CN108675914A - A method of preparing high-purity trifluoroiodomethane - Google Patents
A method of preparing high-purity trifluoroiodomethane Download PDFInfo
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- CN108675914A CN108675914A CN201810628166.6A CN201810628166A CN108675914A CN 108675914 A CN108675914 A CN 108675914A CN 201810628166 A CN201810628166 A CN 201810628166A CN 108675914 A CN108675914 A CN 108675914A
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- trifluoroiodomethane
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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
- C07C17/389—Separation; Purification; Stabilisation; Use of additives by adsorption on solids
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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
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
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Abstract
The invention discloses a kind of methods preparing high-purity trifluoroiodomethane.Raw material trifluoroiodomethane is under certain temperature and pressure, pass through two-stage adsorption column with certain flow, after removing most of water and part organic impurities, into in rectifying column, batch fractionating is carried out at low temperature, tower top emptying removes the impurity such as halogenated alkane, alkenyl halide, halogenated alkynes, nitrogen, oxygen, carbon dioxide, the carbon monoxide of C1 C5, to obtain high-purity trifluoroiodomethane that purity is more than 99.99%, wherein H2O content is less than 30ppmv, and HF contents are less than 1ppmw, meet semiconductor etching and electric insulation industry requirement.This method rational technology, it is easy to operate, it is the desirable technique for preparing high-purity trifluoroiodomethane.
Description
Technical field
The invention belongs to fluorinated organic compound preparing technical fields, are related to the preparation method of high-purity trifluoroiodomethane.
Background technology
Trifluoroiodomethane is most important a kind of product in perfluoroalkyl iodide hydrocarbon, in fire extinguishing, refrigeration, organic synthesis, is partly led
The fields such as body etching, electric insulation extensive application foreground.
General industry product trifluoroiodomethane purity wherein including a variety of inorganic and organic impurities, and works as three 95~99%
Fluorine iodomethane is used as electronics etching gas, or for electric insulation field when, contained by dopant species and quantity pair
There is conclusive influence in downstream product performance, it is therefore desirable to control each impurity content in trifluoroiodomethane, improve product
Purity.
For trifluoroiodomethane method of purification at present disclose report it is less, patent 201710631402.5 reports one kind
The process for separating and purifying of trifluoroiodomethane, this method purify trifluoroiodomethane by the way of extracting rectifying, utilize three
The difference of fluorine iodomethane and the impurity solubility in extractant realizes the refined of target product, and it is big that purity can be obtained using this method
In 99.9% trifluoroiodomethane sterling.However, the patent is not clear for the content of the inorganic impurity in final products
Illustrate, such as N2、O2、H2O、HF、CO2Deng.The presence of these inorganic impurities has semiconductor etching and electric insulation industry important
It influences, especially H2O content generally requires to be less than 50ppmv, and HF contents need to be less than 1ppmw, it is therefore desirable to which exploitation is a kind of new
Purifying technique, so that organic and inorganic impurity content in trifluoroiodomethane is met semiconductor etching and electric insulation industry requirement.
Invention content
The technical problem to be solved in the present invention is, fills up the blank of high-purity trifluoroiodomethane technology of preparing, provides one kind
Technological process is simple, the easily controllable purifying technique of operating process.
The technical solution adopted by the present invention is as follows：
A method of high-purity trifluoroiodomethane being prepared, using following sequential steps：
1) under conditions of closed environment, by raw material trifluoroiodomethane under gas phase condition enter adsorption column remove water and
Part organic impurities；
2) trifluoroiodomethane introduces rectifying column after absorption, carries out batch fractionating, and tower top emptying removes the halogenated of C1-C5
After alkane, alkenyl halide, halogenated alkynes, nitrogen, oxygen, carbon dioxide, carbon monoxide impurities, regathers purity and be more than
The 99.99% filling preservation of high-purity trifluoroiodomethane；
Adsorbent is silica gel, activated alumina, activated carbon, carbon molecular sieve, A type molecular sieve, X-type molecule wherein in adsorption column
Sieve, Y type molecular sieve, type ZSM 5 molecular sieve.
Wherein adsorption column uses two-stage series connection, the preferred silica gel of adsorbent, activated alumina, carbon molecular sieve, A type molecular sieve.
Absorbing process condition in the step 1)：Temperature is -20~50 DEG C, and pressure is -0.1~0.2MPa, gas flow
For 10~1000g/h.
Preferable temperature is 0-30 DEG C, and pressure is 0~0.1MPa, and gas flow is 500~800g/h.
Air speed is 10~300h in the step 1)-1.Air speed is the gas in the unit time, handled by unit volume adsorbent
The scale of construction, air speed=gas flow (L/h)/quantity of sorbent (L)
Rectification temperature -50~20 DEG C in the step 2).
Preferably -25~10 DEG C of rectification temperature in the step 2).
Tower top emptying speed is 0.1~10L/min, emptying time 5-60min in the step 2).
It is preferred that tower top emptying speed is 0.1~3L/min, emptying time 10-30min.；
The raw material trifluoroiodomethane purity is 95-99%.
Filling in step 2) is saved as filling is closed high-purity trifluoroiodomethane is pressurized liquefied using diaphragm type compressor in aluminium
In golden container.
The purifying technique of the present invention removes water and part organic impurities using secondary absorption, then using cryogenic rectification
Inorganic gas and low-boiling point gas emptying are removed, regather 99.99% high-purity trifluoroiodomethane, wherein H by mode2O content
Less than 30ppmv, HF contents are less than 1ppmw, meet semiconductor etching and electric insulation industry requirement.
Advantageous effect
1. preparation method rational technology of the present invention is simple, easily operated, non-pollutant discharge belongs to closed-loop system；
2. stable preparation process of the present invention is reliable, it is suitble to large-scale industrial production.
Description of the drawings
Fig. 1 is high-purity trifluoroiodomethane preparation technology flow chart
Specific embodiment
With reference to embodiment, the present invention will be further described, but does not limit the invention to these specific embodiment parties
Formula.As shown in Figure 1, raw material trifluoroiodomethane after adsorption tower 1# and adsorption tower 2#, eliminates water and part organic impurities,
Trifluoroiodomethane through absorption is imported in rectifying column, tower top emptying removes halogenated alkane, alkenyl halide, the acetylenic halide of C1-C5
After hydrocarbon, nitrogen, oxygen, carbon dioxide, carbon monoxide impurities, regather purity more than 99.99% high-purity trifluoroiodomethane in
In air accumulator, finally utilize diaphragm type compressor that high-purity trifluoroiodomethane is pressurized liquefied filling in aluminum alloy container.
Each impurity content such as following table in trifluoroiodomethane crude product used herein：
1 trifluoroiodomethane crude product impurity content of table
Embodiment 1
Raw material trifluoroiodomethane is at 10 DEG C, under conditions of 0MPa, enters two-stage adsorption column, primary adsorption with 140g/h flows
Silica gel absorber is loaded in column, 3A adsorbent of molecular sieve is loaded in secondary absorption column, removes most of water and part organic impurities；
Rectifying column is introduced after absorption, batch fractionating is carried out at -10~0 DEG C, and tower top emptying flow is 0.3L/min, emptying
Time 30min, detection overhead product purity reach 99.99% or more, product are discharged into air accumulator, is filled with diaphragm type compressor
Into steel cylinder.
Embodiment 2
Raw material trifluoroiodomethane is at 20 DEG C, under conditions of 0.1MPa, enters two-stage adsorption column with 200g/h flows, level-one is inhaled
Activated alumina adsorbents are loaded in attached column, 5A adsorbent of molecular sieve is loaded in secondary absorption column, remove most of water and part
Organic impurities；
Rectifying column is introduced after absorption, batch fractionating is carried out at -15~-10 DEG C, and tower top emptying flow is 0.5L/min, is put
Empty time 20min, detection overhead product purity reach 99.99% or more, product are discharged into air accumulator, is filled with diaphragm type compressor
It feed into steel cylinder.
Embodiment 3
Raw material trifluoroiodomethane enters two-stage adsorption column, level-one under conditions of -10 DEG C, -0.05MPa, with 70g/h flows
Silica gel absorber is loaded in adsorption column, 10X adsorbent of molecular sieve is loaded in secondary absorption column, removes most of water and part is organic
Impurity；
Rectifying column is introduced after absorption, batch fractionating is carried out at -21~-16 DEG C, and tower top emptying flow is 0.8L/min, is put
Empty time 10min, detection overhead product purity reach 99.99% or more, product are discharged into air accumulator, is filled with diaphragm type compressor
It feed into steel cylinder.
Embodiment 4
Raw material trifluoroiodomethane is at 30 DEG C, under conditions of 0.05MPa, enters two-stage adsorption column, level-one with 500g/h flows
Acticarbon is loaded in adsorption column, carbon molecular sieve adsorbent is loaded in secondary absorption column, and removing most of water and part has
Machine impurity；
Rectifying column is introduced after absorption, batch fractionating is carried out at -25~-18 DEG C, and tower top emptying flow is 0.1L/min, is put
Empty time 30min, detection overhead product purity reach 99.99% or more, product are discharged into air accumulator, is filled with diaphragm type compressor
It feed into steel cylinder.
Embodiment 5
Raw material trifluoroiodomethane is at 25 DEG C, under conditions of 0.2MPa, enters two-stage adsorption column with 300g/h flows, level-one is inhaled
Silica gel absorber is loaded in attached column, 13X adsorbent of molecular sieve is loaded in secondary absorption column, removes most of water and part is organic miscellaneous
Matter；
Rectifying column is introduced after absorption, batch fractionating is carried out at -20~-15 DEG C, and tower top emptying flow is 0.3L/min, is put
Empty time 30min, detection overhead product purity reach 99.99% or more, product are discharged into air accumulator, is filled with diaphragm type compressor
It feed into steel cylinder.
Each embodiment experimental result is shown in Table 2
2 each embodiment experimental result of table
| Index | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| H2O | 18.5ppmv | 9.8ppmv | 22.1ppmv | 25.6ppmv | 19.3ppmv |
| N2+O2 | 22ppmv | 15ppmv | 28ppmv | 17ppmv | 20ppmv |
| CO2 | 2.3ppmv | 4.3ppmv | 5.5ppmv | 4.1ppmv | 2.5ppmv |
| CO | 1.5ppmv | 2.2ppmv | 2.4ppmv | 4.2ppmv | 3.1ppmv |
| Nine fluorine butane of 2H- | 12.3ppmv | 10.9ppmv | 14.6ppmv | 18.9ppmv | 17.1ppmv |
| Perfluor -2- butylene | 9.5ppmv | 9.0ppmv | 7.2ppmv | 6.5ppmv | 8.1ppmv |
| Hexafluoro-1,3-butadiene | 2.1ppmv | 3.3ppmv | 4.1ppmv | 6.5ppmv | 3.5ppmv |
| Perfluoropropane | 15.1ppmv | 16.3ppmv | 20.1ppmv | 11.2ppmv | 18.2ppmv |
| HF | 0.5ppmw | 0.3ppmw | 0.3ppmw | 0.7ppmw | 0.5ppmw |
● the detection of He ion chromatographies limits minimum 10ppbv
By above example data it is found that can be improved industrial goods trifluoroiodomethane purity extremely by 97.8% using the technique
99.99% or more.H simultaneously2O content is less than 30ppmv, and HF contents are less than 1ppmw, meet semiconductor etching and electric insulation row
Industry requirement.
Claims (10)
1. a kind of method preparing high-purity trifluoroiodomethane, using following sequential steps：
1) under conditions of closed environment, raw material trifluoroiodomethane is entered into adsorption column under gas phase condition and removes water and part
Organic impurities；
2) trifluoroiodomethane introduces rectifying column after absorption, carries out batch fractionating, and tower top emptying removes the alkyl halide of C1-C5
After hydrocarbon, alkenyl halide, halogenated alkynes, nitrogen, oxygen, carbon dioxide, carbon monoxide impurities, regathers purity and be more than 99.99%
The filling preservation of high-purity trifluoroiodomethane；
Adsorbent is silica gel, activated alumina, activated carbon, carbon molecular sieve, A type molecular sieve, X-type molecular sieve, Y wherein in adsorption column
Type molecular sieve, type ZSM 5 molecular sieve.
2. according to the method described in claim 1, the adsorption column is two-stage series connection adsorption column, wherein adsorbent is silica gel, work
Property aluminium oxide, carbon molecular sieve, A type molecular sieve.
3. according to the method described in claim 1, absorbing process condition in the step 1)：Temperature is -20~50 DEG C, pressure
For -0.1~0.2MPa, gas flow is 10~1000g/h.
4. according to the method described in claim 3, absorbing process condition in the step 1)：Temperature be 0-30 DEG C, pressure be 0~
0.1MPa, gas flow are 500~800g/h.
5. according to the method described in claim 3, air speed is 10~300h in the step 1)-1。
6. according to the method described in claim 1, rectification temperature is -50~20 DEG C in the step 2).
7. according to the method described in claim 6, rectification temperature is -25~10 DEG C in the step 2).
8. according to the method described in claim 6, tower top emptying speed is 0.1~10L/min, emptying time in the step 2)
5-60min。
9. according to the method described in claim 8, tower top emptying speed is 0.1~3L/min, emptying time 10-30min.
10. according to the method described in claim 1, filling in step 2) is saved as high-purity trifluoro iodine using diaphragm type compressor
Methane is pressurized liquefied filling in aluminum alloy container.
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Cited By (4)
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| CN111253209A (en) * | 2020-03-16 | 2020-06-09 | 天津绿菱气体有限公司 | Preparation method of trifluoroiodomethane with high conversion rate |
| 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 |
| CN113286774A (en) * | 2018-12-03 | 2021-08-20 | 霍尼韦尔国际公司 | Process for preparing high purity trifluoroiodomethane |
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| CN113286774A (en) * | 2018-12-03 | 2021-08-20 | 霍尼韦尔国际公司 | Process for preparing high purity trifluoroiodomethane |
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| CN111253209A (en) * | 2020-03-16 | 2020-06-09 | 天津绿菱气体有限公司 | Preparation method of trifluoroiodomethane with high conversion rate |
| 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 |
| 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 |
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Application publication date: 20181019 |