CN104072331A - System and method for preparation and rectification separation of polyfluoro iodoalkane - Google Patents
System and method for preparation and rectification separation of polyfluoro iodoalkane Download PDFInfo
- Publication number
- CN104072331A CN104072331A CN201310100123.8A CN201310100123A CN104072331A CN 104072331 A CN104072331 A CN 104072331A CN 201310100123 A CN201310100123 A CN 201310100123A CN 104072331 A CN104072331 A CN 104072331A
- Authority
- CN
- China
- Prior art keywords
- reactor
- rectifying device
- rectifying
- tower
- cut
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a system and a method for preparation and separation of polyfluoro organic compounds and particularly relates to a system and a method for preparation and rectification separation of polyfluoro iodoalkane. The system for preparation and rectification separation of the polyfluoro iodoalkane comprises three reactors, four rectification devices and a plurality of product storage tanks. The four rectification devices are connected in sequence. In the three reactors, the first reactor is connected to a raw material inlet of the first rectification device, the second rector is connected to the raw material inlet of the second rectification device, the third reactor is connected to the raw material inlet of the third rectification device, fraction outlets of the rectification devices are connected to the inlets of the product storage tanks, and the outlets of the product storage tanks are connected to the reactors. According to the method provided by the invention, single-component perfluoroalkyl iodide of C2, C4, C6 and C8 can be obtained by a plurality of cyclic operation, the purity reaches over 99%, and the high-purity perfluoroalkyl iodide of different components can be collected according to market needs and sold as intermediate products, thus achieving good economic benefit.
Description
Technical field
The invention belongs to acyclic organic compound field, be specifically related to the system and method that a kind of polyfluoro organic compound preparation separates.
Background technology
Full-fluorine alkyl iodide is a class important in organic fluoride, it is the intermediate of synthetic numerous organic fluorides, full-fluorine alkyl iodide has the feature of " two hate three height " (hydrophobic, hate oil, high thermal stability, high chemical stability, high surface), can obtain multiple fine chemicals by full-fluorine alkyl iodide through substitution reaction, also there is These characteristics.Wherein the full-fluorine alkyl iodide of C6～12 has more use value, is mainly used in the intermediate of telomerization, preparation table surface-active agent, fluorine finishing composition and some fine chemicals.Wherein, the above perfluoroalkyl iodides of C8 and C8 is to prepare one of the fluorochemical surfactant that is most widely used now and intermediate of fabric finishing agent.Range of application with tensio-active agent expands, and fluorochemical surfactant is also because its excellent chemical property enjoys favor.Therefore the preparation of C8 and the above perfluoroalkyl iodides of C8 also becomes focus.
Traditional technique is after the perfluoroalkyl iodides of C2～C6 is mixed, complete and react further synthetic C8 or component more than C10 with tetrafluoroethylene at a reactor or in tubular reactor, can produce like this problems such as reaction raw materials composition is unstable, operational condition difference large, product yield is lower, the obvious increase of cyclical operation amount.
PFEI (C
2f
5i) molecular weight 246, is colourless gas under room temperature, sees that light easily decomposes, and the iodine that dissociates, because this unsettled character becomes a kind of telogen of excellent property.Be a kind of important fluorochemical surfactant intermediate, after telomerizing with tetrafluoroethylene monomer, can obtain active, the broad-spectrum many carbon perfluoroalkyl iodides of chemical property, therefore this material has the wide market space.In synthetic PFEI process, generate material comparatively complicated, wherein taking PFEI as main products, produce many carbon perfluoroalkyl iodides such as perfluor butyl iodide, perfluor iodohexane and perfluor iodo-octane simultaneously.Because many carbon perfluoroalkyl iodides has use value, should reclaim purification as far as possible.
Summary of the invention
For the deficiencies in the prior art, the object of the invention is to propose a kind of preparation and the system of rectifying separation polyfluoro idoalkane.
Another object of the present invention is to propose a kind of preparation and the method for rectifying separation polyfluoro idoalkane.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
Prepare and the system of rectifying separation polyfluoro idoalkane, it comprises 3 reactors, 4 rectifying devices and multiple product storage tank,
Described rectifying device is provided with cut outlet, the feed(raw material)inlet at middle part and the tower reactor of bottom at top; Described 4 rectifying devices are connected successively;
In described 3 reactors, the first reactor is connected with the feed(raw material)inlet of the first rectifying device; The second reactor is connected with the feed(raw material)inlet of the second rectifying device; The 3rd reactor is connected with the feed(raw material)inlet of the 3rd rectifying device;
The cut outlet of described rectifying device is connected with the entrance of product storage tank, and the outlet of product storage tank is connected with reactor.
Wherein, in described 4 rectifying devices, the tower reactor of previous rectifying device is connected with the feed(raw material)inlet of next rectifying device, forms successively and connects, and the product in the tower reactor of previous rectifying device enters a rear rectifying device and carries out rectifying.
Wherein, the outlet of the cut of described three rectifying devices is all connected with product storage tank.Each cut outlet connects a product storage tank.Material in product storage tank can be used as direct distribution, also can be delivered to second and/or the 3rd reactor be reaction raw material.
Wherein, the tower reactor of described the 4th rectifying device is connected with product storage tank.
Described system comprises 4-8 product storage tank.
Prepare and the method for rectifying separation polyfluoro idoalkane, be specially: carry out 1 by 3 reactors and 4 rectifying devices simultaneously) to 3) one or more in reaction:
1) PFEI and tetrafluoroethylene carry out telomerization in the first reactor, and the reaction product obtaining enters the first rectifying device, are separated successively by first to fourth rectifying device;
2) perfluor butyl iodide and tetrafluoroethylene carry out telomerization in the second reactor, and the reaction product obtaining enters the second rectifying device, are separated successively by the second to the 4th rectifying device;
3) perfluor iodohexane and tetrafluoroethylene carry out telomerization in the 3rd reactor, and the reaction product obtaining enters the 3rd rectifying device, are separated successively by the 3rd to the 4th rectifying device.
Wherein, described the first rectifying device separates the cut obtaining and returns the second reactor and carry out telomerization; The second rectifying device separates the cut obtaining and returns the 3rd reactor and carry out telomerization.
Wherein, in described the second reactor, perfluor butyl iodide and tetrafluoroethylene mass ratio are 1:0.7-1; In described the 3rd reactor, perfluor iodohexane and tetrafluoroethylene mass ratio are 1:0.3-0.8.
Wherein, the first reactor working pressure is 0.5～4MPa; Temperature is 20～80 DEG C, reaction times 20～480min, and reactant is PFEI and tetrafluoroethylene, its mass ratio is 8:10～15;
The second reactor working pressure is 0.5～4MPa, and temperature is 20～80 DEG C,
The 3rd reactor working pressure is 0.5～4MPa; Temperature is 20～80 DEG C.
The working pressure of described the first rectifying device is 5～40KPa; Tower reactor temperature is 10～60 DEG C;
Described the second rectifying device working pressure is 5～40Kpa, and tower reactor temperature is 20～120 DEG C;
Described the 3rd rectifying device working pressure is-90～20KPa; Tower reactor temperature is 80～120 DEG C;
Described the 4th rectifying device working pressure is-90～20Kpa, and tower reactor temperature is 80～180 DEG C.
Wherein, described the first rectifying device separates the cut of 12-15 DEG C; Described the second rectifying device separates the cut of 65-68 DEG C; Described the 3rd rectifying device separates the cut of 116-118 DEG C; Described the 4th rectifying device tower top separates the cut of 160-162 DEG C, the product introduction product storage tank of tower reactor.
By above-mentioned method, by the reaction product of PFEI reactor (the first reactor), with in pump delivery to the first rectifying device, isolate C2 and C4 and above heavy constituent; C4 and above heavy constituent are delivered in the second rectifying device with pump, isolate C4 and C6 and above heavy constituent; C6 and above heavy constituent are delivered in the 3rd rectifying device with pump, isolate C6 and C8 and above heavy constituent; C8 and above heavy constituent are delivered in the 4th rectifying device with pump, isolate C8 and C10 and above heavy constituent, thereby obtain C2, the C4 of one-component, the perfluoroalkyl iodides of C6, C8.Then the C2 of one-component, C4, C6 perfluoroalkyl iodides (cut) are delivered to respectively to different reactors and carry out again telomerization, each still reactor product separates by each rectifying tower corresponding to each component more successively, obtain one-component perfluoroalkyl iodides, loop telomerization, until obtain required many carbon perfluoroalkyl iodides.
Beneficial effect of the present invention is:
The method that the present invention proposes separates the reaction product of PFEI, obtains high-purity C2, the C4 of single component, the perfluoroalkyl iodides of C6, C8, then stepwise synthesis C8 and above perfluoroalkyl iodides component.Telomerization is become similar addition reaction by this method, thereby reduced the composition that boils of the height in by product.This technological reaction raw material composition is stable, is conducive to determine operational condition, has increased product yield, has largely reduced cyclical operation amount.Meanwhile, while having the market requirement, as C2, C4, C6, the C8 perfluoroalkyl iodides of one-component, can be used as intermediates direct marketing.
The method that the present invention proposes, by repeatedly cyclical operation, can obtain the one-component perfluoroalkyl iodides of C2, C4, C6, C8, purity reaches more than 99%, can, according to market demand, collect high-purity perfluoroalkyl iodides of different components, sell as intermediates, realize good economic benefit;
Compared with traditional technology, single cycle operation yield of the present invention can reach more than 50%, and operational ton obviously reduces;
The present invention can realize effective separation of different components, ensures the unicity of reaction kettle for reaction thing, and operational condition stabilization, has realized the component stability between batch products.
Brief description of the drawings
Fig. 1 is heating and the rectifying separation system of the embodiment of the present invention 1;
Fig. 2 is C2 reactor;
Fig. 3 is C2 receiving vat.
In figure, 1 is C2 reactor, and 2 is that C4 reactor, 3 is C6 reactor, and 4 is perfluoroalkyl iodides compound storage tank, 5 is C2 receiving vat, and 6 is 1# rectifying tower, and 7 is tower reactor, 8 is 1# condenser, and 9 is 2# condenser, and 10 is 3# condenser, 11 is 4# condenser, and 12 is 2# rectifying tower, and 13 is that 3# rectifying tower, 14 is 4# rectifying tower, 15 is C10 and above receiving vat, and 16 is pump, and 17 is tetrafluoroethylene entrance, 18 is C2 perfluoroalkyl iodides entrance, and 19 is the outlet of removing C2 reactor, and 20 for going the outlet of direct marketing.
Embodiment
Following examples are used for illustrating the present invention, but are not used for limiting the scope of the invention.
Embodiment 1: preparation and rectifying separation system
Referring to Fig. 1.The system of preparation and rectifying separation polyfluoro idoalkane, comprises 3 reactors, is respectively C2 reactor 1, C4 reactor 2, C6 reactor 3.4 rectifying devices, are respectively 1# rectifying tower 6,2# rectifying tower 12,3# rectifying tower 13,4# rectifying tower 14.Native system also comprises multiple product storage tanks, comprises perfluoroalkyl iodides compound storage tank 4, C2 receiving vat 5, C4 receiving vat, C6 receiving vat, C8 receiving vat (unnumbered in figure), C10 and above receiving vat 15, and pump 16.
Rectifying tower is provided with cut outlet, the feed(raw material)inlet at middle part and the tower reactor of bottom 7 at top; Described 4 rectifying tower are connected successively, and the tower reactor of previous rectifying device and the feed(raw material)inlet of next rectifying device are connected.
In described 3 reactors, C2 reactor is connected (Fig. 2) with the feed(raw material)inlet of 1# rectifying tower; C4 reactor is connected with the feed(raw material)inlet of 2# rectifying tower; C6 reactor is connected with the feed(raw material)inlet of 3# rectifying tower; C2 reactor is provided with tetrafluoroethylene entrance 17 and C2 perfluoroalkyl iodides entrance 18.C4 reactor C6 reactor also arranges two entrances.
The cut outlet of rectifying tower is connected with the entrance of product storage tank, and the outlet of product storage tank is connected with reactor.Referring to Fig. 3, the discharging of 1# rectifying tower enters C2 receiving vat 5, and the product of this receiving vat can directly go direct marketing (going direct marketing outlet 20) or remove C2 reactor (going the outlet 19 of C2 reactor).In system, be also provided with some pumps and pipeline, for delivery of material.
The cut outlet of four rectifying devices all connects condenser 8,9,10,11, is then connected with product storage tank.Cut is directly put into storage tank by potential difference, and the outlet of product storage tank is by pump delivery in reactor, and rectifier bottoms tower reactor is connected with pump, transports material to and in next rectifying tower, carries out rectifying again.
The tower reactor of the 4th rectifying device is connected with receiving vat 15.
Embodiment 2: preparation and rectifying separation
Utilize the system of embodiment 1 to operate.
1.C2 reactor operational condition, pressure 2MPa; 30 DEG C of temperature, reaction times 80min, reactant consists of PFEI 800Kg, tetrafluoroethylene 1300Kg.Telomerization obtains product perfluor iodoethane, perfluor butyl iodide, perfluor iodohexane, perfluor iodo-octane (being called for short C2 product, C4 product, C6 product, C8 product), and the idoalkane of longer carbochain (being called for short Cn product).
C2 reactor product enters 1# successively, 2#, and 3#, 4# rectifying tower separates.
1# rectifying tower operational condition, pressure: 10KPa; 10 DEG C of tower reactor temperature, the cut that separates 12-15 DEG C obtains C2 product (380Kg).1# rectifying tower separates the cut obtaining and is introduced into products pot, by the conveying of pump, returns the second reactor and carries out telomerization.
2# rectifying tower operational condition, pressure: 10KPa; 30 DEG C of tower reactor temperature, the cut that separates 65-68 DEG C obtains C4 product (281Kg).2# rectifying tower separates the cut obtaining and is introduced into products pot, by the conveying of pump, returns the 3rd reactor and carries out telomerization.
3# rectifying tower operational condition, pressure :-40KPa; Tower reactor temperature: 80 DEG C, the cut that separates 116-118 DEG C obtains C6 product (181Kg).
4# rectifying tower operational condition, pressure-60KPa; Temperature: 140 DEG C, the cut that tower top separation is 160-162 DEG C obtains C8(111Kg) and tower reactor Cn product (130Kg).
After testing, separate rear each one-component purity more than 99%.Revision test repeatedly under same operation condition, the output relative deviation value of each component, in ± 8%, has reached stable operation object.
2.C4 reactor operational condition, pressure: 2MPa; 30 DEG C of temperature, reaction times 120min, reactant consists of perfluor butyl iodide 800Kg, tetrafluoroethylene 700Kg.
C4 reactor product enters 2# successively, 3#, and 4# rectifying tower separates.
2# rectifying tower operational condition, pressure: 10KPa; 30 DEG C of tower reactor temperature, the cut that separates 65-68 DEG C obtains C4 product (360Kg).
3# rectifying tower operational condition, pressure :-40KPa; Tower reactor temperature: 80 DEG C, the cut that separates 116-118 DEG C obtains C6 product (260Kg).
4# rectifying tower operational condition pressure-60KPa; Temperature: 140 DEG C, the cut that tower top separation is 160-162 DEG C obtains C8(150Kg) and tower reactor Cn product (160Kg)
After testing, separate rear each one-component purity more than 99%.Revision test repeatedly under same operation condition, the relative deviation value of each component output, in ± 5%, has reached stable operation object.
3.C6 reactor operational condition, pressure: 2MPa; Temperature: 60 DEG C, reaction times 180min, reactant consists of perfluor iodohexane 800Kg, tetrafluoroethylene 380Kg.
C6 reactor product enters 3# successively, and 4# rectifying tower separates.
3# rectifying tower operational condition, pressure :-40KPa; Tower reactor temperature: 80 DEG C, separate and obtain C6 product (378Kg).
4# rectifying tower operational condition pressure-60KPa; Temperature: 140 DEG C, tower top separates and obtains C8 product (248Kg), and tower reactor obtains Cn product (301Kg).
By above-mentioned method, by the reaction product of PFEI reactor, to 1# rectifying tower, isolate C2 and C4 and above heavy constituent by pump delivery; C4 and above heavy constituent are delivered in 2# rectifying tower with pump, isolate C4 and C6 and above heavy constituent; C6 and above heavy constituent are delivered in 3# rectifying tower with pump, isolate C6 and C8 and above heavy constituent; C8 and above heavy constituent are delivered in 4# rectifying tower with pump, isolate C8 and C10 and above heavy constituent, thereby obtain C2, the C4 of one-component, the perfluoroalkyl iodides of C6, C8.Then the C2 of one-component, C4, C6 perfluoroalkyl iodides (cut) are delivered to respectively to different reactors and carry out again telomerization, each still reactor product separates by each rectifying tower corresponding to each component more successively, obtain one-component perfluoroalkyl iodides, loop telomerization, until obtain required many carbon perfluoroalkyl iodides.After testing, separate rear each one-component purity more than 99%.Revision test repeatedly under same operation condition, the relative deviation value of each component output, in ± 2%, has reached stable operation object.
Embodiment 3: preparation and rectifying separation
Utilize the system of embodiment 1 to operate.
1.C2 reactor operational condition, pressure: 0.5MPa; Temperature: 20 DEG C, reaction times 200min, reactant consists of PFEI 800Kg, tetrafluoroethylene 1200Kg.Telomerization obtains product perfluor iodoethane, perfluor butyl iodide, perfluor iodohexane, perfluor iodo-octane (being called for short C2 product, C4 product, C6 product, C8 product), and the idoalkane of longer carbochain (being called for short Cn product).
C2 reactor product enters 1# successively, 2#, and 3#, 4# rectifying tower separates.
1# rectifying tower operational condition, pressure: 10KPa; 20 DEG C of tower reactor temperature, the cut that separates 12-15 DEG C obtains C2 product (380Kg).Cut is introduced into products pot, by the conveying of pump, returns the second reactor and carries out telomerization.
2# rectifying tower operational condition, pressure: 10KPa; Tower reactor temperature: 40 DEG C, the cut that separates 65-68 DEG C obtains C4 product (281Kg).2# rectifying tower separates the cut obtaining and is introduced into products pot, by the conveying of pump, returns the 3rd reactor and carries out telomerization.
3# rectifying tower operational condition, pressure-10KPa; 90 DEG C of tower reactor temperature, the cut that separates 116-118 DEG C obtains C6 product (181Kg).
4# rectifying tower operational condition, pressure-10KPa; 150 DEG C of tower reactor temperature, the cut that tower top separation is 160-162 DEG C obtains C8(111Kg) and tower reactor Cn product (130Kg).
After testing, separate rear each one-component purity all more than 99%.Multi-pass operations, the relative deviation value of each component output is in ± 8%.
2.C4 reactor operational condition, pressure 2MPa; 30 DEG C of temperature, reaction times 120min, reactant consists of perfluor butyl iodide 800Kg, tetrafluoroethylene 800Kg.
C4 reactor product enters 2# successively, 3#, and 4# rectifying tower separates.
The cut that the separation of 2# rectifying tower is 65-68 DEG C obtains C4 product (350Kg).
The cut that the separation of 3# rectifying tower is 116-118 DEG C obtains C6 product (260Kg).
The cut that the separation of 4# rectifying tower tower top is 160-162 DEG C obtains C8 product (140Kg), and tower reactor obtains Cn product (160Kg)
After testing, separate rear each one-component purity more than 99%.Multi-pass operations, the relative deviation value of each component output, in ± 5%, reaches stable operation object.
3.C6 reactor operational condition, pressure: 2MPa; Temperature: 60 DEG C, reaction times 180min, reactant consists of perfluor iodohexane 800Kg, tetrafluoroethylene 380Kg.
C6 reactor product enters 3# successively, and 4# rectifying tower separates.
3# rectifying tower separates and obtains C6 product (378Kg).
4# rectifying tower tower top separates and obtains C8 product (248Kg), and tower reactor obtains Cn product (301Kg).
After testing, separate rear each one-component purity more than 99%.The relative deviation value of each component output of multi-pass operations, in ± 2%, reaches stable operation object.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, do not departing under the prerequisite of the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. prepare and the system of rectifying separation polyfluoro idoalkane, it is characterized in that, comprise 3 reactors, 4 rectifying devices and multiple product storage tank;
Described rectifying device is provided with cut outlet, the feed(raw material)inlet at middle part and the tower reactor of bottom at top; Described 4 rectifying devices are connected successively;
In described 3 reactors, the first reactor is connected with the feed(raw material)inlet of the first rectifying device; The second reactor is connected with the feed(raw material)inlet of the second rectifying device; The 3rd reactor is connected with the feed(raw material)inlet of the 3rd rectifying device;
The cut outlet of described rectifying device is connected with the entrance of product storage tank, and the outlet of product storage tank is connected with reactor.
2. system claimed in claim 1, is characterized in that, in described 4 rectifying devices, the tower reactor of previous rectifying device is connected with the feed(raw material)inlet of next rectifying device.
3. the system as claimed in claim 1, is characterized in that, the cut outlet of described three rectifying devices is all connected with product storage tank.
4. the system as described in as arbitrary in claim 1～3, is characterized in that, the tower reactor of described the 4th rectifying device is connected with product storage tank.
5. prepare and the method for rectifying separation polyfluoro idoalkane, it is characterized in that, carry out 1 by 3 reactors and 4 rectifying devices simultaneously) to 3) one or more in reaction:
1) PFEI and tetrafluoroethylene carry out telomerization in the first reactor, and the reaction product obtaining enters the first rectifying device, are separated successively by first to fourth rectifying device;
2) perfluor butyl iodide and tetrafluoroethylene carry out telomerization in the second reactor, and the reaction product obtaining enters the second rectifying device, are separated successively by the second to the 4th rectifying device;
3) perfluor iodohexane and tetrafluoroethylene carry out telomerization in the 3rd reactor, and the reaction product obtaining enters the 3rd rectifying device, are separated successively by the 3rd to the 4th rectifying device.
6. method as claimed in claim 5, is characterized in that, described the first rectifying device separates the cut obtaining and returns the second reactor and carry out telomerization; The second rectifying device separates the cut obtaining and returns the 3rd reactor and carry out telomerization.
7. the method as described in claim 5 or 6, is characterized in that, in described the second reactor, perfluor butyl iodide and tetrafluoroethylene mass ratio are 1:0.7-1; In described the 3rd reactor, perfluor iodohexane and tetrafluoroethylene mass ratio are 1:0.3-0.8.
8. the method as described in claim 5 or 6, is characterized in that,
The first reactor working pressure is 0.5～4MPa; Temperature is 20～80 DEG C, reaction times 20～480min, and reactant is PFEI and tetrafluoroethylene, its mass ratio is 8:10～15;
The second reactor working pressure is 0.5～4MPa, and temperature is 20～80 DEG C,
The 3rd reactor working pressure is 0.5～4MPa; Temperature is 20～80 DEG C.
9. the method as described in claim 5 or 6, is characterized in that, the working pressure of described the first rectifying device is 5～40KPa; Tower reactor temperature is 10～60 DEG C;
Described the second rectifying device working pressure is 5～40Kpa, and tower reactor temperature is 20～120 DEG C;
Described the 3rd rectifying device working pressure is-90～20KPa; Tower reactor temperature is 80～120 DEG C;
Described the 4th rectifying device working pressure is-90～20Kpa, and tower reactor temperature is 80～180 DEG C.
10. the method as described in claim 5 or 6, is characterized in that, described the first rectifying device separates the cut of 12-15 DEG C; Described the second rectifying device separates the cut of 65-68 DEG C; Described the 3rd rectifying device separates the cut of 116-118 DEG C; Described the 4th rectifying device tower top separates the cut of 160-162 DEG C, the product introduction product storage tank of tower reactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310100123.8A CN104072331B (en) | 2013-03-26 | 2013-03-26 | A kind ofly prepare the system and method with rectifying separation polyfluoro idoalkane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310100123.8A CN104072331B (en) | 2013-03-26 | 2013-03-26 | A kind ofly prepare the system and method with rectifying separation polyfluoro idoalkane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104072331A true CN104072331A (en) | 2014-10-01 |
| CN104072331B CN104072331B (en) | 2016-01-13 |
Family
ID=51593983
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310100123.8A Active CN104072331B (en) | 2013-03-26 | 2013-03-26 | A kind ofly prepare the system and method with rectifying separation polyfluoro idoalkane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104072331B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105396604A (en) * | 2015-09-14 | 2016-03-16 | 巨化集团技术中心 | Supported catalyst and applications of supported catalyst in perfluoro iodocarbon compound synthesis |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1364934A1 (en) * | 2001-02-07 | 2003-11-26 | Daikin Industries, Ltd. | Method for producing fluoroalkyl iodide telomer mixture and method for producing fluorine-containing (meth)acrylate ester |
| JP2004269413A (en) * | 2003-03-07 | 2004-09-30 | Daikin Ind Ltd | Method for preparing fluoroalykyl iodide telomer mixture and fluorine-containing (meth)acrylic ester mixture |
-
2013
- 2013-03-26 CN CN201310100123.8A patent/CN104072331B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1364934A1 (en) * | 2001-02-07 | 2003-11-26 | Daikin Industries, Ltd. | Method for producing fluoroalkyl iodide telomer mixture and method for producing fluorine-containing (meth)acrylate ester |
| JP2004269413A (en) * | 2003-03-07 | 2004-09-30 | Daikin Ind Ltd | Method for preparing fluoroalykyl iodide telomer mixture and fluorine-containing (meth)acrylic ester mixture |
Non-Patent Citations (1)
| Title |
|---|
| 席先锋等: "全氟碘代烷调聚工艺研究", 《有机氟工业》, no. 1, 31 December 2005 (2005-12-31), pages 15 - 19 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105396604A (en) * | 2015-09-14 | 2016-03-16 | 巨化集团技术中心 | Supported catalyst and applications of supported catalyst in perfluoro iodocarbon compound synthesis |
| CN105396604B (en) * | 2015-09-14 | 2017-10-20 | 巨化集团技术中心 | A kind of loaded catalyst and its application in the synthesis of perfluor iodine hydrocarbon compound |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104072331B (en) | 2016-01-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103709124B (en) | A kind of method of producing epoxy chloropropane | |
| CN1140488C (en) | Method of preparing monofluoromethyl ethers | |
| CN105593165B (en) | The refining methd of phosphorus pentafluoride | |
| CN104364197A (en) | High-purity lithium hexafluorophosphate | |
| CN100509735C (en) | Production of fluormethyl 2,2,2-trifluoro-1-(trifluoromethyl) ethyl ether | |
| US20240050792A1 (en) | Azeotropic or azeotropic-like composition comprising hydrogen fluoride and 1,1,2-trifluoroethane, 1-chloro-2,2-difluoroethane, or 1,2-dichloro-1-fluoroethane | |
| CN104072331B (en) | A kind ofly prepare the system and method with rectifying separation polyfluoro idoalkane | |
| CN101891583A (en) | Method for co-production of trichloroethylene and tetrachloroethylene by gas phase catalysis method | |
| CZ290462B6 (en) | Process for preparing 1,2-dichloroethane by direct chlorination and apparatus for making the same | |
| CN101747238A (en) | Method for separating and preparing methanesulfonyl fluoride CH3SO2F by material generated after reaction of methylsufonyl chloride and potassium fluoride | |
| CN109111477A (en) | A kind of Industrialized synthesis method of dichloromethylphosphine | |
| CN102527414B (en) | Fluorination catalyst for preparing difluoromethane or monochlorodifluoromethane, preparation method and application | |
| KR101127162B1 (en) | Preparing method and apparatus of preparing hydrofluoroether in a semi-continuous process | |
| CN113104823A (en) | Synthesis method of bis (fluorosulfonyl) imide | |
| KR101789849B1 (en) | Process for production of fluoroalkyl iodide | |
| CN109485548B (en) | Method and device for preparing and separating sec-butyl alcohol by hydrolyzing sec-butyl acetate | |
| CN205099353U (en) | Defluorinate equipment of hydrochloric acid in fluorochlorohydrocarbon production technology | |
| JP2017137263A (en) | Method for producing 1,1,1,3-tetrachloropropane | |
| EP2589585B1 (en) | Method for preparing chlorohydrins and method for preparing epichlorohydrin using chlorohydrins prepared thereby | |
| KR20160149440A (en) | Method for separating 3-hydroxypropionic acid and Acrylic Acid | |
| CN105582811A (en) | Raw material purification method for boron isotope separation | |
| CN110433743A (en) | The preparation facilities of perfluor isobutyl acyl fluorides | |
| CN104262207B (en) | A kind of preparation method of sulfonic fluoropolymer compounds | |
| CN111659322A (en) | Device and process for preparing 1,1,1, 3-tetrachloropropane | |
| CN103880588A (en) | Method for preparing perfluoroalkyl iodine through catalytic distillation telomerization |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |