CN220386510U - Device for continuously producing sodium tert-butoxide - Google Patents
Device for continuously producing sodium tert-butoxide Download PDFInfo
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- CN220386510U CN220386510U CN202321802114.9U CN202321802114U CN220386510U CN 220386510 U CN220386510 U CN 220386510U CN 202321802114 U CN202321802114 U CN 202321802114U CN 220386510 U CN220386510 U CN 220386510U
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- kettle
- reaction kettle
- stage
- stage reaction
- absorption tower
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- MFRIHAYPQRLWNB-UHFFFAOYSA-N sodium tert-butoxide Chemical compound [Na+].CC(C)(C)[O-] MFRIHAYPQRLWNB-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000006243 chemical reaction Methods 0.000 claims abstract description 81
- 238000010521 absorption reaction Methods 0.000 claims abstract description 32
- 239000007791 liquid phase Substances 0.000 claims abstract description 29
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 24
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000002425 crystallisation Methods 0.000 claims abstract description 18
- 230000008025 crystallization Effects 0.000 claims abstract description 18
- 239000012071 phase Substances 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000010992 reflux Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 24
- 238000009833 condensation Methods 0.000 claims description 8
- 230000005494 condensation Effects 0.000 claims description 8
- 239000007792 gaseous phase Substances 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 239000002904 solvent Substances 0.000 abstract description 17
- 238000000034 method Methods 0.000 abstract description 14
- 238000002156 mixing Methods 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 7
- ODZPKZBBUMBTMG-UHFFFAOYSA-N sodium amide Chemical compound [NH2-].[Na+] ODZPKZBBUMBTMG-UHFFFAOYSA-N 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 5
- 230000002411 adverse Effects 0.000 abstract description 2
- 239000000109 continuous material Substances 0.000 abstract description 2
- 208000012839 conversion disease Diseases 0.000 abstract description 2
- 238000007599 discharging Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000012847 fine chemical Substances 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 9
- 239000007788 liquid Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000006096 absorbing agent Substances 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- SYXYWTXQFUUWLP-UHFFFAOYSA-N sodium;butan-1-olate Chemical group [Na+].CCCC[O-] SYXYWTXQFUUWLP-UHFFFAOYSA-N 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- -1 medical Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model belongs to the technical field of fine chemical industry, and discloses a device for continuously producing sodium tert-butoxide, which comprises a batching kettle, a tertiary butanol tank, a first-stage reaction kettle, a second-stage reaction kettle, a third-stage reaction kettle, a deep cooler, a first-stage absorption tower, a second-stage absorption tower, a desolventizing crystallization kettle, a condenser, a normal hexane tank and a drying unit, wherein a liquid phase outlet of the batching kettle is connected to the first-stage reaction kettle, and the utility model also discloses a process method for continuously producing sodium tert-butoxide, which comprises the following steps: A. the raw material sodium amide is uniformly dispersed in the solvent and is conveyed into the first-stage reaction kettle, and the adverse effect of back mixing on the reaction conversion rate and the yield is reduced while continuous material feeding and discharging is realized by arranging the three-stage serial reaction kettle; the reaction kettle is provided with a condensing reflux device which is used for condensing the reaction materials and the solvent carried along with the gas phase, reducing the loss of the reaction materials and the solvent and improving the reaction yield.
Description
Technical Field
The utility model belongs to the technical field of fine chemical industry, and particularly relates to a device for continuously producing sodium tert-butoxide.
Background
The sodium tert-butoxide is white powder in appearance, has a molecular formula of C4H9ONa, a molecular weight of 96.10 and a melting point of 180 ℃, is an important organic strong base, and is widely applied to chemical, medical, pesticide, organic synthesis and other reactions. The demand is increasing due to the large number of application fields. Conventional methods of synthesizing sodium tert-butoxide include a metal method and an alkali method. The metal method directly reacts with tert-butyl alcohol and sodium metal, and the method has the defects of long reaction time and low yield, and increases the production risk because hydrogen is generated in the reaction. The alkaline method uses tertiary butanol and sodium hydroxide to react, but has the problems of low reaction rate, low yield, high consumption, high pollution and the like. And the batch process is mainly adopted in the industry at present, and the following defects are common: the single set of device has low yield and large equipment investment; (2) Long reaction time, high energy consumption and unstable product quality; (3) The production environment is poor, the running and leaking are serious in the production process, and the environment is polluted.
Disclosure of Invention
The utility model aims to provide a device for continuously producing sodium tert-butoxide, which aims to solve the problems in the background technology.
In order to achieve the above purpose, the present utility model provides the following technical solutions: a device for continuously producing sodium tert-butoxide comprises a batching kettle, a tert-butanol tank, a first-stage reaction kettle, a second-stage reaction kettle, a third-stage reaction kettle, a deep cooler, a first-stage absorption tower, a second-stage absorption tower, a desolventizing crystallization kettle, a condenser, an n-hexane tank and a drying unit;
the liquid phase outlet of the batching kettle is connected to a first-stage reaction kettle, the liquid phase outlet of the tertiary butanol tank is respectively connected with the first-stage reaction kettle, a second-stage reaction kettle and a third-stage reaction kettle, the liquid phase outlet of the third-stage reaction kettle is connected to a desolventizing crystallization kettle, the gas phase outlets of the first-stage reaction kettle, the second-stage reaction kettle and the third-stage reaction kettle are converged and then connected to a refrigerator, the liquid phase outlet of the refrigerator is connected to a n-hexane tank, the gas phase outlet of the refrigerator is connected to a first-stage absorption tower, the gas phase outlet of the first-stage absorption tower is connected to a second-stage absorption tower, the liquid phase outlet of the second-stage absorption tower is connected to the top of the first-stage absorption tower, the bottom outlet of the desolventizing crystallization kettle is connected to a drying unit, the gas phase outlet of the desolventizing crystallization kettle is connected to a condenser, the liquid phase outlet of the condenser is connected to the n-hexane tank, and the liquid phase outlet of the n-hexane tank is connected to the batching kettle.
Preferably, all be provided with the condensation backward flow ware on first level reation kettle, second level reation kettle, the third level reation kettle, just the condensation backward flow ware top sets up the gaseous phase export, the inside of first level reation kettle, second level reation kettle, third level reation kettle all is equipped with the rotatory stirring subassembly of motor drive, the stirring subassembly includes the (mixing) shaft and installs the puddler in the (mixing) shaft bottom.
Preferably, the batching cauldron bottom is the cone angle form, just inside motor drive rotatory stirring subassembly that is equipped with of batching cauldron, stirring subassembly includes the (mixing) shaft and installs the puddler on the (mixing) shaft, the puddler is echelonment, just the puddler increases in proper order from down to last length.
Preferably, flow regulating valves are arranged on the liquid phase outlet of the batching kettle and the liquid phase outlet pipeline of the tertiary butanol tank.
Compared with the prior art, the utility model has the beneficial effects that:
(1) According to the utility model, by arranging the three-stage serial reaction kettles, the adverse effect of back mixing on the reaction conversion rate and yield is reduced while continuous material feeding and discharging is realized; the reaction kettle is provided with a condensing reflux device which is used for condensing the reaction materials and the solvent carried along with the gas phase, reducing the loss of the reaction materials and the solvent and improving the reaction yield;
(2) According to the utility model, the gas phase outlet of the reaction kettle is connected with the cryocooler, so that the organic materials which are not condensed in the gas phase are further condensed, the organic materials are prevented from entering the absorption tower, and the product quality of ammonia water is improved;
(3) The bottom of the batching kettle is cone-angle-shaped, and a motor-driven rotary stirring assembly is arranged in the batching kettle to prevent solid materials from depositing;
(4) And flow regulating valves are arranged on liquid phase outlets of the batching kettle and liquid phase outlet pipelines of the tertiary butanol tank, so that the feeding proportion is controlled, the material loss is reduced, and the reaction efficiency is improved.
Drawings
FIG. 1 is a schematic diagram of the structure of the present utility model;
in the figure: 1. a batching kettle; 2. a tertiary butanol tank; 3. a first-stage reaction kettle; 4. a second-stage reaction kettle; 5. a third-stage reaction kettle; 6. a chiller; 7. a first stage absorber; 8. a second-stage absorption column; 9. a desolventizing crystallization kettle; 10. a condenser; 11. a n-hexane tank; 12. and a drying unit.
Detailed Description
The following description of the embodiments of the present utility model will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present utility model, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
Referring to fig. 1, the present utility model provides the following technical solutions:
a device for continuously producing sodium tert-butoxide comprises a batching kettle 1, a tert-butanol tank 2, a first-stage reaction kettle 3, a second-stage reaction kettle 4, a third-stage reaction kettle 5, a deep cooler 6, a first-stage absorption tower 7, a second-stage absorption tower 8, a desolventizing crystallization kettle 9, a condenser 10, a normal hexane tank 11 and a drying unit 12;
the liquid phase outlet of the batching kettle 1 is connected to the first-stage reaction kettle 3, the liquid phase outlet of the tertiary butanol tank 2 is respectively connected with the first-stage reaction kettle 3, the second-stage reaction kettle 4 and the third-stage reaction kettle 5, the liquid phase outlet of the third-stage reaction kettle 5 is connected to a desolventizing crystallization kettle 9, the gas phase outlets of the first-stage reaction kettle 3, the second-stage reaction kettle 4 and the third-stage reaction kettle 5 are converged and then are connected to a refrigerator 6, the liquid phase outlet of the refrigerator 6 is connected to a normal hexane tank 11, the gas phase outlet of the refrigerator 6 is connected to a first-stage absorption tower 7, the gas phase outlet of the first-stage absorption tower 7 is connected to a second-stage absorption tower 8, the bottom liquid phase outlet of the second-stage absorption tower 8 is connected to the top of the first-stage absorption tower 7, the bottom outlet of the desolventizing crystallization kettle 9 is connected to a drying unit 12, the gas phase outlet of the desolventizing crystallization kettle 9 is connected to a condenser 10, the liquid phase outlet of the condenser 10 is connected to the normal hexane tank 11, and the liquid phase outlet of the normal hexane tank 11 is connected to the batching kettle 1.
In addition, in the utility model, the first-stage reaction kettle 3, the second-stage reaction kettle 4 and the third-stage reaction kettle 5 are respectively provided with a condensation reflux device, the top of the condensation reflux device is provided with a gas phase outlet, and the inside of the first-stage reaction kettle 3, the second-stage reaction kettle 4 and the third-stage reaction kettle 5 is respectively provided with a stirring component driven by a motor to rotate, and the stirring components comprise a stirring shaft and a stirring rod arranged at the bottom of the stirring shaft.
Preferably, the batching cauldron 1 bottom is the cone angle form, and batching cauldron 1 inside is equipped with the rotatory stirring subassembly of motor drive, and the stirring subassembly includes the (mixing) shaft and installs the puddler on the (mixing) shaft, and the puddler is echelonment, and the puddler increases in proper order from down to last length.
Further, flow regulating valves are arranged on the liquid phase outlet of the batching kettle 1 and the liquid phase outlet pipeline of the tertiary butanol tank 2.
In addition, regarding the process for continuously producing sodium tert-butoxide, the following embodiments are provided in the present utility model:
embodiment one
A process method for continuously producing sodium tert-butoxide comprises the following steps:
A. n-hexane is used as a solvent, sodium amide serving as a raw material is uniformly dispersed in the solvent, is conveyed into a first-stage reaction kettle 3, the liquid level of the first-stage reaction kettle 3 is controlled, and materials are sequentially conveyed into a second-stage reaction kettle 4 and a third-stage reaction kettle 5 through liquid level difference;
B. raw material tertiary butanol is respectively added into a first-stage reaction kettle 3, a second-stage reaction kettle 4 and a third-stage reaction kettle 5 according to a proportion, and is subjected to substitution reaction with sodium amide at the temperature of 40-68 ℃, and tertiary butanol is added into the first-stage reaction kettle 3, the second-stage reaction kettle 4 and the third-stage reaction kettle 5 according to a proportion of 4-6:2-4:1-3 to generate sodium tertiary butoxide and ammonia;
C. the ammonia gas containing trace solvent is discharged through gas phase outlets of a first-stage reaction kettle 3, a second-stage reaction kettle 4 and a third-stage reaction kettle 5, and is conveyed into a first-stage absorption tower 7 and a second-stage absorption tower 8 for treatment after the solvent is recovered by condensation of a cryocooler 6;
D. the process water is used as an absorbent to be conveyed into a second-stage absorption tower 8, ammonia gas is absorbed in countercurrent through the first-stage absorption tower 7 and the second-stage absorption tower 8 to generate ammonia water with the concentration of 10% -25% as a byproduct;
E. the tertiary sodium butoxide solution generated by the reaction enters a desolventizing crystallization kettle 9 to remove the solvent;
F. the sodium tert-butoxide after solvent removal enters a drying section and is dried to obtain a sodium tert-butoxide product;
g: the gas phase of the desolventizing crystallization kettle 9 is condensed and recovered and then is used as a solvent for recycling.
Second embodiment
A process method for continuously producing sodium tert-butoxide comprises the following steps:
A. uniformly dispersing sodium amide serving as a raw material in n-hexane, conveying the sodium amide into a first-stage reaction kettle, controlling the liquid level of the reaction kettle, and sequentially conveying materials into a second-stage reaction kettle and a third-stage reaction kettle through liquid level difference;
B. raw material tertiary butanol is respectively added into each level of reaction kettle according to the proportion of 5:3:2 to carry out displacement reaction with sodium amide at 50 ℃ to generate sodium tertiary butoxide and ammonia;
C. the ammonia gas at the gas phase outlet of the reaction kettle contains a trace amount of solvent, and after the solvent is recovered by cryogenic condensation, the ammonia gas is sent to an absorption tower;
D. the absorber is process water, ammonia gas is subjected to two-stage countercurrent absorption to generate 25% ammonia water as a byproduct;
E. the tertiary sodium butoxide solution generated by the reaction enters a desolventizing crystallization kettle to remove the solvent;
F. the sodium tert-butoxide after the solvent is removed enters a drying working section, and a sodium tert-butoxide product is obtained after drying, wherein the yield is 98.6% and the purity is 99.2%;
g: the gas phase of the desolventizing crystallization kettle is recycled as a solvent after being condensed and recovered.
Although embodiments of the present utility model have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the utility model, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. A device for continuously producing sodium tert-butoxide, which is characterized in that: comprises a batching kettle (1), a tertiary butanol tank (2), a first-stage reaction kettle (3), a second-stage reaction kettle (4), a third-stage reaction kettle (5), a deep cooler (6), a first-stage absorption tower (7), a second-stage absorption tower (8), a desolventizing crystallization kettle (9), a condenser (10), a normal hexane tank (11) and a drying unit (12);
the batching cauldron (1) liquid phase exit linkage is to first level reation kettle (3), tertiary butanol jar (2) liquid phase export is connected with first level reation kettle (3), second level reation kettle (4) and tertiary reation kettle (5) respectively, tertiary reation kettle (5) liquid phase exit linkage is to desolventizing crystallization kettle (9), be connected to refrigerator (6) after the gaseous phase export of first level reation kettle (3), second level reation kettle (4) and tertiary reation kettle (5) meet, the liquid phase export of refrigerator (6) is connected to normal hexane jar (11), the gaseous phase export of refrigerator (6) is connected to first level absorption tower (7), the gaseous phase export of first level absorption tower (7) is connected to second level absorption tower (8), second level absorption tower (8) bottom liquid phase export is connected to first level absorption tower (7) top, desolventizing crystallization kettle (9) bottom exit linkage is to drying unit (12), the gaseous phase export of desolventizing crystallization kettle (9) is connected to condenser (10), the liquid phase export of condenser (10) is connected to normal hexane jar (11), normal hexane jar (11) is connected to the export of normal hexane (11).
2. The device for continuously producing sodium tert-butoxide according to claim 1, wherein the first-stage reaction kettle (3), the second-stage reaction kettle (4) and the third-stage reaction kettle (5) are respectively provided with a condensation reflux device, the top of the condensation reflux device is provided with a gas-phase outlet, and the inside of the first-stage reaction kettle (3), the second-stage reaction kettle (4) and the third-stage reaction kettle (5) is respectively provided with a motor-driven rotary stirring assembly, and the stirring assembly comprises a stirring shaft and a stirring rod arranged at the bottom of the stirring shaft.
3. The device for continuously producing sodium tert-butoxide according to claim 1, wherein the bottom of the batching kettle (1) is cone-angle-shaped, and a stirring assembly driven by a motor to rotate is arranged in the batching kettle (1), the stirring assembly comprises a stirring shaft and a stirring rod arranged on the stirring shaft, the stirring rod is in a ladder shape, and the length of the stirring rod is sequentially increased from bottom to top.
4. The device for continuously producing the sodium tert-butoxide according to claim 1, wherein flow regulating valves are arranged on a liquid phase outlet of the batching kettle (1) and a liquid phase outlet pipeline of the tert-butanol tank (2).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321802114.9U CN220386510U (en) | 2023-07-11 | 2023-07-11 | Device for continuously producing sodium tert-butoxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321802114.9U CN220386510U (en) | 2023-07-11 | 2023-07-11 | Device for continuously producing sodium tert-butoxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN220386510U true CN220386510U (en) | 2024-01-26 |
Family
ID=89606409
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202321802114.9U Active CN220386510U (en) | 2023-07-11 | 2023-07-11 | Device for continuously producing sodium tert-butoxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN220386510U (en) |
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2023
- 2023-07-11 CN CN202321802114.9U patent/CN220386510U/en active Active
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