogen fluoride condenser 2, the temperature of the condenser is controlled at-90 ℃, a hydrogen fluoride discharging device is arranged at the bottom end, automatic discharging can be realized, the hydrogen fluoride is recycled, the cost is greatly reduced, and the purity of the fluorine gas can be improved to more than 98%. The outlet of the hydrogen fluoride condenser 2 is butted with a buffer tank 4.
S2, preparing chlorine trifluoride: fluorine gas in the buffer tank enters a reactor with a novel structure to carry out chemical combination reaction with high-purity chlorine gas; the pressure of the fluorine gas buffer tank 4 is-0.02 Mpa; the fluorine gas conversion rate is higher than 99 percent; the ratio of fluorine to chlorine is about 3:1, the chlorine concentration is 99.999 percent.
S3, condensation: condensing the chlorine trifluoride mixed gas by using a condenser 7, controlling the temperature of the condenser to be between 25 ℃ below zero and 50 ℃ below zero, controlling the pressure to be between 0.03MPa and 0.01MPa, wherein the liquid obtained by condensation is a crude product of chlorine trifluoride, and exhausting the non-condensable gas and unreacted fluorine gas after the non-condensable gas and the unreacted fluorine gas are treated by a tail gas purification system;
s4, recovery vaporization: the prepared chlorine trifluoride gas passes through a recovery vaporizer 7, the temperature of the recovery vaporizer is controlled to be 35-50 ℃, the pressure is-0.02-0.5 MPa, trace unreacted fluorine gas and non-condensable gas are further removed, the concentration of the chlorine trifluoride is controlled to be 99%, the recovery vaporizer is heated and vaporized to provide pressure for a low-pressure adsorption tower 8, and the pressure is controlled to be 0.3-0.5 MPa;
s5, low-pressure adsorption: chlorine trifluoride gas at the outlet of the top of the recovery vaporizer 7 passes through a low-pressure adsorption tower 8 to further adsorb and remove acid substances such as trace hydrogen fluoride impurities, and the content of hydrogen fluoride in a crude product is less than 300PPm after low-pressure adsorption;
s6, rectification: chlorine trifluoride gas from the low-pressure adsorption tower 8 enters a 2-stage rectifying tower 9 from the middle part for rectification;
controlling the temperature of the first-stage rectifying tower to be 9-14 ℃, removing heavy component impurities, and controlling the temperature of tower top gas entering the second-stage rectifying tower to be 5-9 ℃, removing light component impurities;
the content of chlorine trifluoride in gas at the tower bottom of the secondary rectifying tower can reach more than 99.995 percent through detection, and compared with the rectification in other modes (such as primary rectification, the product purity is 99.9 percent, and the chlorine trifluoride product with higher purity can be provided more effectively.
S7, filling: qualified chlorine trifluoride liquid from the tower bottom of the rectifying tower 9 is stored in a storage tank 10, then is pressurized by a metering pump 11, and then is filled into a steel cylinder.
Examples of effects
The purpose of this effect example is to examine the purity of chlorine trifluoride in examples 2 to 7, comparative example 1 and comparative example 2.
The chlorine trifluoride was detected by GC-126PDD helium ion gas chromatography, and the detection parameters were as follows: a first separation channel; the set temperature of the first pre-adsorption column 1 is 45 ℃; the set temperature of the second fluorine-chlorine oil separation column 2 is 45 ℃; the temperature of the third Ag/AL2O3 adsorption column 3 is set to be 50 ℃; the set temperature of a fourth 5A molecular sieve column 4 is 60 ℃; in actual measurement, the corresponding parameters in comparative example 1 and comparative example 2 were the same as those in example 3 and example 6. Analyzing conditions by an instrument, wherein the carrier gas adopts purified ultrapure helium; the flow rate of the column is 30 ml/min; analyzing conditions by using a PDHID pulse helium ionization detector; setting the temperature to be 120 ℃; the instrument analyzes the condition, and the sample gas is conditionally loaded into the chromatograph in positive pressure steady flow injection. The results are shown in table 1:
TABLE 1
As can be seen from Table 1, the purity of the chlorine trifluoride gas prepared by the purification system and the purification method provided by the present application is high, reaching 99.995% or more, and can meet the use requirement of high-purity chlorine trifluoride gas. The data from comparative example 2 show that the temperature and acidity of the electrolyzer and the presence or absence of the hydrogen fluoride adsorption column affect the purity of the fluorine gas, and thus the utilization rate of the fluorine gas and the purity of the chlorine trifluoride product. This is because the purity of fluorine gas is low, which affects the reaction efficiency, impurities in fluorine gas react at high temperature, which lowers the utilization rate of fluorine gas, and chlorine trifluoride raw gas contains many impurities, and under the same parameter purification conditions, the final product contains many impurities and has low purity. Compared with the comparative example 1, the embodiment 1 has the advantages that a hydrogen fluoride adsorption system is added in the fluorine gas purification process, so that trace hydrogen fluoride impurities can be removed, the hydrogen fluoride content in the product is greatly reduced, and the product purity is improved. Compared with the comparative examples 1 and 2, the metal ion index in the product is reduced to 1PPmw after the metal ions in the gas are filtered by the precision filter added in the purification process.
The purification system and the purification method for high-purity chlorine trifluoride have the following advantages:
first, according to the purification method of high-purity chlorine trifluoride provided by the application, chlorine trifluoride gas passes through a condensation section, a vaporization section, an adsorption system and a rectification system, so that the utilization rate of fluorine gas is over 98%, and the purity of chlorine trifluoride gas is 99.995%.
The purification system of high-purity chlorine trifluoride provided by the application has the advantages that the fluorine gas dust remover is additionally arranged at the outlet of the electrolytic cell, the pipe blocking rate can be effectively reduced, the hydrogen fluoride condenser is additionally arranged, the hydrogen fluoride utilization rate can be recovered, a large amount of cost is saved, the hydrogen fluoride adsorption tower is additionally arranged, the content of hydrogen fluoride in fluorine gas can be effectively further reduced, the filter is additionally arranged, the content of solid particles and metal ions in product gas can be effectively further reduced, the content of impurities such as hydrogen fluoride, solid particle substances and metal ions in the finally obtained chlorine trifluoride gas is extremely low, and the purity of the chlorine trifluoride gas reaches 99.995%.
Third, in the purification system provided by the application, the purity of the purified fluorine gas is high, the reaction rate with the high-purity chlorine gas is high, the reaction is more sufficient, and the utilization rate of the fluorine gas during the reaction is higher.
The purification system provided by the application can effectively reduce the blockage of the reactor caused by the vaporized potassium hydrogen fluoride when meeting cold by arranging the fluorine gas dust remover, thereby reducing the maintenance rate of the reactor;
the purification system provided by the application is additionally provided with the hydrogen fluoride adsorption tower, so that trace hydrogen fluoride in the product gas is fully adsorbed, and the quality index of the hydrogen fluoride in the product gas is greatly reduced;
the purification system provided by the application is additionally provided with the precision filter, so that trace solid particles and metal ions in the product gas are fully filtered, and the quality indexes of the solid particles and the metal ions in the product gas are greatly reduced;
the effect is seven, and this application has adopted second grade rectification, compares in original traditional one-level rectification, and product purity is higher, and the impurity is still less.
The preparation method provided by the application can effectively control the purity of the produced fluorine gas by controlling the specific temperature and acidity of the electrolytic cell, and ensures the high efficiency and purity of the subsequent reaction.
The embodiments described above are some, but not all embodiments of the utility model. The detailed description of the embodiments of the present invention is not intended to limit the scope of the utility model as claimed, but is merely representative of selected embodiments of the utility model. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (10)
1. High-purity level chlorine trifluoride's reaction unit, its characterized in that, including casing and level set up in baffle in the casing, the baffle will the casing is separated the charging chamber and the reaction chamber of intercommunication from top to bottom, casing outer wall cover is equipped with heating member, be provided with fluorine gas feed inlet and chlorine gas feed inlet on the wall of charging chamber, the reaction chamber is provided with chlorine trifluoride gas outlet.
2. The apparatus for reacting high purity grade chlorine trifluoride according to claim 1, wherein said partition is horizontally disposed at the middle-upper portion of the reactor.
3. The apparatus for reacting high purity chlorine trifluoride according to claim 1, wherein said partition plate is provided with through holes.
4. The apparatus for reacting high purity grade chlorine trifluoride according to claim 3, wherein said through holes have an area which is half of the cross section of the housing.
5. The apparatus as claimed in claim 1, wherein the heating element is an electric heating blanket.
6. The apparatus of claim 5, wherein the electric blanket is wrapped around the entire outer wall of the housing.
7. The apparatus for reacting high purity grade chlorine trifluoride according to claim 1, further comprising a thermometer disposed through a wall of said reaction chamber and in a middle portion of said housing.
8. The apparatus for reacting high purity chlorine trifluoride according to claim 1, wherein said fluorine gas inlet is formed through a side wall of said feed chamber, said fluorine gas inlet is formed at a middle portion thereof in the feed chamber, and a shower head is provided at an outlet end of said fluorine gas inlet.
9. The apparatus as claimed in claim 1, wherein the chlorine gas inlet has an end extending downward 200mm from the top wall of the chamber and a gas outlet end provided with a shower nozzle.
10. The apparatus for reacting high purity chlorine trifluoride according to claim 1, wherein said chlorine trifluoride gas outlet is provided at the bottom of said reaction chamber.
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| CN114950301B (en) * | 2022-05-31 | 2023-05-02 | 中船(邯郸)派瑞特种气体股份有限公司 | Iodine pentafluoride synthesizer |
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