CN107176902A - A kind of CF3I process for separating and purifying - Google Patents
A kind of CF3I process for separating and purifying Download PDFInfo
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- CN107176902A CN107176902A CN201710631402.5A CN201710631402A CN107176902A CN 107176902 A CN107176902 A CN 107176902A CN 201710631402 A CN201710631402 A CN 201710631402A CN 107176902 A CN107176902 A CN 107176902A
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- tower
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- cf3i
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/093—Preparation of halogenated hydrocarbons by replacement by halogens
- C07C17/15—Preparation of halogenated hydrocarbons by replacement by halogens with oxygen as auxiliary reagent, e.g. oxychlorination
- C07C17/158—Preparation of halogenated hydrocarbons by replacement by halogens with oxygen as auxiliary reagent, e.g. oxychlorination of halogenated hydrocarbons
Abstract
The invention discloses a kind of CF3I process for separating and purifying, the technique is the method that the product mixed gas separation purification that prepared by fluoroform gas phase into CF3I obtains CF3I monomer.By the component in substep separation gaseous mixture, separating-purifying CF3I is reached.The system has the rate of recovery high, good separating effect, the low feature of cost.The present invention has the features such as rate of recovery is high, product purity is high, separation is thorough during separating-purifying CF3I；Technological process is simple, and safety coefficient is high, it is easy to operate, separating-purifying is with low cost.Value with industrialized production.
Description
Technical field
The invention belongs to the separating-purifying of the high saturated vapor pressure gas of gas phase organic synthesis field and collection, more particularly, to
A kind of main component is fluoroform and the separating-purifying and recovery process of CF3I mixed gas.
Background technology
CF3I (CF3I), boiling point is -22.5 DEG C, and critical pressure is 3.95MPa, and normal atmosphere pressure is colourless nothing
Taste gas.CF3The spy such as I has that fire-fighting efficiency is high as extinguishing chemical, had a safety feature, economic utility is high, leave no trace after fire extinguishing
Point, is BTM (breathing out dragon 1301) preferably substitute species；It is used as refrigerant, CF3I is non-ignitable, with oil-soluble and material
The characteristics of compatibility is fine, it is considered to be one of ideal substitute of traditional freon refrigerant constituent element.In addition, CF3I is fluorine-containing
The other fields such as intermediate, conductor etching, foaming agent are also with a wide range of applications.
At present, CF3I process for separation and purification is also rarely reported, especially with CF3H synthesizes for raw material gas-phase catalysis
CF3I, its reaction equation is as follows：
(CN101219925), the separating-purifying of mixed gas is not yet reported that.Contain a certain amount of on-condensible gas in mixed gas,
And the larger raw material CF of saturated vapour pressure3H, the operating pressure of whole system is larger, CF3I and C4F8Vapor of mixture can be formed
Thing.Azeotropic mixture usually requires to carry out separating-purifying to mixture using extraction and distillation technology.The usual implication of extracting rectifying
Refer to that lower than component relative volatility to be separated (or boiling point is than component to be separated extremely being continuously added to close at the top of rectifying column
It is few high 50 DEG C) material (solvent), the relative volatility of component to be separated in tower can be changed by so making.Therefore a kind of knot is provided
The mono- ﹑ Jie energy Huan Bao ﹑ Yun row Ping Wen ﹑ An of the mono- ﹑ Cao Fang of the work Bian ﹑ Gong skills Jian of structure Jian are complete, and Ke Kao ﹑ product purities Gao ﹑ equipment Shao ﹑ investments are low
CF3I mixed gas purifying plant and method of purification, it appears particularly important and with wide market prospects.
The content of the invention
The technical problem to be solved in the present invention is, fills up existing separating-purifying CF3I blank, purification needed for overcoming is mixed
Close and there is on-condensible gas in gas, gas saturated vapor pressure is big, and there is the technical barriers such as azeotropic combination, there is provided a kind of structural manufacturing process
It is simple efficient, the CF that process is easily controlled3I gaseous mixtures purifying plant and method of purification.
The process for separating and purifying principle and advantage of the present invention：
Extractant of the present invention, separating degree both when making extracting rectifying>CF in 1.5, and tower top3I monomers are pure
Degree is more than 99.9%, and the residual quantity of extractant is less than 50ppm.
The method of separating-purifying CF3I in CF3I crude product mixed gas, the mixed gas is with CF3H
CF is synthesized for raw material gas-phase catalysis3I product mixtures, wherein containing fluoroform raw material, CF3I, five fluorine iodine second
Alkane, octafluoro butylene, pentafluoroethane, carbon dioxide and oxygen, its reaction equation is as follows：
The process for separation and purification comprises the following steps：
(1) mixed gas removes on-condensible gas by degassing tower 1, then removes CF by degassing tower 23H and C2F5H。
(2) extractive distillation column rectifying is entered after deaerating, extractant is ketones solvent or acetate solvent, CF3I monomers
From recovered overhead, tower reactor is rich in octafluoro -2- butylene and C2F5I extractant.
The ketones solvent is acetone, MEK or butanone；The acetic acid esters is methyl acetate, ethyl acetate or second
Propyl propionate.
Filler in the extraction tower is preferably metal Intelux filling, metal Pall ring granular filler or metal
Liquid-gas ratio is preferably 20~0.1 in structured packing, extraction tower:1 (volume ratio of gas of the extractant with entering extractive distillation column)
The spray temperature of the liquid of the extractive distillation column is preferably -30~50 DEG C；The operating pressure of extractive distillation column is excellent
Elect 0.1~2.0MPa as；The tower top temperature of the extractive distillation column is preferably -40~20 DEG C, and bottom temperature is preferably 20~100
℃。
The spray of the liquid of the extractive distillation column more preferably temperature is -10~20 DEG C；The operating pressure of extractive distillation column
More preferably 0.1~1.0MPa；The tower top temperature of the extractive distillation column is more preferably -40~-10 DEG C, and bottom temperature is more preferably
For 20~70 DEG C.
The filler of the degassing tower 1 and degassing tower 2 is ceramic ring, glass spring, woven wire or Raschig ring, and tower top is followed
Preferably -20~-50 DEG C of ring coolant temperature, preferably 20~100 DEG C of bottom temperature, degassing tower operating pressure preferably 0.1~
2.0MPa。
The temperature of the tower top circulating cooling liquid of the degassing tower 1 is more preferably -40~-20 DEG C, and bottom temperature is more preferably
20~65 DEG C, the pressure of degassing tower is more preferably 0.1~1.0MPa；The temperature of the tower top circulating cooling liquid of degassing tower 2 is more preferably
For -50~-30 DEG C, bottom temperature is more preferably 50~70 DEG C, and the pressure of degassing tower is more preferably 0.3~0.8MPa.
It is described to be rich in octafluoro -2- butylene and C2F5I extractant is desorbed into desorber, and the extraction of desorber tower reactor is molten
Agent is recycled after cooling, parses the octafluoro -2- butylene and C of column overhead2F5I is separately recovered in corresponding collecting tank.
The process conditions of the desorber are preferably 0.1~2.0MPa for the operating pressure of desorber；The extracting rectifying
The tower top temperature of tower is preferably -10~10 DEG C, and bottom temperature is preferably 50~80 DEG C.
In extracting rectifying, the solvent of selection should have boiling point higher, the property such as physicochemical properties stabilization, and can not
With non-solvent component formation azeotropic mixture.For extracting rectifying, following principle should be followed when selection solvent：
1) solvent selected in extracting rectifying should have selectivity as big as possible, that is, can effectively make stock blend after adding
Relative volatility change to segregative direction；
2) solvent selected in extracting rectifying has preferable dissolubility, can be sufficiently mixed with component to be separated, so as to protect
The sufficiently small solvent ratio of card and rectifiying plate efficiency；
3) solvent selected in extracting rectifying can not chemically react with component to be separated；
4) solvent selected in extracting rectifying should have stronger heat endurance and chemical stability；
5) solvent selected in extracting rectifying should have relatively low specific heat and evaporation latent heat, so as to reduce in extracting rectifying
Energy consumption；
6) solvent selected in extracting rectifying should have less molal volume, so as to reduce tower reactor volume and tower body holds liquid
Amount；
7) solvent viscosity selected in extracting rectifying should not be too big, is so easy to the conveying of material, reaches good mass transfer
And heat transfer efficiency；
8) solvent selected in extracting rectifying should as nontoxic as possible, non-corrosiveness, beneficial to environmental protection, and price economy is easy
Arrive.
Ketones solvent and acetate solvent of the present invention can not only obtain the CF of high-purity as extractant3I
Monomer, and extractant can be controlled in CF3Residual quantity in I monomers is in reduced levels.Other accessory substances and solvent are through solution
Tower physical desorption is inhaled, changes the temperature of system in desorber, by accessory substance and extractant gas-liquid separation, extractant, which can be circulated, to be made
With.
Advantage of the present invention：
The method of the invention operating flexibility is big, and technique quick-reading flow sheets is short, and extractant is cheap and easily obtains, behaviour
Make cost low, small investment, therefore this method is suitable for industrialized production.And the extractant of the present invention can obtain high-purity
CF3I monomers, and residual quantity is very low.
Brief description of the drawings
Fig. 1 is CF3I (CF3I) the flow chart of purification.
Embodiment
The present invention will be further described with reference to the accompanying drawings and examples, the scheme of embodiment described here, does not limit
The present invention, one of skill in the art can make improvements and change according to the spirit of the present invention, these described improvement
It is regarded as within the scope of the invention with change, the scope of the present invention and essence are defined by the claims.
Embodiment 1
By CF3I crude products are passed through degassing tower 1 (filler is woven wire) fore-running and remove on-condensible gas, and the tower top of degassing tower 1 is followed
The temperature of ring coolant is -20 DEG C, and bottom temperature is 30 DEG C, and the pressure of degassing tower is 0.1MPa；It will remove after on-condensible gas
CF3I crude products are passed through degassing tower 2 and remove CF3H and C2F5The gases such as H, the tower top circulation of degassing tower 2 (filler is woven wire) is cold
But the temperature of liquid is -45 DEG C, and bottom temperature is 60 DEG C, and the pressure of degassing tower is 0.5MPa.CF after deaerating twice3I
Crude product is passed through extractive distillation column, and extractant is acetone, and extracting rectifying is carried out according to the technological parameter of table 1, and purity is 99.96%
CF3I monomers are rich in octafluoro -2- butylene and a small amount of C from recovered overhead, tower reactor2F5I extractant is desorbed into desorber, desorption
The acetone of tower tower reactor is recycled after cooling, parses the octafluoro -2- butylene and a small amount of C of column overhead2F5I is separately recovered in relative
In the collecting tank answered.
Table 1
Embodiment 2
By CF3I crude products are passed through degassing tower 1 (filler is Raschig ring) fore-running and remove on-condensible gas, the tower top circulation of degassing tower 1
The temperature of coolant is -30 DEG C, and bottom temperature is 40 DEG C, and the pressure of degassing tower is 0.3MPa；It will remove after on-condensible gas
CF3I crude products are passed through degassing tower 2 and remove CF3H and C2F5The gases such as H, the tower top circulating cooling liquid of degassing tower 2 (filler is Raschig ring)
Temperature be -40 DEG C, bottom temperature is 70 DEG C, and the pressure of degassing tower is 0.7MPa.CF after deaerating twice3I crude products
Extractive distillation column is passed through, extractant is methyl acetate, extracting rectifying is carried out according to the technological parameter of table 2, purity is 99.99%
CF3I monomers are rich in octafluoro -2- butylene and a small amount of C from recovered overhead, tower reactor2F5I extractant is desorbed into desorber, desorption
The methyl acetate of tower tower reactor is recycled after cooling, parses the octafluoro -2- butylene and a small amount of C of column overhead2F5I be separately recovered in
In corresponding collecting tank.
Table 2
Embodiment 3
By CF3I crude products are passed through degassing tower 1 (filler is glass spring) fore-running and remove on-condensible gas, and the tower top of degassing tower 1 is followed
The temperature of ring coolant is -40 DEG C, and bottom temperature is 65 DEG C, and the pressure of degassing tower is 0.8MPa；It will remove after on-condensible gas
CF3I crude products are passed through degassing tower 2 and remove CF3H and C2F5The gases such as H, the tower top circulation of degassing tower 2 (filler is glass spring) is cold
But the temperature of liquid is -35 DEG C, and bottom temperature is 55 DEG C, and the pressure of degassing tower is 0.5MPa.CF after deaerating twice3I
Crude product is passed through extractive distillation column, and extractant is MEK, carries out extracting rectifying according to the technological parameter of table 3, purity is 99.95%
CF3I monomers are rich in octafluoro -2- butylene and a small amount of C from recovered overhead, tower reactor2F5I extractant is desorbed into desorber, solution
The MEK for inhaling tower tower reactor is recycled after cooling, parses the octafluoro -2- butylene and a small amount of C of column overhead2F5I be separately recovered in
In corresponding collecting tank.
Table 3
Embodiment 4
By CF3I crude products are passed through degassing tower 1 (filler is ceramic ring) fore-running and remove on-condensible gas, and the tower top circulation of degassing tower 1 is cold
But the temperature of liquid is -35 DEG C, and bottom temperature is 50 DEG C, and the pressure of degassing tower is 0.9MPa；It will remove after on-condensible gas
CF3I crude products are passed through degassing tower 2 and remove CF3H and C2F5The gases such as H, the tower top circulating cooling liquid of degassing tower 2 (filler is ceramic ring)
Temperature is -45 DEG C, and bottom temperature is 65 DEG C, and the pressure of degassing tower is 0.4MPa.CF after deaerating twice3I crude products lead to
Enter extractive distillation column, extractant is propyl acetate, extracting rectifying is carried out according to the technological parameter of table 4, purity is 99.96%
CF3I monomers are rich in octafluoro -2- butylene and a small amount of C from recovered overhead, tower reactor2F5I extractant is desorbed into desorber, desorption
The propyl acetate of tower tower reactor is recycled after cooling, parses the octafluoro -2- butylene and a small amount of C of column overhead2F5I be separately recovered in
In corresponding collecting tank.
Table 4
Claims (9)
1. the method for separating-purifying CF3I from CF3I crude product mixed gas, the mixed gas is with CF3H
CF is synthesized for raw material gas-phase catalysis3I product mixtures, wherein containing fluoroform raw material, CF3I, five fluorine iodine second
Alkane, octafluoro butylene, pentafluoroethane, carbon dioxide and oxygen, its reaction equation is as follows：
The process for separation and purification comprises the following steps：
(1) mixed gas removes on-condensible gas by degassing tower 1, then removes CF by degassing tower 23H and C2F5H,
(2) extractive distillation column rectifying is entered after deaerating, extractant is ketones solvent or acetate solvent, CF3I monomers are from tower
Top is reclaimed, and tower reactor is rich in octafluoro -2- butylene and C2F5I extractant.
2. according to the method described in claim 1, the ketones solvent is acetone, MEK or butanone；The acetic acid esters is
Methyl acetate, ethyl acetate or propyl acetate.
3. the filler in method according to claim 2, the extraction tower is preferably metal Intelux filling, metal
Liquid-gas ratio is 20~0.1 in Pall ring granular filler or metal structured packing, extraction tower:1.
4. method according to claim 3, the spray temperature of the liquid of the extractive distillation column is -30~50 DEG C；Extraction
The operating pressure of rectifying column is 0.1~2.0MPa；The tower top temperature of the extractive distillation column is -40~20 DEG C, and bottom temperature is excellent
Elect 20~100 DEG C as.
5. method according to claim 4, the spray temperature of the liquid of the extractive distillation column is -10~20 DEG C；Extraction
The operating pressure of rectifying column is 0.1~1.0MPa；The tower top temperature of the extractive distillation column is -40~-10 DEG C, and bottom temperature is
20~70 DEG C.
6. according to the method described in claim 1, the filler of the degassing tower 1 and degassing tower 2 is ceramic ring, glass spring, metal
Silk screen or Raschig ring, preferably -20~-50 DEG C of the circulating cooling liquid temperature of tower top, preferably 20~100 DEG C of bottom temperature, degassing
Tower operating pressure preferably 0.1~2.0MPa.
7. method according to claim 6, the temperature of the tower top circulating cooling liquid of the degassing tower 1 is -40~-20 DEG C,
Bottom temperature is 20~65 DEG C, and the pressure of degassing tower is 0.1~1.0MPa；The temperature of the tower top circulating cooling liquid of degassing tower 2 for-
50~-30 DEG C DEG C, bottom temperature is 50~70 DEG C, and the pressure of degassing tower is 0.3~0.8MPa.
8. according to the method described in claim 1, described be rich in octafluoro -2- butylene and C2F5I extractant enters desorber solution
Inhale, the extractant of desorber tower reactor is recycled after cooling, parse the octafluoro -2- butylene and C of column overhead2F5I is separately recovered
In corresponding collecting tank.
9. method according to claim 8, the process conditions of the desorber be desorber operating pressure be 0.1~
2.0MPa；The tower top temperature of the extractive distillation column is -10~10 DEG C, and bottom temperature is 50~80 DEG C.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108675914A (en) * | 2018-06-19 | 2018-10-19 | 宇极（廊坊）新材料有限公司 | A method of preparing high-purity trifluoroiodomethane |
| US20200172457A1 (en) * | 2018-12-03 | 2020-06-04 | Honeywell International Inc. | Processes for producing high-purity trifluoroiodomethane |
| CN112739673A (en) * | 2018-08-24 | 2021-04-30 | 霍尼韦尔国际公司 | Process for producing trifluoroiodomethane and trifluoroacetyl iodide |
| CN112888756A (en) * | 2018-10-15 | 2021-06-01 | 霍尼韦尔国际公司 | Azeotrope or azeotrope-like composition of trifluoroiodomethane (CF3I) and Hexafluoropropylene (HFP) |
| CN113214794A (en) * | 2021-04-26 | 2021-08-06 | 泉州宇极新材料科技有限公司 | Near-azeotropic mixture of trifluoroiodomethane and octafluorobutene, preparation method and application thereof |
| FR3107280A1 (en) * | 2020-02-19 | 2021-08-20 | Arkema France | Composition comprising an iodofluorocarbon compound |
| CN113423681A (en) * | 2019-02-18 | 2021-09-21 | 霍尼韦尔国际公司 | One-step process for making trifluoroiodomethane from trifluoroacetyl halide, hydrogen and iodine |
| WO2022082181A1 (en) * | 2020-10-14 | 2022-04-21 | Honeywell International Inc. | Trifluoroacetyl iodide compositions useful for making trifluoroiodomethane |
| WO2022104370A1 (en) * | 2020-11-13 | 2022-05-19 | Honeywell International Inc. | Methods for separation of azeotrope or azeotrope-like compositions of trifluoroiodomethane (cf3i) and trifluoroacetyl chloride (cf3coci) |
| CN115181004A (en) * | 2022-09-09 | 2022-10-14 | 天津绿菱气体有限公司 | Preparation method of trifluoroiodomethane |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108675914A (en) * | 2018-06-19 | 2018-10-19 | 宇极（廊坊）新材料有限公司 | A method of preparing high-purity trifluoroiodomethane |
| CN112739673A (en) * | 2018-08-24 | 2021-04-30 | 霍尼韦尔国际公司 | Process for producing trifluoroiodomethane and trifluoroacetyl iodide |
| CN112888756A (en) * | 2018-10-15 | 2021-06-01 | 霍尼韦尔国际公司 | Azeotrope or azeotrope-like composition of trifluoroiodomethane (CF3I) and Hexafluoropropylene (HFP) |
| EP3867330A4 (en) * | 2018-10-15 | 2022-07-13 | Honeywell International Inc. | Azeotrope or azeotrope-like compositions of trifluoroiodomethane (cf3i) and hexafluoropropene (hfp) |
| US20200172457A1 (en) * | 2018-12-03 | 2020-06-04 | Honeywell International Inc. | Processes for producing high-purity trifluoroiodomethane |
| WO2020117745A1 (en) * | 2018-12-03 | 2020-06-11 | Honeywell International Inc. | Processes for producing high-purity trifluoroiodomethane |
| US10941091B2 (en) * | 2018-12-03 | 2021-03-09 | Honeywell International Inc. | Processes for producing high-purity trifluoroiodomethane |
| CN113286774A (en) * | 2018-12-03 | 2021-08-20 | 霍尼韦尔国际公司 | Process for preparing high purity trifluoroiodomethane |
| CN113423681A (en) * | 2019-02-18 | 2021-09-21 | 霍尼韦尔国际公司 | One-step process for making trifluoroiodomethane from trifluoroacetyl halide, hydrogen and iodine |
| FR3107280A1 (en) * | 2020-02-19 | 2021-08-20 | Arkema France | Composition comprising an iodofluorocarbon compound |
| WO2021165618A1 (en) * | 2020-02-19 | 2021-08-26 | Arkema France | Composition comprising an iodofluorocarbon compound |
| CN115443175A (en) * | 2020-02-19 | 2022-12-06 | 阿科玛法国公司 | Compositions comprising iodofluorocarbons |
| WO2022082181A1 (en) * | 2020-10-14 | 2022-04-21 | Honeywell International Inc. | Trifluoroacetyl iodide compositions useful for making trifluoroiodomethane |
| WO2022104370A1 (en) * | 2020-11-13 | 2022-05-19 | Honeywell International Inc. | Methods for separation of azeotrope or azeotrope-like compositions of trifluoroiodomethane (cf3i) and trifluoroacetyl chloride (cf3coci) |
| US11565992B2 (en) | 2020-11-13 | 2023-01-31 | Honeywell International Inc. | Methods for separation of azeotrope or azeotrope-like compositions of trifluoroiodomethane (CF3I) and trifluoroacetyl chloride (CF3COCI) |
| CN113214794B (en) * | 2021-04-26 | 2022-07-08 | 泉州宇极新材料科技有限公司 | Near-azeotropic mixture of trifluoroiodomethane and octafluorobutene, preparation method and application thereof |
| CN113214794A (en) * | 2021-04-26 | 2021-08-06 | 泉州宇极新材料科技有限公司 | Near-azeotropic mixture of trifluoroiodomethane and octafluorobutene, preparation method and application thereof |
| CN115181004A (en) * | 2022-09-09 | 2022-10-14 | 天津绿菱气体有限公司 | Preparation method of trifluoroiodomethane |
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