CN211724739U - Difluoro trichloroethane purification device - Google Patents
Difluoro trichloroethane purification device Download PDFInfo
- Publication number
- CN211724739U CN211724739U CN201922440813.3U CN201922440813U CN211724739U CN 211724739 U CN211724739 U CN 211724739U CN 201922440813 U CN201922440813 U CN 201922440813U CN 211724739 U CN211724739 U CN 211724739U
- Authority
- CN
- China
- Prior art keywords
- kettle
- rectifying
- tower
- tower body
- difluorotrichloroethane
- 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.)
- Active
Links
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model relates to a purification device of difluorotrichloroethane, wherein a rectifying kettle comprises a lower kettle, a liquid membrane separator and an upper kettle, a jacket is arranged outside the lower kettle, circulating cooling water with the temperature of 40-70 ℃ is introduced into the jacket, feed liquid is filled in the lower kettle, and a drain outlet is arranged at the bottom of the lower kettle; an exhaust pipe is arranged at the top of the upper kettle, a horizontal feeding spray pipe is inserted in the upper kettle, and a rectifying kettle shielding pump extracts feed liquid from the lower kettle and performs reflux circulation from the feeding spray pipe; the rectifying tower comprises a tower body, a reboiler at the bottom of the tower body and a cooler at the top of the tower body, wherein a heat exchange medium at 70-100 ℃ is filled in the reboiler, and cooling water at 20-30 ℃ is filled in the cooler; the rectifying tower shielding pump extracts feed liquid from the lower part of the rectifying kettle and flows back from the middle part of the tower body, the output end of the cooler at the top of the tower body is connected with a difluorochloroethane recovery tank, and the reboiler is connected with a difluorotrichloroethane storage tank. The device adopts the matching of the rectifying still and the rectifying tower to rectify different components at different temperatures and respectively recover, and the purity of the recovered by-products is high.
Description
Technical Field
The utility model relates to a chemical production field, concretely relates to purification device of difluorotrichloroethane.
Background
The residual liquid of the prior difluoromono-chloroethane rectifying still contains a plurality of fluoride compounds, and the fluoride compounds can be used for preparing fluorine-containing medical intermediates after being separated. However, these fluorides have disadvantages of complicated composition, difficulty in separation, and low purity of the separated product. The problems of low conversion rate, more byproducts and limited application in the later process of synthesizing the fluorine-containing medical intermediate can be caused during recycling.
Disclosure of Invention
An object of the utility model is to provide a difluoro trichloroethane purification device can effectively draw high-purity difluoro trichloroethane in difluoro monochloroethane rectifying still raffinate.
In order to achieve the above purpose, the utility model adopts the technical proposal that:
the difluorotrichloroethane purification device comprises a rectification kettle, a rectification kettle shielding pump, a rectification tower and a rectification tower shielding pump, wherein the rectification kettle comprises a lower kettle, a liquid membrane separator and an upper kettle, a jacket is arranged on the outer side of the lower kettle, circulating cooling water with the temperature of 40-70 ℃ is introduced into the jacket, feed liquid is filled in the lower kettle, and a drain outlet is formed in the bottom of the lower kettle; the top of the upper kettle is provided with an exhaust pipe, a horizontal feeding spray pipe is inserted in the upper kettle, the rectifying kettle shielding pump extracts feed liquid from the lower kettle and performs reflux circulation from the feeding spray pipe, the rectifying tower comprises a tower body, a reboiler at the bottom of the tower body and a cooler at the top of the tower body, a heat exchange medium with the temperature of 70-100 ℃ is introduced into the reboiler, and cooling water with the temperature of 20-30 ℃ is introduced into the cooler; the rectifying tower shielding pump extracts feed liquid from the lower part of the rectifying kettle and flows back from the middle part of the tower body, the output end of the cooler at the top of the tower body is connected with a difluorochloroethane recovery tank, and the reboiler is connected with a difluorotrichloroethane storage tank.
Further, the liquid membrane separator is a shell-and-tube heat exchanger, the tube side is communicated with the cavities of the upper kettle and the lower kettle, and circulating cooling water is introduced into the shell side.
Further, a distributor is arranged between the feeding spray pipe and the liquid membrane separator, and the distributor is installed in the upper kettle; the distributor comprises a circular pore plate and vertical distribution pipes arranged in each pore of the circular pore plate.
Further, the exhaust pipe is a sleeve type cooler.
After taking above technical scheme, the beneficial effects of the utility model are that: the rectification kettle is matched with the rectification tower to rectify different components at different temperatures and respectively recover, the purity of the recovered by-product is high, and the purity of the difluorotrichloroethane can reach 95%.
Drawings
FIG. 1 is a schematic diagram of the structure of a rectifying still;
FIG. 2 is a schematic view of the structure of a rectifying column.
In the figure: lower cauldron 1, liquid membrane separator 2, go up cauldron 3, canned pump 4, flange 5, drain 6, level gauge 7, press from both sides cover 8, double-pipe cooler 9, feeding spray tube 10, distributor 11, tower body 12, reboiler 13, cooler 14, rectifying column canned pump 15, difluorochloroethane holding tank 16, difluorotrichloroethane holding tank 17.
Detailed Description
The following detailed description of the embodiments of the present invention is made with reference to the accompanying drawings:
as shown in the figure, the difluorotrichloroethane purification device consists of a primary rectifying kettle and a primary rectifying tower. The device separates and extracts difluorotrichloroethane from difluoromonochloroethane rectifying still residual liquid. The main components in the residual liquid comprise difluoroethane, difluoromonochloroethane, difluorochloroethane, difluorotrichloroethane and the like.
The rectifying still is used for separating difluoromono-chloroethane and difluoroethane in residual liquid and comprises a lower still 1, a liquid membrane separator 2, an upper still 3 and a rectifying still shielding pump 4. The liquid membrane separator 2 is arranged between the upper kettle 1 and the lower kettle 3. The upper surface and the lower surface of the liquid membrane separator 2 are both flange surfaces, and are connected with the upper kettle and the lower kettle through the flanges 5 and bolts, so that subsequent disassembly and maintenance are convenient. The liquid membrane separator 2 is a shell-and-tube heat exchanger, the tube side of the liquid membrane separator 2 is communicated with the cavities of the upper kettle 1 and the lower kettle 3, and hot water with the temperature of 40-70 ℃ is introduced into the shell side of the liquid membrane separator 2. There is drain 6 bottom cauldron 1 down, and cauldron 1 side-mounting has level gauge 7 down, is convenient for monitor the inside liquid level condition. The outer side of the lower kettle 1 is provided with a jacket 8, hot water with the temperature of 40-70 ℃ is filled in the jacket 8, mixed liquid in the lower kettle 1 is heated, difluoromono-chloroethane is gasified, and the mixed liquid is sequentially recovered from the top of the upper kettle 3 through a liquid membrane separator 2 and the upper kettle 3. The top of the upper kettle 3 is provided with a vertical sleeve cooler 9, the length of the sleeve cooler 9 is 2 meters, and the inner diameter is 100-125 mm. The cooling water with the temperature of 20-30 ℃ is introduced into the sleeve cooler 9. A feeding spray pipe 10 and a distributor 11 are arranged in the upper kettle 3, and the distributor 11 is arranged in the upper kettle 3 and is positioned below the feeding spray pipe 10; the distributor 11 comprises a circular orifice plate and vertical distribution pipes mounted in each orifice of the circular orifice plate. The feeding spray pipe 10 is a horizontal pipeline, the rectifying still shielding pump 4 pumps the feed liquid in the lower kettle 1 and then sends the feed liquid to the feeding spray pipe 10, the feed liquid is sprayed out from the feeding spray pipe 10, uniformly distributed by a distributor 11 below the feed liquid and flows downwards from the tube pass of the liquid film separator 2, exchanges heat with the liquid film separator 2 and evaporates, difluoromono-chloroethane is gasified and sent upwards from the sleeve cooler 9 of the upper kettle to a lower-level condenser for recycling, and a small amount of gaseous difluorochloroethane, difluorotrichloroethane and difluorochloroethane are liquefied in the sleeve cooler 9 and flow back to the lower kettle 1. One circulation is completed, and after multiple circulations, difluoromono-chloroethane and difluoroethane in the feed liquid can be completely separated.
The rectifying tower is used for separating difluorochloroethane and difluorotrichloroethane, the rectifying tower comprises a tower body 12, a tower body bottom reboiler 13 and a cooler 14 arranged at the top of the tower body, residual liquid is extracted from the bottom of the rectifying kettle by using a rectifying tower shielding pump 15 and is sent to the middle part of the tower body 12 to be refluxed, and the components of the residual liquid sent into the rectifying tower are 65 percent of difluorochloroethane, 30 percent of difluorotrichloroethane, and 5 percent of water and other impurities. A reboiler 13 is internally filled with a heat exchange medium at 70-100 ℃, difluorotrichloroethane and a small amount of difluorotrichloroethane in the residual liquid are evaporated, a cooler 14 at the top of the tower is internally filled with cooling water at 20-30 ℃, and difluorochloroethane is liquefied and recycled into a difluorochloroethane collecting tank 16. The residual liquid at the bottom of the tower is difluorotrichloroethane with the purity of 95 percent, and is pumped into a difluorotrichloroethane collecting tank 17.
Claims (4)
1. The difluorotrichloroethane purification device comprises a rectification kettle, a rectification kettle shielding pump, a rectification tower and a rectification tower shielding pump, wherein the rectification kettle comprises a lower kettle, a liquid membrane separator and an upper kettle, a jacket is arranged on the outer side of the lower kettle, circulating cooling water with the temperature of 40-70 ℃ is introduced into the jacket, feed liquid is filled in the lower kettle, and a drain outlet is formed in the bottom of the lower kettle; an exhaust pipe is arranged at the top of the upper kettle, a horizontal feeding spray pipe is inserted in the upper kettle, and the rectifying kettle shielding pump extracts feed liquid from the lower kettle and performs reflux circulation from the feeding spray pipe; the rectifying tower is characterized by comprising a tower body, a reboiler at the bottom of the tower body and a cooler at the top of the tower body, wherein a heat exchange medium with the temperature of 70-100 ℃ is filled in the reboiler, and cooling water with the temperature of 20-30 ℃ is filled in the cooler; the rectifying tower shielding pump extracts feed liquid from the lower part of the rectifying kettle and flows back from the middle part of the tower body, the output end of the cooler at the top of the tower body is connected with a difluorochloroethane recovery tank, and the reboiler is connected with a difluorotrichloroethane storage tank.
2. The purification device of difluorotrichloroethane as claimed in claim 1, wherein the liquid membrane separator is a shell-and-tube heat exchanger, the tube side of the shell-and-tube heat exchanger is communicated with the cavities of the upper kettle and the lower kettle, and circulating cooling water is introduced into the shell side of the shell-and-tube heat exchanger.
3. The purification device of difluorotrichloroethane as claimed in claim 1, wherein a distributor is arranged between the feed nozzle and the liquid membrane separator, and the distributor is installed in the upper kettle; the distributor comprises a circular pore plate and vertical distribution pipes arranged in each pore of the circular pore plate.
4. The purification apparatus of difluorotrichloroethane as claimed in claim 1, wherein the vent line is a double pipe cooler.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922440813.3U CN211724739U (en) | 2019-12-30 | 2019-12-30 | Difluoro trichloroethane purification device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922440813.3U CN211724739U (en) | 2019-12-30 | 2019-12-30 | Difluoro trichloroethane purification device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN211724739U true CN211724739U (en) | 2020-10-23 |
Family
ID=72871994
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201922440813.3U Active CN211724739U (en) | 2019-12-30 | 2019-12-30 | Difluoro trichloroethane purification device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN211724739U (en) |
-
2019
- 2019-12-30 CN CN201922440813.3U patent/CN211724739U/en active Active
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107008026A (en) | Nickel sulfate evaporative crystallization technique | |
| CN110686529B (en) | Novel asphalt falling film cooler and liquid-receiving film forming method thereof | |
| CN105111171B (en) | Using hexahydro-phthalic acid diisobutyl ester as the technique of solvent recovery cis-butenedioic anhydride | |
| CN211724739U (en) | Difluoro trichloroethane purification device | |
| CN101891672B (en) | Separation and purification method and device for extracting and purifying piperidinol product from piperidone hydrogenation reaction solution | |
| CN108314611B (en) | Equipment and production process for preparing camphor by continuous gas phase dehydrogenation of isoborneol | |
| CN204275521U (en) | A kind of liquid ammonia gasification dry evaporator | |
| CN106554270A (en) | A kind of processing method of monoxone by-product crystalline mother solution | |
| CN211724740U (en) | Rectifying still for rectifying and purifying difluoromono-chloroethane | |
| CN106831360A (en) | A kind of continuous process for preparing β naphthyl methyl ethers | |
| CN217489790U (en) | Reflux condensing device in alkyd production | |
| CN212594079U (en) | Gas phase separation device for low-boiling-point impurities in titanium tetrachloride | |
| CN107162909B (en) | A kind of thermal coupling methods and device that vinyl acetate is refined | |
| CN207130215U (en) | A kind of system for producing middle matter washing oil | |
| CN211920891U (en) | Sulfuric acid process titanium white powder vacuum crystallization system | |
| CN203842338U (en) | Heat gradient utilization device in methanol rectification process | |
| CN208599441U (en) | A kind of equipment of NMP recycling purification | |
| CN111921219A (en) | Gas phase separation device and separation method for low-boiling-point impurities in titanium tetrachloride | |
| CN102489030A (en) | Three-tower energy-saving differential pressure alcohol distillation production system and technological process thereof | |
| CN204824676U (en) | Methyl alcohol purification system | |
| CN219185869U (en) | Rectifying column cooling system for preparing and recycling methanol by using N, N-dimethylaniline | |
| CN112546655A (en) | Deuterium-depleted water preparation device, preparation method and application | |
| CN206366208U (en) | A kind of methanol recovery device | |
| CN211585264U (en) | Etherification reaction rectification device for isoflurane | |
| CN217527498U (en) | Edulcoration system of methyl isopropyl ketone production usefulness |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |