CN106215852B - A kind of method of fluorine-containing organic gas purifying - Google Patents
A kind of method of fluorine-containing organic gas purifying Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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Abstract
The present invention relates to a kind of methods of fluorine-containing organic gas purifying, are prepared for high-efficiency adsorbent first.It first passes through molecular sieve and is adsorbed and removed moisture, enter back into the adsorption tower equipped with this high-efficiency adsorbent of plural serial stage, temperature -100~-20 DEG C, 0.3~3MPa of pressure, flow velocity 3-10BV/h, fluorine-containing organic gas after absorption obtains high-purity fluorine-containing organic gas product using removing impurities matter purification techniques known in the industry.
Description
Technical field
The present invention relates to a kind of method of purification, especially a kind of method of fluorine-containing organic gas purifying.
Background technique
Semiconducter IC processing procedure mainly based on four ion implanting, diffusion, epitaxial growth and photoetching fundamental technologies gradually
Grow up.Since element each in integrated circuit and line are quite fine, in manufacturing process, if by grit, metal
Pollution, it is easy to cause the damage of circuit function in chip, form short circuit or open circuit etc., cause integrated circuit failure and
Influence the formation of geometrical characteristic.Therefore in the production process other than outside contamination source to be excluded, production of integrated circuits step is such as
It is required to carry out cleaning before High temperature diffusion, ion implanting etc..
Fluorine-containing cleaning agent shows extraordinary performance in semiconductor and electronics industry cleaning especially dry method cleaning.
Fluorine-containing cleaning agent boiling point is lower, exists under room temperature with gas phase, therefore is very easy to carry out dry vapor cleaning.Fluorine-containing cleaning agent master
It to include CF4、C2F6、C3F8、c-C4F8、SF6、NF3、CF2O、F2Deng the fluorine-containing purge gas of tradition mainly includes carbon tetrafluoride
(CF4), perfluoroethane (C2F6), octafluoropropane (C3F8), octafluorocyclobutane (c-C4F8), sulfur hexafluoride (SF6), Nitrogen trifluoride
(NF3) etc. kinds, semiconductor cleaning in, mainly with C in situ2F6With CF4Based on equal perfluors nitrogen compound (PFC) cleaning.
CN1455699 discloses a kind of method for producing adsorbent；High-purity octafluoropropane or octafluorocyclobutane；Purifying and life
The method for producing the octafluoropropane or octafluorocyclobutane；With its purposes.Method of the purifying by including the following steps produces pure
Change adsorbent to carry out: (1) by former charcoal acid elution, being then washed with water；(2) by former charcoal deoxidation and/or dehydration；(3) former charcoal exists
It is carbonized again at 500-700 DEG C of temperature；(4) former charcoal steams at 700-900 DEG C of temperature comprising inert gas, carbon dioxide and water
It is activated in the mixed gas stream of vapour.
CN103664502 discloses a kind of octafluoropropane purification process, comprising: under normal temperature conditions by octafluoropropane raw material
Carry out room temperature absorption；By the octafluoropropane raw material by room temperature absorption at -37 DEG C~10 DEG C, under the conditions of 0.1~0.6MPa
Carry out rectifying；The octafluoropropane raw material Jing Guo rectifying is subjected to cryogenic absorption at a temperature of -100 DEG C~-30 DEG C；It will pass through
The octafluoropropane raw material of cryogenic absorption carries out pressurized adsorbent under the pressure condition of 0.5~1.5MPa, obtains octafluoropropane
Product.Using the present invention, most of containing chlorine fluorine carbon compound impurity in octafluoropropane raw material is not only removed, but also solve existing
Carbon dioxide and water remove the inadequate problem of depth in technology, reduce energy consumption, enhance the adsorption effect of adsorbent, make octafluoropropane
Product reaches purity 99.999% or more.
For adsorbent in the prior art using high-temperature process or steam activation is preceding needed, energy consumption is higher, needs further
Optimization technique.
Summary of the invention
It is pure to provide a kind of fluorine-containing organic gas for above-mentioned technical problem present in present invention aims to solve the prior art
The method of change.It is characterized in that preparation step includes:
(1) preparation of high-efficiency adsorbent
By weight: by flyash and by iron chloride FeCl3·6H2O, 1- ethyl diethyldithiocarbamate ether -3- methylimidazole is double
The pillared liquid each component that (fluoroform sulphonyl) inferior amine salt, deionized water form is by 100: 2-10: 0.05-0.5: 500-1000
Ratio mixing carries out intercalation modifying, in 80-100 DEG C of stirring 30-80h；Add the tallow of flyash quality degree 1-5
Base double hydroxyethyl amine oxide, the choline chloride of flyash quality degree 0.5-2, flyash quality degree 1-5
Urea, in 50-80 DEG C of stirring 10-30h, then be centrifuged, wash, be granulated, drying etc. processes can obtain high-efficiency adsorbent product；
(2) fluorine-containing organic gas purifying
Fluorine-containing organic gas crude product first passes through molecular sieve and is adsorbed and removed moisture, enters back into efficiently inhaling equipped with this for plural serial stage
Attached dose of adsorption tower, temperature -100~-20 DEG C, 0.3~3MPa of pressure, flow velocity 3-10BV/h, the fluorine-containing organic gas after absorption
Using removing impurities matter purification techniques known in the industry, including rectification under vacuum, low-boiling gas is sloughed, obtains high-purity fluorine-containing having
Machine gas products.
Bis- (fluoroform sulphonyl) inferior amine salts of 1- ethyl diethyldithiocarbamate ether -3- methylimidazole in step 1 are commercial product, as in
The product of the Lanzhou Ke Yuan Chemical Physics Research Institute；Polyethylene glycol oxide tallow amine is commercial product, as Shandong sends Buddhist nun's chemistry to have
The product of limit company production.
The fluorine-containing organic gas includes octafluoropropane C3F8, octafluorocyclobutane C4F8, fluoromethane R41, difluoromethane
R32, fluoroform R23, perfluoroethane R116.
The molecular sieve desiccant be known molecular sieve, it is preferable to use the example of molecular sieve include X-type molecular sieve,
A type molecular sieve, molecular sieve can be handled using preceding by pretreatment, such as acid, heat treatment and steam treatment.
The flyash be coal dust formed after high-temp combustion one kind like pozzolana mixed material.It is burning coal
Power plant coal is worn into 100 microns of coal dusts below, spray into burner hearth with preheated air and burn at suspended state, generation is contaminated with
The high-temperature flue gas of a large amount of incombustible has just obtained flyash through dust collect plant trapping.The chemical composition of flyash and clayey phase
Seemingly, main component is silica, aluminum oxide, di-iron trioxide, calcium oxide and uncompleted burned carbon.With high specific surface
Product, general specific surface area (cm2/ g) 800~19500.
The plural serial stage can be connected in series for 2-5 grades of adsorption towers.
The present invention is by adopting the above-described technical solution, have the advantages that
(1) pass through iron chloride FeCl3·6H2Bis- (fluoroform sulphonyl) inferior amine salts of O, 1- ethyl diethyldithiocarbamate ether -3- methylimidazole
The flyash of intercalation modifying synthesis, the ability of adsorbed gas are enhanced.
(2) choline chloride is loaded, the ability of absorption carbon dioxide can be improved in the adsorbent of urea.
(3) flyash is cheap, and the preparation of high-efficiency adsorbent does not need high-temperature process, reduces energy consumption.
Specific embodiment
Following instance is only to further illustrate the present invention, is not limitation the scope of protection of the invention.
Embodiment 1
(1) preparation of high-efficiency adsorbent
100Kg flyash, 5Kg iron chloride FeCl are added in 2000L reactor3·6H2O, 0.2Kg1- ethyl diethyldithiocarbamate ether-
Bis- (fluoroform sulphonyl) inferior amine salts of 3- methylimidazole, the mixing of 800Kg deionized water carry out intercalation modifying, in 90 DEG C of stirring 60h；
The urea for adding the tallow base double hydroxyethyl amine oxide of 3Kg, the choline chloride of 1Kg, 3Kg, in 70 DEG C of stirring 20h, then through from
The heart washs, and is granulated, and the processes such as drying obtain high-efficiency adsorbent product；
(2) fluorine-containing organic gas purifying
Octafluoropropane C3F8Crude product first passes through 5A molecular sieve and is adsorbed and removed moisture, enters back into 3 grades of concatenated are equipped with and originally efficiently inhales
Attached dose of adsorption tower, -80 DEG C of temperature, pressure 0.8MPa, flow velocity 5BV/h, the octafluoropropane C after absorption3F8Gas is using in the industry
Well known removing impurities matter purification techniques, including rectification under vacuum, slough low-boiling gas, obtain high-purity octafluoropropane C3F8Product.
Product number B-1.
Embodiment 2
(1) preparation of high-efficiency adsorbent
100Kg flyash, 2Kg iron chloride FeCl are added in 2000L reactor3·6H2O, 0.05Kg1- ethyl diethyldithiocarbamate
Bis- (fluoroform sulphonyl) inferior amine salts of ether -3- methylimidazole, the mixing of 500Kg deionized water carry out intercalation modifying, stir at 80 DEG C
30h；The urea for adding the tallow base double hydroxyethyl amine oxide of 1Kg, the choline chloride of 0.5Kg, 1Kg, in 50 DEG C of stirring 10h,
It is centrifuged, is washed again, is granulated, the processes such as drying obtain high-efficiency adsorbent product；
(2) fluorine-containing organic gas purifying
Octafluorocyclobutane C4F8Crude product first passes through 4A molecular sieve and is adsorbed and removed moisture, enter back into 2 grades it is concatenated equipped with this efficiently
The adsorption tower of adsorbent, -100 DEG C of temperature, pressure 0.3MPa, flow velocity 3BV/h, the octafluorocyclobutane C after absorption4F8Gas passes through again
Removing impurities matter purification techniques known in the industry, including rectification under vacuum are crossed, low-boiling gas is sloughed, obtains high-purity octafluorocyclobutane
C4F8Product.Product number B-2.
Embodiment 3
(1) preparation of high-efficiency adsorbent
100Kg flyash, 10Kg iron chloride FeCl are added in 2000L reactor3·6H2O, 0.5Kg1- ethyl diethyldithiocarbamate
Bis- (fluoroform sulphonyl) inferior amine salts of ether -3- methylimidazole, the mixing of 1000Kg deionized water carry out intercalation modifying, stir at 100 DEG C
Mix 80h；The urea for adding the tallow base double hydroxyethyl amine oxide of 5Kg, the choline chloride of 2Kg, 5Kg, in 80 DEG C of stirring 30h,
It is centrifuged, is washed again, is granulated, the processes such as drying obtain high-efficiency adsorbent product；
(2) fluorine-containing organic gas purifying
Fluoromethane R41 crude product first passes through 3A molecular sieve and is adsorbed and removed moisture, enter back into 5 grades it is concatenated equipped with this efficient absorption
The adsorption tower of agent, -20 DEG C of temperature, pressure 3MPa, flow velocity 10BV/h, the fluoromethane R41 gas after absorption is using known in the industry
Removing impurities matter purification techniques, including rectification under vacuum sloughs low-boiling gas, obtains high-purity fluoromethane R41 product.Product is compiled
Number B-3.
Embodiment 4
(1) preparation of high-efficiency adsorbent
100Kg flyash, 4Kg iron chloride FeCl are added in 2000L reactor3·6H2O, 0.7Kg1- ethyl diethyldithiocarbamate ether-
Bis- (fluoroform sulphonyl) inferior amine salts of 3- methylimidazole, the mixing of 700Kg deionized water carry out intercalation modifying, in 90 DEG C of stirring 60h；
The urea for adding the tallow base double hydroxyethyl amine oxide of 2Kg, the choline chloride of 1Kg, 2Kg, in 70 DEG C of stirring 20h, then through from
The heart washs, and is granulated, and the processes such as drying obtain high-efficiency adsorbent product；
(2) fluorine-containing organic gas purifying
Difluoromethane R32 crude product first passes through 10X molecular sieve and is adsorbed and removed moisture, enter back into 3 grades it is concatenated equipped with this efficiently
The adsorption tower of adsorbent, -83 DEG C of temperature, pressure 0.9MPa, flow velocity 5BV/h, the difluoromethane R32 gas after absorption is using industry
Interior well known removing impurities matter purification techniques, including rectification under vacuum, slough low-boiling gas, obtain high-purity difluoromethane R32 and produce
Product.Product number B-4.
Embodiment 5
(1) preparation of high-efficiency adsorbent
100Kg flyash, 3Kg iron chloride FeCl are added in 2000L reactor3·6H2O, 1.3Kgl- ethyl diethyldithiocarbamate ether-
Bis- (fluoroform sulphonyl) inferior amine salts of 3- methylimidazole, the mixing of 1000Kg deionized water carry out intercalation modifying, stir at 80 DEG C
50h；The urea for adding the tallow base double hydroxyethyl amine oxide of 1.6Kg, the choline chloride of 2Kg, 2Kg, in 78 DEG C of stirring 21h,
It is centrifuged, is washed again, is granulated, the processes such as drying obtain high-efficiency adsorbent product；
(2) fluorine-containing organic gas purifying
Fluoroform R23 crude product first passes through 5A molecular sieve and is adsorbed and removed moisture, enters back into 3 grades of concatenated are equipped with and originally efficiently inhales
Attached dose of adsorption tower, -70 DEG C of temperature, pressure 1MPa, flow velocity 2BV/h, the fluoroform R23 gas after absorption is using public in the industry
The removing impurities matter purification techniques known, including rectification under vacuum, slough low-boiling gas, obtain high-purity fluoroform R23 product.It produces
Product number B-5.
Embodiment 6
(1) preparation of high-efficiency adsorbent
100Kg flyash, 8Kg iron chloride FeCl are added in 2000L reactor3·6H2O, 0.5Kg1- ethyl diethyldithiocarbamate ether-
Bis- (fluoroform sulphonyl) inferior amine salts of 3- methylimidazole, the mixing of 600Kg deionized water carry out intercalation modifying, in 90 DEG C of stirring 40h；
The urea for adding the tallow base double hydroxyethyl amine oxide of 3Kg, the choline chloride of 2Kg, 3Kg, in 80 DEG C of stirring 13h, then through from
The heart washs, and is granulated, and the processes such as drying obtain high-efficiency adsorbent product；
(2) fluorine-containing organic gas purifying
Perfluoroethane R116 crude product first passes through 10X molecular sieve and is adsorbed and removed moisture, enter back into 3 grades it is concatenated equipped with this efficiently
The adsorption tower of adsorbent, -90 DEG C of temperature, pressure 2.8MPa, flow velocity 4BV/h, perfluoroethane R116 gas after absorption using
Removing impurities matter purification techniques known in the industry, including rectification under vacuum, slough low-boiling gas, obtain high-purity perfluoroethane R116
Product.Product number B-6.
Comparative example 1
Iron chloride FeCl3·6H2O is added without, the other the same as in Example 1, product number B-7.
Comparative example 2
Bis- (fluoroform sulphonyl) inferior amine salts of 1- ethyl diethyldithiocarbamate ether -3- methylimidazole are added without, the other the same as in Example 1, are produced
Product number B-8.
Comparative example 3
Choline chloride is added without, the other the same as in Example 1, product number B-9.
Comparative example 4: removing step 1, and step 2 is adsorbed using X-type molecular sieve, the other the same as in Example 1, product number B-10.
Embodiment 4
The product purity of embodiment 1-6 and comparative example 1-4 and the volumetric concentration of carbon dioxide are detected, see the table below:
The above is only specific embodiments of the present invention, but technical characteristic of the invention is not limited thereto.It is any with this hair
Based on bright, to solve essentially identical technical problem, essentially identical technical effect is realized, made simple change, etc.
With replacement or modification etc., all it is covered by among protection scope of the present invention.
Claims (6)
1. a kind of method of fluorine-containing organic gas purifying, it is characterised in that
Preparation step includes: the preparation of (1) adsorbent
By weight: by flyash and by iron chloride FeCl3·6H2O, the bis- (trifluoros of 1- ethyl diethyldithiocarbamate ether -3- methylimidazole
Sulfonyl methane) inferior amine salt, deionized water composition pillared liquid each component in 100: 2-10: 0.05-0.5: 500-1000 ratio
Mixing carries out intercalation modifying, in 80-100 DEG C of stirring 30-80h；Add the tallow base of flyash quality degree 1-5%
Double hydroxyethyl amine oxide, the choline chloride of flyash quality degree 0.5-2%, flyash quality degree 1-5%
Urea, in 50-80 DEG C of stirring 10-30h, then be centrifuged, washed, is granulated, baking process can obtain adsorbent product；
(2) fluorine-containing organic gas purifying
Fluorine-containing organic gas crude product first passes through molecular sieve and is adsorbed and removed moisture, enters back into the suction equipped with this adsorbent of plural serial stage
Attached tower, temperature -100~-20 DEG C, 0.3~3MPa of pressure, flow velocity 3-10BV/h, the fluorine-containing organic gas after absorption is using de-
Impurity purification techniques sloughs low-boiling gas, obtains high-purity fluorine-containing organic gas product.
2. a kind of method of fluorine-containing organic gas purifying according to claim 1, it is characterised in that
Flyash described in step (1) be coal dust formed after high-temp combustion one kind like pozzolana mixed material；It is
Coal is worn into 100 microns of coal dusts below by the power plant of burning coal, is sprayed into burner hearth with preheated air and is burnt at suspended state, generates
It is contaminated with the high-temperature flue gas of a large amount of incombustible, has just obtained flyash through dust collect plant trapping；Ingredient is silica, three oxidations
Two aluminium, di-iron trioxide, calcium oxide and uncompleted burned carbon have high specific surface area, 800~19500cm of specific surface area2/g。
3. a kind of method of fluorine-containing organic gas purifying according to claim 1, it is characterised in that
Fluorine-containing organic gas described in step (2) includes octafluoropropane C3F8, octafluorocyclobutane C4F8, fluoromethane R41, difluoro first
Alkane R32, fluoroform R23, perfluoroethane R116.
4. a kind of method of fluorine-containing organic gas purifying according to claim 1, it is characterised in that
Molecular sieve desiccant described in step (2) is known molecular sieve, and the molecular sieve used includes X-type molecular sieve, A type point
Sub- sieve, molecular sieve, by pretreatment, can be selected from acid processing, heat treatment and steam treatment using preceding.
5. a kind of method of fluorine-containing organic gas purifying according to claim 1, it is characterised in that
Plural serial stage described in step (2) is connected in series for 2-5 grades of adsorption towers.
6. a kind of method of fluorine-containing organic gas purifying according to claim 1, it is characterised in that
Removing impurities matter purification techniques described in step (2) is rectifying isolation technics, including multistage rectification or single-stage rectifying.
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| CN109251124B (en) * | 2018-11-01 | 2022-01-18 | 广东华特气体股份有限公司 | Purification process of monofluoromethane |
| CN110526834B (en) * | 2019-09-20 | 2022-05-20 | 泉州宇极新材料科技有限公司 | Method for preparing high-purity perfluoroisobutyronitrile |
| CN111170888A (en) * | 2020-01-02 | 2020-05-19 | 黎明化工研究设计院有限责任公司 | Method for purifying heptafluoroisobutyronitrile |
| CN112694387A (en) * | 2020-12-30 | 2021-04-23 | 广东华特气体股份有限公司 | Difluoromethane purification method |
| CN113877313B (en) * | 2021-10-25 | 2022-06-17 | 上海杰视医疗科技有限公司 | Purification device and purification method for medical perfluoropropane |
| CN115043702B (en) * | 2022-07-26 | 2023-12-22 | 浙江人行道化工有限公司 | Octafluorocyclobutane and purification method thereof |
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