CN203540491U - Reactor for preparing antimony pentafluoride - Google Patents
Reactor for preparing antimony pentafluoride Download PDFInfo
- Publication number
- CN203540491U CN203540491U CN201320730036.6U CN201320730036U CN203540491U CN 203540491 U CN203540491 U CN 203540491U CN 201320730036 U CN201320730036 U CN 201320730036U CN 203540491 U CN203540491 U CN 203540491U
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- CN
- China
- Prior art keywords
- reactor
- antimony
- tray
- reaction
- valve
- 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.)
- Expired - Lifetime
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- 229910021630 Antimony pentafluoride Inorganic materials 0.000 title claims abstract description 26
- VBVBHWZYQGJZLR-UHFFFAOYSA-I antimony pentafluoride Chemical compound F[Sb](F)(F)(F)F VBVBHWZYQGJZLR-UHFFFAOYSA-I 0.000 title claims abstract description 26
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 27
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 27
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000011737 fluorine Substances 0.000 claims abstract description 14
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 14
- 238000007599 discharging Methods 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 18
- 238000000034 method Methods 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 14
- 238000010992 reflux Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- BNZTUWKQHHYTKS-UHFFFAOYSA-K [Sb](Cl)(Cl)Cl.[F] Chemical compound [Sb](Cl)(Cl)Cl.[F] BNZTUWKQHHYTKS-UHFFFAOYSA-K 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- VMPVEPPRYRXYNP-UHFFFAOYSA-I antimony(5+);pentachloride Chemical compound Cl[Sb](Cl)(Cl)(Cl)Cl VMPVEPPRYRXYNP-UHFFFAOYSA-I 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002887 superconductor Substances 0.000 description 1
Images
Abstract
The utility model discloses a reactor for preparing antimony pentafluoride. The reactor is internally and respectively provided with an antimony tray and a condenser from bottom to top; the side wall of the reactor, which is level to the antimony tray, is provided with a steam heating sleeve and a feeding hole; the bottom of the reactor is provided with a fluorine inlet and a discharging port; the top of the reactor is provided with an emptying valve, a pressurizing valve and a pressure gauge valve; and the bottom of the antimony tray has two or more small gas inlet holes. The reactor disclosed by the utility model has the advantages that fluorine reacts with metal antimony directly to generate the antimony pentafluoride, so that the quality of a product is improved, simultaneously the simplifying action to the process is also achieved and the operation is convenient; the antimony tray has the small gas inlet holes, so that the reaction is complete; condensed and returned liquid takes away partial reaction heat, so that the temperature in the reactor is well controlled, and simultaneously the continuous conduction of reaction is also guaranteed; and the internal chemical corrosion of the reaction is reduced, so that the service life of the reactor is prolonged.
Description
Technical field
The utility model has related to the production equipment of antimony pentafluoride, relates in particular to a kind of reactor of preparing antimony pentafluoride.
Background technology
Antimony pentafluoride can form and embed compound with graphite and fluorographite, and they have than graphite and the much higher conducting power of fluorographite, likely as superconductor.Antimony pentafluoride is a kind of high energy fluorization agent, is widely used in medical pharmacy industry (anticancer class medicine).
Produce at present the mode more complicated of antimony pentafluoride, the product degree of depositing that reaction generates is not high, impurity separation difficulty.To equipment require high.Concrete mode is as follows:
To being equipped with in the aluminum reactor of gas introduction tube, reflux condenser, thermometer boss, add Antimony pentachloride 600g, the temperature of reflux condenser is remained on-45 degree.Make the temperature of reactant mixture maintain 10～35 degree on one side, among 2～3hs from gas introduction tube import hydrogen fluoride gas 360g on one side.Be heated to 60～70 degree, to stopping producing after hydrogen chloride, be cooled to 40 degree thereafter.Then reflux condensation mode actuator temperature is risen to 12～25 degree.To steam unreacted hydrogen fluoride.Finally, reactor is heated to 140～150 degree, to eliminate hydrogen fluoride.Now the residue in reactor is thick antimony pentafluoride, and contains a small amount of fluorine antimony chloride impurity.Thick antimony pentafluoride is carried out to fractionation with aluminum device, and airtight being kept in aluminum container.
Utility model content
The purpose of this utility model is in order to overcome above-mentioned the deficiencies in the prior art, provides a kind of reactive mode fairly simple antimony pentafluoride reactor.
To achieve these goals, the technical solution adopted in the utility model is:
A kind of reactor of preparing antimony pentafluoride, in reactor, be respectively equipped with from lower to upper antimony pallet and condenser, the sidewall of reactor and antimony pallet level is provided with steam jacket and charging aperture, reactor bottom starts to have into fluorine gas mouth and discharging opening, the top of reactor is provided with emptying valve, pressurization valve and pressure gage valve, and described antimony tray bottom is provided with two or more small air inlet holes.
Wherein, described condenser is shell and tube condenser.
For better observing response situation, the utility model is further optimized, and described antimony tray bottom is also provided with thermometer.
For sampling in course of reaction detects, described reactor bottom is further provided with sample cock.
The beneficial effects of the utility model are: this reacting appliance system for antimony pentafluoride is, by fluorine gas directly and the metallic antimony generation antimony pentafluoride that reacts, when improving the quality of products, also technique have been played to simplification effect, easy to operate.Described antimony pallet is provided with small air inlet hole so that reaction is more abundant, and condensation reflux liquid is taken away the temperature that part reaction heat has well been controlled inside reactor, has also guaranteed that the continuity of reaction is carried out simultaneously.Reduce inside reactor chemical attack, thereby extended the life-span of reactor.
Accompanying drawing explanation
Fig. 1 is the structural representation of the utility model reactor;
Wherein,
1, enter fluorine gas mouth; 2, discharging opening; 3, sample cock; 4, thermometer; 5, antimony pallet; 6, steam jacket; 7, charging aperture; 8, condenser; 9, emptying valve; 10, pressure gage valve; 11, pressurization valve.
The specific embodiment
By describing technology contents of the present utility model, structural feature in detail, being realized object and effect, below in conjunction with embodiment and coordinate accompanying drawing to be explained in detail.
See also Fig. 1, as shown in the figure, in the utility model reactor, be respectively equipped with from lower to upper antimony pallet 5 and condenser 8, the sidewall of reactor and antimony pallet 5 levels is provided with steam jacket 6 and charging aperture 7, and described antimony pallet 5 is provided with small air inlet hole so that reaction is more abundant; Metallic antimony is placed on antimony pallet 5 by charging aperture 7, by 6 pairs of reactors of steam jacket, heated, described condenser 8 is general stram condenser, the present embodiment adopts shell and tube condenser, reactor bottom starts to have into fluorine gas mouth 1 and discharging opening 2, enter fluorine gas mouth 1 and be communicated with outside fluorine gas by pipeline and fluorine gas valve, the top of reactor is provided with emptying valve 9, pressurization valve 11 and pressure gage valve 10.For better observing response situation, the utility model is further optimized, and described antimony tray bottom is also provided with thermometer 4.For sampling in course of reaction detects, described reactor bottom is further provided with sample cock 3.
Said structure, when specifically preparing antimony pentafluoride, comprises the following steps:
1) metallic antimony is carried out to fragmentation soon, particle diameter is controlled at 1cm left and right, adds on the antimony pallet in reactor;
2) reactor is taken out to negative pressure, and be heated to 120 degree by steam jacket, remove the moisture content in reactor and material;
3) to passing into nitrogen in reactor, be pressurized to normal pressure;
4) by entering fluorine gas mouth, to reactor, pass into slowly fluorine gas, fluorine gas react and generates antimony pentafluoride steam with metallic antimony on antimony pallet when rising from bottom, starts intensification, through repeatedly emptying at this moment reacting, discharge nitrogen remaining in reactor, until surge tank pressure no longer rises;
5) antimony pentafluoride steam is refluxed and is formulated antimony pentafluoride finished product by condenser condenses.
For more effective control reaction temperature, in step 5), the antimony pentafluoride finished product of condensing reflux is taken away to a part of heat through conversion zone.The antimony pentafluoride dropping process of condensing reflux is taken away part heat, makes reaction temperature finally maintain a stationary value, and question response temperature starts to decline, and when reactor pressure starts to rise, reaction is reached home.By fluorine gas directly and the metallic antimony generation antimony pentafluoride that reacts, when improving the quality of products, also technique has been played to simplification effect, easy to operate.Condensation reflux liquid is taken away the temperature that part reaction heat has well been controlled inside reactor, has also guaranteed that the continuity of reaction is carried out simultaneously.Reduce inside reactor chemical attack, thereby extended the life-span of reactor.
The foregoing is only embodiment of the present utility model; not thereby limit the scope of the claims of the present utility model; every equivalent structure or conversion of equivalent flow process that utilizes the utility model description and accompanying drawing content to do; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present utility model.
Claims (4)
1. a reactor of preparing antimony pentafluoride, it is characterized in that, in reactor, be respectively equipped with from lower to upper antimony pallet and condenser, the sidewall of reactor and antimony pallet level is provided with steam jacket and charging aperture, reactor bottom starts to have into fluorine gas mouth and discharging opening, the top of reactor is provided with emptying valve, pressurization valve and pressure gage valve, and described antimony tray bottom is provided with two or more small air inlet holes.
2. the reactor of preparing antimony pentafluoride according to claim 1, is characterized in that, described condenser is shell and tube condenser.
3. the reactor of preparing antimony pentafluoride according to claim 1, is characterized in that, described antimony tray bottom is also provided with thermometer.
4. the reactor of preparing antimony pentafluoride according to claim 3, is characterized in that, described reactor bottom is further provided with sample cock.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320730036.6U CN203540491U (en) | 2013-11-18 | 2013-11-18 | Reactor for preparing antimony pentafluoride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320730036.6U CN203540491U (en) | 2013-11-18 | 2013-11-18 | Reactor for preparing antimony pentafluoride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN203540491U true CN203540491U (en) | 2014-04-16 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201320730036.6U Expired - Lifetime CN203540491U (en) | 2013-11-18 | 2013-11-18 | Reactor for preparing antimony pentafluoride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN203540491U (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105352339A (en) * | 2015-08-11 | 2016-02-24 | 中国矿业大学 | Evaporative condenser used for chemical industry |
| CN107128896A (en) * | 2017-07-17 | 2017-09-05 | 洛阳森蓝化工材料科技有限公司 | A kind of fluorographite pipe reaction stove |
| CN114655982A (en) * | 2022-04-07 | 2022-06-24 | 九江诺尔新材料科技有限公司 | Continuous production method and application of antimony pentafluoride |
-
2013
- 2013-11-18 CN CN201320730036.6U patent/CN203540491U/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105352339A (en) * | 2015-08-11 | 2016-02-24 | 中国矿业大学 | Evaporative condenser used for chemical industry |
| CN105352339B (en) * | 2015-08-11 | 2019-04-23 | 中国矿业大学 | A kind of evaporative condenser for chemical industry |
| CN107128896A (en) * | 2017-07-17 | 2017-09-05 | 洛阳森蓝化工材料科技有限公司 | A kind of fluorographite pipe reaction stove |
| CN114655982A (en) * | 2022-04-07 | 2022-06-24 | 九江诺尔新材料科技有限公司 | Continuous production method and application of antimony pentafluoride |
| CN114655982B (en) * | 2022-04-07 | 2023-09-08 | 九江诺尔新材料科技有限公司 | Continuous production method and application of antimony pentafluoride |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 354000 Nanping Province, Shaowu City, sun mouth new ammonia Road, No. 18 Patentee after: FUJIAN YONGJING TECHNOLOGY Co.,Ltd. Address before: 354000 Nanping Province, Shaowu City, sun mouth new ammonia Road, No. 18 Patentee before: FUJIAN SHAOWU YONGJING CHEMICAL Co.,Ltd. |
|
| CP03 | Change of name, title or address |
Address after: 354001 Jinling Road, Jintong Industrial Park, Shaowu, Fujian Province, No. 6 Patentee after: FUJIAN YONGJING TECHNOLOGY CO.,LTD. Address before: 354000 Nanping Province, Shaowu City, sun mouth new ammonia Road, No. 18 Patentee before: FUJIAN YONGJING TECHNOLOGY Co.,Ltd. |
|
| CP03 | Change of name, title or address | ||
| CX01 | Expiry of patent term |
Granted publication date: 20140416 |
|
| CX01 | Expiry of patent term |