CN111704108A - Continuous production process of high-purity chlorine - Google Patents
Continuous production process of high-purity chlorine Download PDFInfo
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- CN111704108A CN111704108A CN202010623553.8A CN202010623553A CN111704108A CN 111704108 A CN111704108 A CN 111704108A CN 202010623553 A CN202010623553 A CN 202010623553A CN 111704108 A CN111704108 A CN 111704108A
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- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000000460 chlorine Substances 0.000 title claims abstract description 57
- 229910052801 chlorine Inorganic materials 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000010924 continuous production Methods 0.000 title claims abstract description 24
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000003463 adsorbent Substances 0.000 claims abstract description 33
- 238000001179 sorption measurement Methods 0.000 claims abstract description 28
- 239000012535 impurity Substances 0.000 claims abstract description 27
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910001868 water Inorganic materials 0.000 claims abstract description 24
- 238000002309 gasification Methods 0.000 claims abstract description 19
- 150000001875 compounds Chemical class 0.000 claims abstract description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 239000007791 liquid phase Substances 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 32
- 239000002808 molecular sieve Substances 0.000 claims description 30
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 30
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 27
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000003513 alkali Substances 0.000 claims description 7
- 230000008929 regeneration Effects 0.000 claims description 6
- 238000011069 regeneration method Methods 0.000 claims description 6
- 238000009924 canning Methods 0.000 claims description 3
- 230000006835 compression Effects 0.000 claims description 3
- 238000007906 compression Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000013329 compounding Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000005049 silicon tetrachloride Substances 0.000 description 3
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000002274 desiccant Substances 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000012320 chlorinating reagent Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/075—Purification ; Separation of liquid chlorine
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0743—Purification ; Separation of gaseous or dissolved chlorine
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Separation Of Gases By Adsorption (AREA)
Abstract
The invention provides a continuous production process of high-purity chlorine, which comprises the following steps: step S1, introducing liquid chlorine from a liquid phase space valve of an industrial liquid chlorine tank into a gasification device, and gasifying at a first temperature to obtain gasified nitrogen; step S2, introducing the nitrogen obtained in the step S1 into an adsorption device, and adsorbing by a compound adsorbent to obtain crude high-purity chlorine with the water content of less than or equal to 0.3 ppmv; step S3, introducing the crude high-purity chlorine obtained in the step S2 into a primary rectifying device, and rectifying and removing heavy component impurities in the crude high-purity chlorine under a first pressure to obtain primary high-purity chlorine; and step S4, introducing the primary high-purity chlorine gas obtained in the step S3 into a secondary rectification device, and rectifying and removing light component impurities in the primary high-purity chlorine gas under a second pressure to obtain secondary high-purity chlorine gas. The invention solves the technical problem of low yield in the traditional high-purity chlorine production process by optimizing the high-purity chlorine production process.
Description
Technical Field
The invention relates to the technical field of preparation of high-purity gas, in particular to a continuous production process of high-purity chlorine.
Background
Chlorine is one of the main products in the chlor-alkali industry, and is a strong oxidant and a chlorinating agent. The high-purity chlorine gas is high-purity gas obtained by purifying industrial liquid chlorine and is used as standard gas and correction gas; in addition, the high-purity chlorine can also be applied to the fields of microelectronics, optical fiber cables, high-temperature superconductivity and high-performance alloy smelting, and the like, and the advanced scientific and technological fields of related industry, basic scientific research and the like.
For a long time, high-purity chlorine in China always depends on import, and the purity of the high-purity chlorine produced by an adsorption purification method in China only exists in 80-90 years, and can reach 99.996%. The adsorption method for preparing high-purity chlorine needs to remove impurities in industrial chlorine deeply, and the impurities comprise water, oxygen, nitrogen, carbon dioxide, carbon monoxide, hydrogen, methane and other gases. The adsorption method is to remove carbon dioxide, hydrocarbons and metal ions thereof by adopting chemically treated zeolite adsorption, remove water by using a drying agent and zeolite secondary adsorption, condense and separate low-boiling-point impurities, and obtain high-purity chlorine by low-temperature bottling. The preparation of the high-purity chlorine prepared by the adsorption method needs to prepare a drying agent and an adsorbent which are not corroded by the chlorine and do not cause chlorination reaction, and select proper process conditions for drying, adsorption, regeneration and condensation, and the like, which are the problems of great technical difficulty and a lot of research contents.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a continuous production process of high-purity chlorine, which aims to solve the technical problem of low yield of the traditional high-purity chlorine production process in the related technology.
The invention provides a continuous production process of high-purity chlorine, which comprises the following steps:
step S1, introducing liquid chlorine from a liquid phase space valve of an industrial liquid chlorine tank into a gasification device, and gasifying at a first temperature to obtain gasified nitrogen;
step S2, introducing the nitrogen obtained in the step S1 into an adsorption device, and adsorbing by a compound adsorbent to obtain crude high-purity chlorine with the water content of less than or equal to 0.3 ppmv;
step S3, introducing the crude high-purity chlorine obtained in the step S2 into a primary rectifying device, and rectifying and removing heavy component impurities in the crude high-purity chlorine under a first pressure to obtain primary high-purity chlorine;
and step S4, introducing the primary high-purity chlorine gas obtained in the step S3 into a secondary rectification device, and rectifying and removing light component impurities in the primary high-purity chlorine gas under a second pressure to obtain secondary high-purity chlorine gas.
Optionally, the first temperature is in a range of 20-60 ℃.
Optionally, the built adsorbent is a built combined adsorbent of a molecular sieve and activated alumina.
Optionally, the mass fraction ratio of the molecular sieve to the activated alumina is 4:6 to 7: 3.
Optionally, the first pressure is 0.6 to 0.8 MPa.
Optionally, the second pressure is 0.4-0.6 MPa.
Optionally, the height of the first rectifying device is 10-14 m; and/or the presence of a gas in the gas,
the height of the second rectifying device is 10-14 m.
Optionally, the adsorption device comprises a use tank and a regeneration tank which are connected in parallel between the gasification device and the primary rectification device through gas circuits.
Optionally, the first rectification device comprises a first refrigerating unit and a first heating element, and the first refrigerating unit is arranged at the top of the first rectification device; the first heating device is additionally arranged at the bottom of the first rectifying device; and/or the presence of a gas in the gas,
the second rectifying device comprises a second refrigerating unit and a second heating element, the second refrigerating unit is arranged at the top of the second rectifying device, and the second heating element is arranged at the bottom of the second rectifying device.
Optionally, the continuous production process further comprises:
step S5, bottling the secondary high-purity chlorine gas obtained in the step S4 by a compression canning system to obtain bottled high-purity liquid nitrogen;
step S6, introducing heavy component impurities removed by the primary rectifying device into a tail gas treatment device, and treating with alkali liquor;
and step S7, introducing the light component impurities removed by the secondary rectification device into a tail gas treatment device, and treating with alkali liquor.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a continuous production process of high-purity chlorine, which takes industrial liquid chlorine as an initial raw material and obtains the high-purity chlorine meeting the index through the processes of gasification, single-stage adsorption, secondary rectification and the like, the whole process is simple and easy to operate, and the continuous industrial production of the high-purity chlorine can be realized; the pollution source in the production process is less, and the obtained product has high quality; the water content of the obtained high-purity chlorine gas is lower than 0.3ppmv, and the purity reaches 99.999 percent.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly apparent, the technical solutions of the present invention are further described below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
At present, no formal high-purity chlorine manufacturers exist in China in the related technology, only the research center of special gas of the Ministry of Dali Guangdong has a small amount of production technology for intermittently preparing high-purity chlorine by an adsorption method, and the yield is basically 5 tons/year. The China gas Association has a large market for the use of special gas, the annual usage amount is about 300 tons, and the total sales of foreign famous gas sellers such as Prikex, Linde gas, air products company and French liquefied air group in China can reach 300 tons per year. Thus, the China market for high purity chlorine is basically monopolized by foreign manufacturers. Based on the technical scheme, the invention provides a continuous production process of high-purity chlorine, and realizes a production line of high-purity chlorine capable of producing 1000 tons per year.
Based on the above, the invention provides a continuous production process of high-purity chlorine gas, which comprises the following steps:
step S1, introducing liquid chlorine from a liquid phase space valve of an industrial liquid chlorine tank into a gasification device, and gasifying at a first temperature to obtain gasified nitrogen;
step S2, introducing the nitrogen obtained in the step S1 into an adsorption device, and adsorbing by a compound adsorbent to obtain crude high-purity chlorine with the water content of less than or equal to 0.3 ppmv;
step S3, introducing the crude high-purity chlorine obtained in the step S2 into a primary rectifying device, and rectifying and removing heavy component impurities in the crude high-purity chlorine under a first pressure to obtain primary high-purity chlorine;
and step S4, introducing the primary high-purity chlorine gas obtained in the step S3 into a secondary rectification device, and rectifying and removing light component impurities in the primary high-purity chlorine gas under a second pressure to obtain secondary high-purity chlorine gas.
Optionally, the first temperature is in a range of 20-60 ℃. For example, but not limited to, the first temperature is in the range of 31-40 ℃.
Optionally, the built adsorbent is a built combined adsorbent of a molecular sieve and activated alumina.
Optionally, the mass fraction ratio of the molecular sieve to the activated alumina is 4:6 to 7: 3. For example, but not limiting of, the ratio of the mass fractions of the molecular sieve and the activated alumina is 6: 4.
Optionally, the first pressure is 0.6 to 0.8 MPa.
Optionally, the second pressure is 0.4-0.6 MPa.
Optionally, the height of the first rectifying device is 10-14 m; and/or the presence of a gas in the gas,
the height of the second rectifying device is 10-14 m.
Optionally, the adsorption device comprises a use tank and a regeneration tank which are connected in parallel between the gasification device and the primary rectification device through gas circuits.
Optionally, the first rectification device comprises a first refrigerating unit and a first heating element, and the first refrigerating unit is arranged at the top of the first rectification device; the first heating device is additionally arranged at the bottom of the first rectifying device; and/or the presence of a gas in the gas,
the second rectifying device comprises a second refrigerating unit and a second heating element, the second refrigerating unit is arranged at the top of the second rectifying device, and the second heating element is arranged at the bottom of the second rectifying device.
Optionally, the continuous production process further comprises:
step S5, bottling the secondary high-purity chlorine gas obtained in the step S4 by a compression canning system to obtain bottled high-purity liquid nitrogen;
step S6, introducing heavy component impurities removed by the primary rectifying device into a tail gas treatment device, and treating with alkali liquor;
and step S7, introducing the light component impurities removed by the secondary rectification device into a tail gas treatment device, and treating with alkali liquor.
The embodiment of the invention provides a continuous production process of high-purity chlorine, which takes industrial liquid chlorine as an initial raw material and obtains the high-purity chlorine meeting the index through the processes of gasification, single-stage adsorption, secondary rectification and the like, the whole process is simple and easy to operate, and the continuous industrial production of the high-purity chlorine can be realized; the pollution source in the production process is less, and the obtained product has high quality; the water content of the obtained high-purity chlorine gas is lower than 0.3ppmv, and the purity reaches 99.999 percent.
Specifically, for the gasification process, in order to improve the mass transfer driving force of gas in the single-stage adsorption process and the two-stage rectification process, the temperature of the gasification process is set. Specifically, when the first temperature is too low, the feeding speed of industrial liquid chlorine is slow, the mass transfer driving force is insufficient, and the yield of the produced high-purity chlorine gas is low; when the first temperature is too high, the pressure in the rectification process is also higher, the relative volatilization of light component impurities is reduced due to the too high rectification pressure, the rectification effect is worsened, the yield of high-purity chlorine is reduced, and the safety risk in the rectification process is also improved due to the too high rectification pressure. Therefore, in the embodiment of the invention, a large number of experiments prove that when the first temperature is 20-60 ℃, a product with qualified product quality can be obtained, and the yield of high-purity chlorine gas is improved.
Specifically, GB5138-2016 states that the mass fraction of water in qualified industrial liquid chlorine products is less than or equal to 0.04% (i.e., the volume fraction is about 1600ppmv), and the water content of high-purity chlorine gas is less than 0.3ppmv, so that a large amount of water needs to be removed in the production process from industrial liquid chlorine to high-purity liquid chlorine. Therefore, for the single-stage adsorption process, in order to remove the moisture in the industrial liquid chlorine to the maximum extent, a compound adsorbent is designed (namely, the molecular sieve and the activated alumina are compounded according to the mass fraction of 4: 6-7: 3). In addition, in the embodiment of the invention, the single-stage adsorption of the high-purity chlorine can be realized by the compound adsorbent, the multi-stage physical adsorption drying in the traditional process is avoided, the simplification of the process is realized, and the effect is excellent.
Specifically, for the secondary rectification process, in order to remove impurities in the chlorine gas with low water content to the maximum extent and reduce the pressure in the rectification process, a secondary distillation process for removing heavy component impurities and then removing light component impurities is designed, so that the pressure of the high-purity chlorine gas after rectification can be reduced (lower than the gasification pressure of GB11984-2008 & ltchlorine safety code & gt, which is 1.0MPa), and the pressure value of the high-purity chlorine gas discharged from a distillation device can meet the national standard; the impurity removal operation of removing the heavy component impurities first and then removing the light component impurities in the embodiment of the invention also avoids the use of a diaphragm compressor in the traditional impurity removal process (removing the light component impurities first and then removing the heavy component impurities), and reduces the product pollution path caused by the diaphragm rupture of the diaphragm compressor.
To more clearly illustrate the technical effects of the continuous production process of high purity chlorine gas proposed by the present invention, the present invention provides the following data for the examples. It should be understood that the data set forth in the following examples are merely intended to better illustrate the technical effect of the continuous process for the production of high purity chlorine gas as set forth in the present invention and are not to be construed as being equivalent to all experimental data.
Example set 1
Selection of gasification unit temperature
1. And (3) experimental operation: controlling the gasification device according to a first temperature (gasification temperature) shown in table 1, filling a compound component adsorbent of a molecular sieve and activated alumina with a mass fraction ratio of 6:4 into the adsorption device, carrying out an experiment with a first pressure of 0.6-0.8 MPa in the first rectification device and a second pressure of 0.4-0.6 MPa in the second rectification device, and obtaining result data shown in table 1. Wherein the height of the first and second rectification devices is 12 meters.
TABLE 1 different temperature selection for gasification plants
| Group of embodiments | First temperature (. degree. C.) | Average yield (Kg/h) | Yield (%) | Quality of the product |
| Example 1 | 20～30 | 80 | 90 | Qualified |
| Example 2 | 31～40 | 150 | 98 | Qualified |
| Example 3 | 41～50 | 120 | 82 | Qualified |
| Example 4 | 51～60 | 100 | 78 | Qualified |
2. And (4) analyzing results: as can be seen from table 1 above, in a certain temperature range (i.e., 20 to 40 ℃), as the first temperature (i.e., the gasification temperature) increases, the average yield of the high-purity chlorine gas is also greatly increased, and the yield of the high-purity chlorine gas is also greatly increased; over a certain temperature range (namely 31-40 ℃), the average yield of the high-purity chlorine gas is greatly reduced and the yield of the high-purity chlorine gas is also greatly reduced along with the increase of the first temperature (namely the gasification temperature). Specifically, when the first temperature (i.e. the gasification temperature) is within the range of 31-40 ℃, the average yield of the high-purity chlorine gas is the highest and reaches 150Kg/h, and at this time, the yield of the high-purity chlorine gas is the highest and reaches 98%.
Example group 2
1. Moisture removal from high purity chlorine gas under different adsorbent conditions
a. And (3) experimental operation: respectively selecting 3 different adsorbents of active alumina, a molecular sieve and a compound component of the molecular sieve and the active alumina (the mass fraction ratio of the molecular sieve to the active oxidant in the compound component is 6:4) to remove water in the high-purity chlorine, and obtaining result data shown in table 2.
TABLE 2 removal of moisture from high purity chlorine gas under different adsorbents
b. And (4) analyzing results: as can be seen from Table 2, under the condition of the same amount of the adsorbent, the compound adsorbent compounded by the molecular sieve and the activated alumina according to the mass fraction of 6:4 has the best dehydration effect, and the water content in the high-purity chlorine gas can reach 0.27ppmv and is far lower than 0.3 ppmv.
2. Selection of different compounding ratios of molecular sieve and active alumina
a. And (3) experimental operation: different compound proportions of the molecular sieve and the activated alumina, namely 1:9, 2:8, 3:7, 4:6, 5:5, 6:4, 7:3 and 8:2, are respectively selected as adsorbents to remove water in the high-purity chlorine gas, and result data shown in table 3 are obtained.
TABLE 3 removal of water from high-purity chlorine at different compounding ratios
b. And (4) analyzing results: as can be seen from table 3, under a certain compounding ratio of the molecular sieve to the activated alumina (i.e., the compounding ratio of the molecular sieve to the activated alumina is in the range of 1:9 to 6:4), as the mass percentage of the molecular sieve increases, the more water in the high-purity chlorine gas is removed, the lower the water content in the high-purity chlorine gas is; when the compounding ratio of the molecular sieve to the activated alumina exceeds a certain value (namely the compounding ratio of the molecular sieve to the activated alumina is 6:4), the removal of water in the high-purity chlorine gas is less and the water content in the high-purity chlorine gas is higher along with the increase of the mass percentage of the molecular sieve. Wherein, when the compounding ratio of the molecular sieve to the active alumina is 6:4, the water content in the high-purity chlorine is the lowest and can reach 0.27 ppmv.
3. Single stage adsorption and selection of multiple stages of adsorption
a. And (3) experimental operation: and respectively selecting the compound adsorbent of the molecular sieve and the activated alumina, the silicon tetrachloride adsorbent, the molecular sieve adsorbent and the alumina adsorbent with the same dosage to remove the water in the high-purity chlorine. Wherein, the compounding ratio of the molecular sieve to the activated alumina is 6:4, and single-stage adsorption operation is carried out; the silicon tetrachloride adsorbent, the molecular sieve adsorbent and the alumina adsorbent were subjected to two-stage adsorption operation, and the result data shown in table 4 were obtained.
TABLE 4 removal of water from high-purity chlorine at different compounding ratios
b. And (4) analyzing results: as can be seen from Table 4, the single-stage adsorption operation of the composite adsorbent consisting of the molecular sieve and the activated alumina in the composite ratio of 6:4 is far higher than the two-stage adsorption operation of a single adsorbent (such as silicon tetrachloride, the molecular sieve, alumina and the like) in removing moisture in high-purity chlorine; and the quality of the chlorine after regeneration of the compound adsorbent is far higher than that of the chlorine after regeneration of the single adsorbent. Wherein the compound adsorbent of the molecular sieve and the active alumina with the compound proportion of 6:4 can ensure that the water content in the high-purity chlorine gas reaches 0.27ppmv, and the mass of the regenerated compound adsorbent of the molecular sieve and the active alumina with the compound proportion of 6:4 can reach 30 t.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (10)
1. A continuous production process of high-purity chlorine gas is characterized by comprising the following steps:
step S1, introducing liquid chlorine from a liquid phase space valve of an industrial liquid chlorine tank into a gasification device, and gasifying at a first temperature to obtain gasified nitrogen;
step S2, introducing the nitrogen obtained in the step S1 into an adsorption device, and adsorbing by a compound adsorbent to obtain crude high-purity chlorine with the water content of less than or equal to 0.3 ppmv;
step S3, introducing the crude high-purity chlorine obtained in the step S2 into a primary rectifying device, and rectifying and removing heavy component impurities in the crude high-purity chlorine under a first pressure to obtain primary high-purity chlorine;
and step S4, introducing the primary high-purity chlorine gas obtained in the step S3 into a secondary rectification device, and rectifying and removing light component impurities in the primary high-purity chlorine gas under a second pressure to obtain secondary high-purity chlorine gas.
2. The continuous process for producing high purity chlorine gas of claim 1, wherein the first temperature is in the range of 20 ℃ to 60 ℃.
3. The continuous process for producing high purity chlorine gas of claim 1, wherein the built adsorbent is a built adsorbent of a molecular sieve and activated alumina.
4. The continuous production process of high purity chlorine gas according to claim 3, wherein the mass fraction ratio of the molecular sieve to the activated alumina is 4:6 to 7: 3.
5. The continuous process for producing high purity chlorine gas of claim 1, wherein the first pressure is in the range of 0.6 to 0.8 MPa.
6. The continuous process for producing high purity chlorine gas of claim 5, wherein the second pressure is in the range of 0.4 to 0.6 MPa.
7. The continuous process for the production of high purity chlorine according to any of claims 1 to 6, wherein the height of the first rectification unit is 10 to 14 meters; and/or the presence of a gas in the gas,
the height of the second rectifying device is 10-14 m.
8. The continuous production process of high purity chlorine gas as claimed in any one of claims 1 to 6, wherein the adsorption unit comprises a use tank and a regeneration tank connected in parallel with the gas circuit between the gasification unit and the primary rectification unit.
9. The continuous production process of high-purity chlorine gas according to any one of claims 1 to 6, wherein the first rectification device comprises a first refrigerating unit and a first heating element, and the first refrigerating unit is arranged at the top of the first rectification device; the first heating device is additionally arranged at the bottom of the first rectifying device; and/or the presence of a gas in the gas,
the second rectifying device comprises a second refrigerating unit and a second heating element, the second refrigerating unit is arranged at the top of the second rectifying device, and the second heating element is arranged at the bottom of the second rectifying device.
10. The continuous process for the production of high purity chlorine of any of claims 1 to 6, further comprising:
step S5, bottling the secondary high-purity chlorine gas obtained in the step S4 by a compression canning system to obtain bottled high-purity liquid nitrogen;
step S6, introducing heavy component impurities removed by the primary rectifying device into a tail gas treatment device, and treating with alkali liquor;
and step S7, introducing the light component impurities removed by the secondary rectification device into a tail gas treatment device, and treating with alkali liquor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010623553.8A CN111704108A (en) | 2020-06-30 | 2020-06-30 | Continuous production process of high-purity chlorine |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1054402A (en) * | 1990-01-19 | 1991-09-11 | 波克集团股份有限公司 | The cryogenic purincation of gas |
| CN103626129A (en) * | 2013-08-09 | 2014-03-12 | 杭州电化集团有限公司 | Preparation method for electronic-grade high-purity chlorine from industrial liquid chlorine |
| CN107739024A (en) * | 2017-11-14 | 2018-02-27 | 合肥创想能源环境科技有限公司 | The technique that a kind of UF membrane composite algorithm prepares nitrogen |
| CN110683513A (en) * | 2019-11-12 | 2020-01-14 | 浙江博瑞电子科技有限公司 | Preparation method of high-purity chlorine |
| CN210764317U (en) * | 2019-09-17 | 2020-06-16 | 苏州金宏气体股份有限公司 | Electronic grade hydrogen bromide purification device |
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2020
- 2020-06-30 CN CN202010623553.8A patent/CN111704108A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1054402A (en) * | 1990-01-19 | 1991-09-11 | 波克集团股份有限公司 | The cryogenic purincation of gas |
| CN103626129A (en) * | 2013-08-09 | 2014-03-12 | 杭州电化集团有限公司 | Preparation method for electronic-grade high-purity chlorine from industrial liquid chlorine |
| CN107739024A (en) * | 2017-11-14 | 2018-02-27 | 合肥创想能源环境科技有限公司 | The technique that a kind of UF membrane composite algorithm prepares nitrogen |
| CN210764317U (en) * | 2019-09-17 | 2020-06-16 | 苏州金宏气体股份有限公司 | Electronic grade hydrogen bromide purification device |
| CN110683513A (en) * | 2019-11-12 | 2020-01-14 | 浙江博瑞电子科技有限公司 | Preparation method of high-purity chlorine |
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