CN216877880U - Device for preparing chloro-tertiary pentane by reactive distillation - Google Patents
Device for preparing chloro-tertiary pentane by reactive distillation Download PDFInfo
- Publication number
- CN216877880U CN216877880U CN202220220902.6U CN202220220902U CN216877880U CN 216877880 U CN216877880 U CN 216877880U CN 202220220902 U CN202220220902 U CN 202220220902U CN 216877880 U CN216877880 U CN 216877880U
- Authority
- CN
- China
- Prior art keywords
- addition
- inlet
- outlet
- tower reactor
- hydrochloric acid
- 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
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model discloses a device for preparing chloro-tertiary pentane by reactive distillation, which comprises a tower reactor, an addition reboiling device, a hydrochloric acid deep cooler, an addition phase separator, an addition salt acid tank, an addition discharge pump and an addition salt acid pump, wherein the top of the tower reactor is provided with a circulating hydrochloric acid inlet, the middle upper part of the tower reactor is provided with an isoamylene inlet, the middle lower part of the tower reactor is provided with a hydrogen chloride inlet and a reflux port, the bottom of the tower reactor is provided with a material outlet, and the middle part of the material outlet and the reflux port are connected with the addition reboiling device respectively. Isoamylene maintains a high conversion.
Description
Technical Field
The utility model relates to the technical field of chemical industry, in particular to a device for preparing chloro-tertiary pentane through reactive distillation.
Background
Chlorotentane is mainly used as an intermediate for producing pinacolone, which is a main raw material for pesticides, medicines and spices. In the existing process for preparing chloro-tertiary pentane, a hydrochloric acid addition process is generally adopted, namely quantitative isoamylene reacts with excessive hydrochloric acid at the temperature of 5 +/-2 ℃, the dripping time of the isoamylene is 2.5-3h, and the temperature is kept for 2h after the dripping is finished. The technology has the defects that the addition amount of hydrochloric acid is too large, a large amount of waste acid is generated, the post-treatment is difficult, and the environmental protection burden is large; the conversion rate of isoamylene is low, the product content is relatively low and is only 92-93 wt%, and the production process is intermittent production. The patent CN cyclic hydrochloric acid inlet 102557860 (preparation method of chloro-tert-pentane) co-produces phosphorous acid, and phosphorus trichloride is hydrolyzed to generate phosphorous acid and byproduct hydrogen chloride gas is subjected to addition reaction with isoamylene, so that the addition amount of hydrochloric acid is reduced, and continuous production can be realized. However, the phosphorus trichloride raw material is safe to transport and store , and the phosphorous acid production device needs additional investment. Therefore, a production device which is safe, efficient and low in cost is imperative.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a device for preparing chloro-tertiary pentane through reactive distillation, which overcomes the defects in the prior art.
In order to achieve the purpose, the utility model provides the following technical scheme:
the utility model discloses a device for preparing chloro-tertiary pentane through reaction rectification, which comprises a tower reactor, an addition reboiling device, a hydrochloric acid deep cooler, an addition phase separator, an addition salt acid tank, an addition discharge pump and an addition salt acid pump, wherein the top of the tower reactor is provided with a circulating hydrochloric acid inlet, the middle upper part of the tower reactor is provided with an isoamylene inlet, the middle lower part of the tower reactor is provided with a hydrogen chloride inlet and a reflux port, the bottom of the tower reactor is provided with a material outlet, the middle part of the material outlet and the reflux port is connected with the addition reboiling device, the material outlet is connected with the inlet of the addition discharge pump, the top of the addition phase separator is provided with the material inlet, the upper part of the tower reactor is provided with a chloro-tertiary pentane outlet, the bottom of the tower reactor is provided with a hydrochloric acid outlet, the outlet of the addition discharge pump is connected with the material inlet, the hydrochloric acid outlet is connected with the inlet of the addition salt acid tank, the outlet of the addition salt acid pump is connected with the inlet of the addition salt acid pump, and the outlet of the addition hydrochloric acid pump is connected with the inlet of the circulating hydrochloric acid after passing through the hydrochloric acid deep cooler.
Optionally, the top of the tower reactor is also provided with a hydrogen chloride tail gas outlet.
Optionally, the addition reboiler is provided with a hot water inlet and a hot water outlet, and the hot water inlet and the hot water outlet are both connected with a hot water tank.
Optionally, the hydrochloric acid deep cooler is provided with a chilled water inlet and a chilled water outlet.
Optionally, a temperature display is arranged on a tower kettle at the bottom of the tower reactor.
Optionally, the inlets of the addition discharge pump and the addition salt acid pump are both provided with control valves.
Optionally, the tower body of the tower reactor comprises a packed tower, a bubble cap tower, a sieve plate tower and a vertical sieve plate tower.
The utility model has the beneficial effects that: the utility model relates to a device for preparing chloro-tert-pentane by reactive distillation, which adopts a reactive distillation coupling technology to realize continuous production, namely, isoamylene, hydrogen chloride and hydrochloric acid are subjected to chemical (addition reaction) reaction at the middle upper part of a tower, a chlorinated solution after reaction at a tower kettle is heated to a temperature higher than 20 ℃ of the boiling point of the isoamylene by a reboiler, the unreacted isoamylene can be evaporated and then returned to the reaction tower, and the isoamylene keeps high conversion rate. The reacted materials are injected into a phase separator for layering, so that the content of the chloro-tert-pentane generated by the reaction is obviously increased to over 99wt% from 92-93 wt% of the intermittent reaction, and in addition, the cyclic hydrochloric acid is added to adjust the reaction temperature in the tower, so that the safety of an addition system is guaranteed; the hydrochloric acid is recycled in addition reaction, so that the generation amount of waste hydrochloric acid is greatly reduced, namely the hydrochloric acid amount in the integral pinacolone production is reduced by 50%; the hydrogen chloride gas is generated by analyzing waste hydrochloric acid generated by condensation reaction, and a clean production process that waste acid is not discharged is achieved.
The features and advantages of the present invention will be described in detail by embodiments in conjunction with the accompanying drawings.
Drawings
FIG. 1 is a schematic structural diagram of an embodiment of the present invention;
in the figure: the device comprises a tower reactor 10, a hydrogen chloride tail gas outlet 101, a circulating hydrochloric acid inlet 102, an isoamylene inlet 103, a hydrogen chloride inlet 104, a reflux port 105, an addition reboiling device 11, a hydrochloric acid deep cooler 12, an addition phase separator 13, a material inlet 131, a chlorinated tertiary pentane outlet 132, a hydrochloric acid outlet 133, an addition salt acid tank 14, an addition discharge pump 15 and an addition salt acid pump 16.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings and examples. It should be understood, however, that the description herein of specific embodiments is only intended to illustrate the utility model and not to limit the scope of the utility model. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
Referring to fig. 1, an embodiment of the present invention provides a device for preparing chloro-trimethylpentane by reactive distillation, including a tower reactor 10, an addition reboiler 11, a hydrochloric acid chiller 12, an addition phase separator 13, an addition salt acid tank 14, an addition discharge pump 15, and an addition salt acid pump 16, wherein a hydrogen chloride tail gas outlet 101 and a circulating hydrochloric acid inlet 102 are arranged at the top of the tower reactor 10, an isoamylene inlet 103 is arranged at the middle upper portion, a hydrogen chloride inlet 104 and a reflux port 105 are arranged at the middle lower portion, a material outlet 106 is arranged at the bottom, the addition reboiler 11 is connected between the material outlet 106 and the reflux port 105, the material outlet 106 is connected with the inlet of the addition discharge pump 15, a material inlet 131 is arranged at the top of the addition phase separator 13, a chloro-trimethylpentane outlet 132 is arranged at the upper portion, a hydrochloric acid outlet 133 is arranged at the bottom, the outlet of the addition discharge pump 15 is connected with the material inlet 131, the hydrochloric acid outlet 133 is connected with the inlet of the addition salt acid tank 14, the outlet of the addition salt acid tank 14 is connected with the inlet of the addition salt acid pump 16, and the outlet of the addition salt acid pump 16 passes through the hydrochloric acid deep cooler 12 and then is connected with the circulating hydrochloric acid inlet 102.
And the addition reboiler 11 is provided with a hot water inlet and a hot water outlet which are both connected with a hot water tank.
And a chilled water inlet and a chilled water outlet are formed in the hydrochloric acid deep cooler 12.
And a temperature display is arranged on the tower kettle at the bottom of the tower reactor 10.
The inlets of the addition discharge pump 15 and the addition salt acid pump 16 are both provided with control valves.
The tower body of the tower reactor 10 comprises a packed tower, a bubble cap tower, a sieve plate tower and a vertical sieve plate tower, and the material of the packing in the packed tower comprises ceramics, PVDF, PTFE, PE and graphite.
The working process of the utility model is as follows:
in the working process of the device for preparing chloro-tertiary-pentane by reactive distillation, isoamylene enters a tower reactor 10 through an isoamylene inlet 103 at the middle upper part of the tower reactor 10, hydrogen chloride gas from a hydrochloric acid analysis process enters the middle lower part of the tower reactor 10 through a hydrogen chloride inlet 104, circulating hydrochloric acid in an addition salt acid tank 14 is pumped out by an addition salt acid pump 16, the hydrogen chloride gas is cooled by a hydrochloric acid deep cooler 12 and then enters the top of the tower reactor 10 through a circulating hydrochloric acid inlet 102, addition reaction is carried out in the tower reactor 10, an addition liquid enters a tower kettle at the bottom of the tower, a material flows through an addition reboiling device 11 from a material outlet 106 and then returns to the tower kettle through a reflux opening 105, the material is heated by hot water in the addition reboiling device 11 and the temperature is controlled to enter the tower kettle, a temperature display on the tower kettle displays the material temperature, the chlorinated liquid in the tower kettle is heated to be more than 20 ℃ higher than the boiling point of the isoamylene by the addition reboiling device 11, unreacted isoamylene can be evaporated and then returned to the reaction tower, materials are pumped into an addition phase separator 13 for layering through an addition discharging pump 15 after the isoamylene is evaporated, heavy-phase hydrochloric acid enters an addition salt acid tank 14 through a hydrochloric acid outlet 133 at the bottom, and light-phase chloro-tert-pentane in the phase separator enters a condensation reaction process through a chloro-tert-pentane outlet 132 at the upper part.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the utility model, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (6)
1. A device for preparing chloro-tertiary pentane by reactive distillation is characterized in that: the device comprises a tower reactor (10), an addition reboiling device (11), a hydrochloric acid deep cooler (12), an addition phase splitter (13), an addition salt acid tank (14), an addition discharging pump (15) and an addition salt acid pump (16), wherein the top of the tower reactor (10) is provided with a circulating hydrochloric acid inlet (102), the middle upper part of the tower reactor is provided with an isoamylene inlet (103), the middle lower part of the tower reactor is provided with a hydrogen chloride inlet (104) and a reflux port (105), the bottom of the tower reactor is provided with a material outlet (106), the material outlet (106) and the middle of the reflux port (105) are connected with the addition reboiling device (11), the material outlet (106) is connected with the inlet of the addition discharging pump (15), the top of the addition phase splitter (13) is provided with a material inlet (131), the upper part of the addition phase splitter is provided with a chlorinated special pentane outlet (132), the bottom of the tower reactor is provided with a hydrochloric acid outlet (133), the outlet of the addition discharging pump (15) is connected with the material inlet (131), the hydrochloric acid outlet (133) is connected with the inlet of the addition salt acid tank (14), the outlet of the addition salt acid tank (14) is connected with the inlet of the addition salt acid pump (16), and the outlet of the addition salt acid pump (16) passes through the hydrochloric acid deep cooler (12) and then is connected with the circulating hydrochloric acid inlet (102).
2. The apparatus for preparing chloro-tert-pentane by reactive distillation according to claim 1, wherein: the top of the tower reactor (10) is also provided with a hydrogen chloride tail gas outlet (101).
3. The apparatus for preparing chloro-tert-pentane by reactive distillation according to claim 1, wherein: the addition reboiling device (11) is provided with a hot water inlet and a hot water outlet which are both connected with a hot water tank.
4. The apparatus for preparing chloro-tert-pentane by reactive distillation according to claim 1, wherein: and a chilled water inlet and a chilled water outlet are arranged on the hydrochloric acid deep cooler (12).
5. The apparatus for preparing chloro-tert-pentane by reactive distillation according to claim 1, wherein: and a temperature display is arranged on a tower kettle at the bottom of the tower reactor (10).
6. The apparatus for preparing chloro-tert-pentane by reactive distillation according to claim 1, wherein: and control valves are arranged at the inlets of the addition discharge pump (15) and the addition salt acid pump (16).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220220902.6U CN216877880U (en) | 2022-01-27 | 2022-01-27 | Device for preparing chloro-tertiary pentane by reactive distillation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220220902.6U CN216877880U (en) | 2022-01-27 | 2022-01-27 | Device for preparing chloro-tertiary pentane by reactive distillation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN216877880U true CN216877880U (en) | 2022-07-05 |
Family
ID=82182703
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202220220902.6U Active CN216877880U (en) | 2022-01-27 | 2022-01-27 | Device for preparing chloro-tertiary pentane by reactive distillation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN216877880U (en) |
-
2022
- 2022-01-27 CN CN202220220902.6U patent/CN216877880U/en active Active
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101747298B (en) | Process for preparing high-purity diketene | |
| CN107089922B (en) | The production technology of glycine side product sodium chloride | |
| CN102408396B (en) | Method for preparing versatate glycidyl | |
| CN101353289B (en) | Method for extracting trans-dichloroethylene from low-boiling residue of ethinyltrichloride production by gas-phase catalytic process | |
| CN216877880U (en) | Device for preparing chloro-tertiary pentane by reactive distillation | |
| CN103524478B (en) | Device and method for shortening ketalation time in ibuprofen synthesis process | |
| CN109651067A (en) | A kind of preparation process of 1,1,2- trichloroethanes | |
| US20240174628A1 (en) | Method for continuously preparing crude ethylene sulfate | |
| CN102502566A (en) | Technology for synthesizing lithium hexafluorophosphate | |
| CN211256109U (en) | Tetraethyl ammonium hydroxide preparation device | |
| CN106220491B (en) | Production of chloroacetic acid method | |
| CN115784181A (en) | Continuous reaction rectification preparation system of phosphorus pentafluoride and preparation thereof | |
| CN202379748U (en) | Reverse disproportionation reaction device for preparing trichlorosilane | |
| CN108658756A (en) | A kind of method that the dechlorination of trichloroacetic acid selectivity prepares dichloroacetic acid | |
| CN205099353U (en) | Defluorinate equipment of hydrochloric acid in fluorochlorohydrocarbon production technology | |
| CN101805248B (en) | Method for continuously synthesizing trichloracetic aldehyde and device thereof | |
| CN106478402A (en) | The method that ethanol acid crystal is prepared by methyl glycollate | |
| CN201850135U (en) | Hydrogen chloride gas drying device | |
| CN106748628B (en) | A kind of method that low temperature continuous chlorination prepares mixed-chlorotoluene | |
| CN1075298A (en) | A kind of method of producing chlorine dioxide of high concentration and stable state | |
| CN114195675B (en) | Method for preparing ethyl hydrazine by continuous flow of microreactor | |
| CN103936548B (en) | A kind of method of 1,2-ethylene dichloride chlorination production vinyl trichloride | |
| CN105036137B (en) | Method for preparing silane by disproportionation of dichlorosilane as raw material | |
| CN102795982B (en) | Method and device for industrially producing benzoylbenzene by carbon tetrachloride process | |
| CN220514169U (en) | Dichloropropanol apparatus for producing |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |