CN105597354B - Nitromethane reduced pressure distillation system - Google Patents
Nitromethane reduced pressure distillation system Download PDFInfo
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- CN105597354B CN105597354B CN201510786822.1A CN201510786822A CN105597354B CN 105597354 B CN105597354 B CN 105597354B CN 201510786822 A CN201510786822 A CN 201510786822A CN 105597354 B CN105597354 B CN 105597354B
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- 238000004821 distillation Methods 0.000 title claims abstract description 101
- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical compound C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 239000007788 liquid Substances 0.000 claims abstract description 76
- 239000000126 substance Substances 0.000 claims abstract description 69
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 61
- 238000000926 separation method Methods 0.000 claims abstract description 39
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 29
- 238000012432 intermediate storage Methods 0.000 claims abstract description 9
- 238000003860 storage Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 238000003786 synthesis reaction Methods 0.000 claims description 19
- 230000015572 biosynthetic process Effects 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 16
- 238000005086 pumping Methods 0.000 claims description 15
- 238000009835 boiling Methods 0.000 claims description 11
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 9
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 4
- 238000005352 clarification Methods 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 claims description 2
- 238000005292 vacuum distillation Methods 0.000 claims 6
- 238000000746 purification Methods 0.000 abstract description 18
- 230000000694 effects Effects 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 2
- 238000004134 energy conservation Methods 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000000034 method Methods 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- LFHISGNCFUNFFM-UHFFFAOYSA-N chloropicrin Chemical compound [O-][N+](=O)C(Cl)(Cl)Cl LFHISGNCFUNFFM-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000003254 gasoline additive Substances 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- JTJMJGYZQZDUJJ-UHFFFAOYSA-N phencyclidine Chemical compound C1CCCCN1C1(C=2C=CC=CC=2)CCCCC1 JTJMJGYZQZDUJJ-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002760 rocket fuel Substances 0.000 description 1
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Abstract
The invention relates to a nitromethane reduced pressure distillation system, and belongs to the technical field of nitromethane purification. The nitromethane reduced pressure distillation system comprises a crude nitromethane intermediate storage tank, a distillation kettle, a condenser, a finished product receiving tank and a vacuum unit, wherein the condenser comprises a kettle top condenser and a finished product condenser; the three-way valve is connected with a liquid separation bottle, the liquid separation bottle is respectively connected with the distillation kettle and the low-boiling-point substance receiving tank, and a section of pipeline connecting the liquid separation bottle and the distillation kettle is set as a U-shaped pipe; the finished product condenser, the liquid separating bottle, the low-boiling-point substance receiving tank and the finished product receiving tank are respectively connected with the vacuum unit; the low-boiling-point substance receiving tank and the finished product receiving tank are also respectively connected with the nitrogen storage tank. The invention has the advantages of scientific and reasonable design, low operation cost, safety, energy conservation, environmental protection, high purification efficiency and good purification effect, and fully utilizes impurities generated in the purification.
Description
Technical Field
The invention relates to a nitromethane reduced pressure distillation system, and belongs to the technical field of nitromethane purification.
Background
Nitromethane is colorless oily liquid, is dissolved in ethanol, diethyl ether and dimethylformamide, and is partially dissolved in water. It can be used for organic synthesis of chloropicrin, nitroalcohol, explosive, rocket fuel, medicine, dye, insecticide and gasoline additive, and can also be used as organic solvent.
Nitromethane is an important chemical raw material, the purification of the nitromethane is very important, and the nitromethane is generally industrially prepared by an atmospheric distillation method. However, there are several problems: (1) the boiling point of nitromethane is 101.2 ℃ under normal pressure, and when the distillation kettle needs to be heated to about 103 ℃, the nitromethane can be evaporated out in large quantity, so that the energy consumption is serious; (2) the flash point of the nitromethane is very low and is only 35 ℃, and high-temperature steam is used for normal-pressure distillation, so that great potential safety hazard exists; (3) the existing normal pressure distillation purification device has poor purification efficiency, for example, a 5000L distillation kettle distills 99.9% of nitromethane, and the normal pressure distillation needs 45-55 hours and takes a long time; (4) the normal pressure distillation purification device has poor purification effect, can not meet the requirements of customers, and does not recycle low-boiling-point substances and high-boiling-point substances generated in the purification. Therefore, a purification system which is safe, energy-saving and can fully purify raw materials is urgently needed to be developed.
Disclosure of Invention
The invention aims to provide a nitromethane reduced pressure distillation system which is scientific and reasonable in design, low in operation cost, safe, energy-saving, environment-friendly, high in purification efficiency and good in purification effect, and impurities generated in purification are fully utilized.
The nitromethane reduced pressure distillation system comprises a crude nitromethane intermediate storage tank, a distillation kettle, a condenser, a finished product receiving tank and a vacuum unit, wherein the condenser comprises a kettle top condenser and a finished product condenser; the three-way valve is connected with a liquid separation bottle, the liquid separation bottle is respectively connected with the distillation kettle and the low-boiling-point substance receiving tank, and a section of pipeline connecting the liquid separation bottle and the distillation kettle is set as a U-shaped pipe; the finished product condenser, the liquid separating bottle, the low-boiling-point substance receiving tank and the finished product receiving tank are respectively connected with the vacuum unit; the low-boiling-point substance receiving tank and the finished product receiving tank are also respectively connected with the nitrogen storage tank.
The distillation still is of a jacket type structure, and the inside of the jacket is connected with a hot water circulating system.
The distillation still is also connected with a liquid level alarm interlocking device, and when the liquid level in the distillation still reaches an upper limit value (for example, alarming at 4000L and interlocking closing at 4500L) and a lower limit value (for example, alarming at 500L and interlocking closing at 350L after distillation is finished), the liquid level alarm interlocking device is automatically started.
And a thermometer is arranged on a pipeline above the condenser at the top of the kettle.
The height of the U-shaped tube is 0.8-1.2m, preferably 1 m. The U-shaped pipe is used as a liquid sealing device, and nitromethane in the pipeline of the U-shaped pipe is used as a liquid sealing medium, so that gas in the distillation kettle is prevented from entering the liquid separation bottle through the U-shaped pipe.
The bottom of the distillation kettle is connected with a high-boiling-point substance receiving tank, and the high-boiling-point substance receiving tank is respectively connected with a vacuum unit and a nitrogen storage tank.
The atmospheric valve is established in the top of jar body top gas exit to establish and take out the vacuum valve and advance nitrogen gas valve below, the jar body is including low thing receiving tank, high thing receiving tank and the finished product receiving tank of boiling.
The high-boiling-point substance receiving tank is also connected with a nitromethane synthesis device, so that the high-boiling-point substance is recycled.
The low-boiling-point substance receiving tank is also connected with a nitromethane synthesis device, so that the reutilization of the low-boiling-point substances is realized.
And the finished product receiving tank is connected with a hydroxylamine hydrochloride synthesis device or a nitromethane filling device.
And a guide plate is arranged in the lower seal head of the finished product condenser.
The vacuum unit is connected with the tail gas absorption tower.
When the nitromethane is subjected to reduced pressure distillation, a kettle top condenser and a finished product condenser are checked, and circulating water is started. And checking and opening a vacuum valve on a finished product condenser end socket and a vacuum valve on a liquid separation bottle, starting a vacuum unit for vacuumizing, automatically controlling the crude nitromethane in a crude nitromethane intermediate storage tank through a central control room, pumping the crude nitromethane into each distillation kettle to about 4500L, and then closing a distillation kettle feeding valve. When the vacuum of the system reaches more than-0.08 MPa, hot water at 60-90 ℃ is conveyed into a jacket of the distillation kettle to be heated, liquid begins to appear in the liquid separation bottle along with the rise of the temperature in the distillation kettle, the liquid level in the liquid separation bottle is closely observed, a reflux valve of the liquid separation bottle is timely adjusted, the liquid level is controlled not to be higher than an overflow port of a low-boiling-point substance, and a mixture of nitromethane and water flows back into the distillation kettle. The heating range is controlled by adjusting the hot water amount and the circulating water amount of a condenser on the top of the kettle, when the temperature in the kettle reaches about 53 ℃, liquid in a liquid separation bottle begins to be layered, at the moment, a vacuumizing valve on a low-boiling-point substance receiving tank is opened, when the vacuum is balanced, a control valve of the low-boiling-point substance receiving tank is opened to place upper-layer low-boiling-point substances into the low-boiling-point substance receiving tank, the opening and closing degree of a reflux valve of the liquid separation bottle is controlled to keep a layered state, and lower-layer nitromethane is refluxed into a distillation kettle.
When the temperature in the distillation kettle reaches above 55 ℃, the circulating water of the condenser at the top of the distillation kettle is fully opened, the temperature of the gas phase at the top of the distillation kettle is higher than 55 ℃, when the clarification of the refluxing nitromethane is observed to be not turbid any more, sampling analysis is carried out, when the analysis is qualified, a vacuumizing valve on the finished product receiving tank is opened, when the vacuum is balanced, a discharging valve on the finished product receiving tank is opened, a water inlet valve of the condenser at the top of the distillation kettle is closed, a three-way valve is adjusted to be switched to complete distillation, and the distilled nitro.
When the three-way valve is switched to complete distillation and liquid in the liquid separation bottle is discharged completely, the vacuum pumping valve on the liquid separation bottle is closed. And closing a vacuum pumping valve of the low-boiling-point substance receiving tank, opening a nitrogen inlet valve of the low-boiling-point substance receiving tank to break vacuum, closing a nitrogen inlet valve, then opening a emptying valve of the low-boiling-point substance receiving tank, and opening a emptying valve of the low-boiling-point substance receiving tank to pump the low-boiling-point substances to the nitromethane synthesis device.
When the distillation is completed to the residual 500L, the hot water valve is properly turned down, when the distillation is completed to the residual 350L, the hot water valve of the jacket is closed, the vacuum-pumping valve of the high-boiling-point substance receiving tank is opened, when the vacuum is balanced, the discharge valve at the bottom of the distillation kettle is opened, and the residual liquid is discharged to the high-boiling-point substance receiving tank. After the distillation kettle is completely discharged, a bottom valve of the distillation kettle is closed, a nitrogen valve is opened to break the vacuum of the high-boiling residue receiving tank, a nitrogen inlet valve is closed, a discharge valve is opened, and the residual liquid is pumped to a nitromethane synthesis device.
After the distillation is finished, closing a feed valve and a vacuum pumping valve of the finished product receiving tank, opening a nitrogen inlet valve of the finished product receiving tank, breaking vacuum by using nitrogen, closing a nitrogen inlet valve, opening an emptying valve of the finished product receiving tank, and opening a pump to send the finished product nitromethane to a hydroxylamine hydrochloride synthesis device or a nitromethane filling device.
And (5) conveying the gas pumped out by the vacuum unit to a nitromethane tail gas absorption tower for treatment.
Compared with the prior art, the invention has the following beneficial effects:
(1) the boiling point of nitromethane is reduced to about 40 ℃ by adopting a reduced pressure distillation method, so that the method is safe and energy-saving;
(2) the nitromethane can be heated and distilled by using hot water with the temperature of about 60-90 ℃, so that the method is safe and energy-saving;
(3) the purification efficiency is high, for example, a 5000L distillation kettle is used for distilling 99.9 percent of nitromethane, the normal pressure distillation needs 45 to 55 hours, while the system only needs 25 to 30 hours, and the efficiency is improved by about 50 percent;
(4) the low-boiling-point substance and the high-boiling-point substance generated in the purification are reused, so that the energy is saved and the environment is protected;
(5) the purification effect is good, the requirements of customers are met, and the economic benefit and the industrial value are obvious.
Drawings
FIG. 1 is a schematic structural view of the present invention;
in the figure: 1. a crude nitromethane intermediate storage tank; 2. a kettle top condenser; 3. a finished product condenser; 4. a three-way valve; 5. a nitrogen storage tank; 6. a vacuum unit; 7. a tail gas absorption tower; 8. a nitromethane synthesis device; 9. a finished product receiving tank; 10. a low-boiling-point substance receiving tank; 11. a liquid separating bottle; 12. a high-boiling residue receiving tank; 13. and (5) a distillation kettle.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the practice of the invention.
Example 1
As shown in fig. 1, the nitromethane reduced pressure distillation system comprises a crude nitromethane intermediate storage tank 1, a distillation still 13, a condenser, a finished product receiving tank 9 and a vacuum unit 6, wherein the condenser comprises a still top condenser 2 and a finished product condenser 3, and the crude nitromethane intermediate storage tank 1 is sequentially connected with the distillation still 13, the still top condenser 2, the finished product condenser 3, a three-way valve 4 and the finished product receiving tank 9; the three-way valve 4 is connected with a liquid separation bottle 11, the liquid separation bottle 11 is respectively connected with a distillation kettle 13 and a low-boiling-point substance receiving tank 10, and a section of pipeline connecting the liquid separation bottle 11 with the distillation kettle 13 is set as a U-shaped pipe; the finished product condenser 3, the liquid separation bottle 11, the low-boiling-point substance receiving tank 10 and the finished product receiving tank 9 are respectively connected with the vacuum unit 6; the low-boiling-point substance receiving tank 10 and the finished product receiving tank 9 are also respectively connected with the nitrogen storage tank 5.
The distillation kettle 13 is of a jacket type structure, and the inside of the jacket is connected with a hot water circulating system.
The distillation still 13 is also connected with a liquid level alarm interlocking device, and is in interlocking closing when the liquid level in the distillation still reaches 4000L and the alarm is carried out at 4500L, and is in interlocking closing when the distillation is finished and the alarm is carried out at the time of 500L and the alarm is carried out at 350L.
A thermometer is arranged on the pipeline above the kettle top condenser 2.
The height of the U-shaped pipe is 1 m. The U-shaped pipe is used as a liquid sealing device, and nitromethane in the pipeline of the U-shaped pipe is used as a liquid sealing medium, so that gas in the distillation kettle is prevented from entering the liquid separation bottle through the U-shaped pipe.
The bottom of the distillation kettle 13 is connected with a high-boiling-point substance receiving tank 12, and the high-boiling-point substance receiving tank 12 is respectively connected with a vacuum unit 6 and a nitrogen storage tank 5.
The atmospheric valve is established in the top of jar body top gas exit to establish and take out the vacuum valve and advance nitrogen gas valve below, the jar body is including low thing receiving tank 10, high thing receiving tank 12 and the finished product receiving tank 9 of boiling.
The high-boiling-point substance receiving tank 12 is also connected with the nitromethane synthesis device 8, so that the high-boiling-point substance is reused.
The low-boiling-point substance receiving tank 10 is also connected with the nitromethane synthesis device 8, so that the low-boiling-point substance is reused.
And the finished product receiving tank 9 is connected with a nitromethane filling device.
And a guide plate is arranged in the lower seal head of the finished product condenser 3.
The vacuum unit 6 is connected with the tail gas absorption tower 7.
When the nitromethane is subjected to reduced pressure distillation, the kettle top condenser 2 and the finished product condenser 3 are checked, and circulating water is started. Checking and opening a vacuum valve on a finished product condenser 3 end socket and a vacuum valve on a liquid separation bottle 11, starting a vacuum unit 6 for vacuumizing, automatically controlling the crude nitromethane in a crude nitromethane intermediate storage tank 1 by a central control room, pumping the crude nitromethane into each distillation kettle 13 to about 4500L, and then closing a feeding valve of the distillation kettle 13. When the vacuum of the system reaches more than-0.08 MPa, hot water at 60-90 ℃ is conveyed into a jacket of the distillation kettle 13 to be heated, the liquid separation bottle 11 begins to generate liquid along with the temperature rise in the distillation kettle 13, the liquid level in the liquid separation bottle 11 is closely observed, a reflux valve of the liquid separation bottle 11 is timely adjusted, the liquid level is controlled not to be higher than an overflow port of a low-boiling-point substance, and a mixture of nitromethane and water is refluxed into the distillation kettle 13. The heating range is controlled by adjusting the hot water amount and the circulating water amount of the kettle top condenser 2, when the temperature in the kettle reaches about 53 ℃, the liquid in the liquid separation bottle 11 begins to be layered, at this time, a vacuum-pumping valve on the low-boiling-point substance receiving tank 10 is opened, when the vacuum is balanced, a control valve of the low-boiling-point substance receiving tank 10 is opened to place the upper-layer low-boiling-point substance into the low-boiling-point substance receiving tank 10, the opening and closing degree of a reflux valve of the liquid separation bottle 11 is controlled to keep the layered state, and the lower-layer nitromethane is refluxed into the distillation kettle.
When the temperature in the distillation kettle 13 reaches above 55 ℃, circulating water in the kettle top condenser 2 is fully opened, the temperature of a gas phase at the top of the distillation kettle 13 is higher than 55 ℃, when the clarification of the returned nitromethane is observed to be not turbid any more, sampling analysis is carried out, when the analysis is qualified, a vacuumizing valve on the finished product receiving tank 9 is opened, when the vacuum is balanced, a discharging valve on the finished product receiving tank 9 is opened, a water inlet valve of the kettle top condenser 2 is closed, the three-way valve 4 is adjusted to be turned into complete distillation, and the distilled nitromethane is placed into the finished product receiving tank 9.
When the three-way valve 4 is switched to complete distillation and the liquid in the liquid separation bottle 11 is discharged completely, the vacuum pumping valve on the liquid separation bottle 11 is closed. And (3) closing the vacuum-pumping valve of the low-boiling-point substance receiving tank 10, then opening a nitrogen inlet valve of the low-boiling-point substance receiving tank 10 to break vacuum, then closing a nitrogen inlet valve, then opening a vent valve of the low-boiling-point substance receiving tank 10, and opening a discharge valve of the low-boiling-point substance receiving tank 10 to pump the low-boiling-point substances to the nitromethane synthesis device 8.
When the distillation is completed to the residual 500L, the hot water valve is properly turned down, when the distillation is completed to the residual 350L, the hot water valve of the jacket is closed, the vacuum valve of the high boiling substance receiving tank 12 is opened, when the vacuum is balanced, the discharge valve at the bottom of the distillation kettle 13 is opened, and the residual liquid is discharged to the high boiling substance receiving tank 12. After the distillation kettle is completely discharged, a bottom valve of the distillation kettle 13 is closed, a nitrogen valve is opened to break the vacuum of the high-boiling residue receiving tank 12, a nitrogen inlet valve is closed, a discharge valve is opened, and the residual liquid is pumped to the nitromethane synthesis device 8.
After the distillation is finished, closing a feed valve and a vacuum pumping valve of the finished product receiving tank 9, opening a nitrogen inlet valve of the finished product receiving tank 9, breaking vacuum by using nitrogen, closing a nitrogen inlet valve, opening an emptying valve of the finished product receiving tank 9, and opening a pump to send the finished product nitromethane to a hydroxylamine hydrochloride synthesis device or a nitromethane filling device.
And the gas pumped out by the vacuum unit 6 is sent to a nitromethane tail gas absorption tower 7 for treatment.
Claims (6)
1. The utility model provides a nitromethane vacuum distillation system, includes storage tank (1) in the middle of crude nitromethane, stills (13), condenser, finished product receiving tank (9) and vacuum unit (6), its characterized in that: the condenser comprises a kettle top condenser (2) and a finished product condenser (3), wherein a crude nitromethane intermediate storage tank (1) is sequentially connected with a distillation kettle (13), the kettle top condenser (2), the finished product condenser (3), a three-way valve (4) and a finished product receiving tank (9); the three-way valve (4) is connected with a liquid separation bottle (11), the liquid separation bottle (11) is respectively connected with a distillation kettle (13) and a low-boiling-point substance receiving tank (10), and a section of pipeline connecting the liquid separation bottle (11) and the distillation kettle (13) is set as a U-shaped pipe; the finished product condenser (3), the liquid separating bottle (11), the low-boiling-point substance receiving tank (10) and the finished product receiving tank (9) are respectively connected with the vacuum unit (6); the low-boiling-point substance receiving tank (10) and the finished product receiving tank (9) are also respectively connected with the nitrogen storage tank (5);
the distillation kettle (13) is of a jacket type structure, and the inside of the jacket is connected with a hot water circulating system;
the bottom of the distillation kettle (13) is connected with a high-boiling-point substance receiving tank (12);
the vacuum unit (6) is connected with the tail gas absorption tower (7);
nitromethane in the U-shaped pipeline serves as a liquid seal medium;
when the nitromethane is subjected to reduced pressure distillation, firstly, a kettle top condenser and a finished product condenser are checked, and circulating water is started; checking and opening a vacuum valve on a finished product condenser end socket and a vacuum valve on a liquid separation bottle, starting a vacuum unit for vacuumizing, automatically controlling the crude nitromethane in a crude nitromethane intermediate storage tank through a central control room, pumping the crude nitromethane into each distillation kettle to 4500L, and then closing a distillation kettle feeding valve; when the vacuum of the system reaches more than-0.08 MPa, hot water at 60-90 ℃ is conveyed into a jacket of the distillation kettle for heating, liquid begins to appear in the liquid separation bottle along with the temperature rise in the distillation kettle, the liquid level in the liquid separation bottle is closely observed, a reflux valve of the liquid separation bottle is timely adjusted, the liquid level is controlled not to be higher than an overflow port of a low-boiling-point substance, and a mixture of nitromethane and water is refluxed into the distillation kettle; controlling the temperature rise range by adjusting the hot water amount and the circulating water amount of a condenser at the top of the kettle, when the temperature in the kettle reaches 53 ℃, starting the liquid in the liquid separation bottle to stratify, then opening a vacuum-pumping valve on the low-boiling-point substance receiving tank, when the vacuum is balanced, opening a control valve of the low-boiling-point substance receiving tank to place the upper-layer low-boiling-point substance into the low-boiling-point substance receiving tank, controlling the opening and closing degree of a reflux valve of the liquid separation bottle to keep a stratified state, and refluxing the lower-layer nitromethane into the distillation kettle for continuous;
when the temperature in the distillation kettle reaches above 55 ℃, the circulating water of the condenser at the top of the distillation kettle is fully opened, the temperature of the gas phase at the top of the distillation kettle is higher than 55 ℃, when the clarification of the refluxing nitromethane is observed to be not turbid any more, sampling analysis is carried out, when the analysis is qualified, a vacuumizing valve on a finished product receiving tank is opened, when the vacuum is balanced, a discharging valve on the finished product receiving tank is opened, a water inlet valve of the condenser at the top of the distillation kettle is closed, a three-way valve is adjusted to be switched to complete distillation, and the distilled nitro;
when the three-way valve is switched to complete distillation and liquid in the liquid separation bottle is discharged completely, the vacuum pumping valve on the liquid separation bottle is closed; closing a vacuum pumping valve of the low-boiling-point substance receiving tank, opening a nitrogen inlet valve of the low-boiling-point substance receiving tank to break vacuum, closing a nitrogen inlet valve, then opening a emptying valve of the low-boiling-point substance receiving tank, and opening a emptying valve of the low-boiling-point substance receiving tank to pump the low-boiling-point substances to the nitromethane synthesis device;
when the distillation is completed to the residual 500L in the kettle, properly reducing the hot water valve, when the distillation is completed to the residual 350L, closing the hot water valve of the jacket, opening the vacuumizing valve of the high-boiling-point substance receiving tank, and when the vacuum is balanced, opening the discharge valve at the bottom of the distillation kettle, and discharging residual liquid to the high-boiling-point substance receiving tank; after the distillation emptying valve is closed after the emptying, the nitrogen valve is opened to break the vacuum of the high-boiling residue receiving tank, the nitrogen inlet valve is closed to open the emptying valve, and the residual liquid is pumped to a nitromethane synthesis device;
after distillation is finished, closing a feed valve and a vacuum pumping valve of a finished product receiving tank, opening a nitrogen inlet valve of the finished product receiving tank, breaking vacuum by using nitrogen, closing a nitrogen inlet valve, opening an emptying valve of the finished product receiving tank, and opening a pump to send the finished product nitromethane to a hydroxylamine hydrochloride synthesis device or a nitromethane filling device;
the high-boiling-point substance receiving tank (12) is also connected with a nitromethane synthesis device (8); the low-boiling-point substance receiving tank (10) is also connected with a nitromethane synthesis device (8); the finished product receiving tank (9) is connected with a hydroxylamine hydrochloride synthesis device or a nitromethane filling device;
the atmospheric valve is established in the top of jar body top gas exit to establish and be in evacuation valve and advance nitrogen gas valve below, the jar body is including low thing receiving tank (10), high thing receiving tank (12) and the finished product receiving tank (9) of boiling.
2. The nitromethane vacuum distillation system according to claim 1, wherein: the distillation still (13) is also connected with a liquid level alarm interlocking device.
3. The nitromethane vacuum distillation system according to claim 1, wherein: a thermometer is arranged on the pipeline above the kettle top condenser (2).
4. The nitromethane vacuum distillation system according to claim 1, wherein: the height of the U-shaped pipe is 0.8-1.2 m.
5. A nitromethane vacuum distillation system according to claim 1 or 4, wherein: the high-boiling-point substance receiving tank (12) is respectively connected with the vacuum unit (6) and the nitrogen storage tank (5).
6. The nitromethane vacuum distillation system according to claim 1, wherein: a guide plate is arranged in the lower seal head of the finished product condenser (3).
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| CN201510786822.1A CN105597354B (en) | 2015-11-16 | 2015-11-16 | Nitromethane reduced pressure distillation system |
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| CN113214086B (en) * | 2021-05-26 | 2022-09-13 | 山东中盛药化设备有限公司 | Continuous rectification and purification process of nitromethane |
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| CN203030013U (en) * | 2012-12-26 | 2013-07-03 | 溧阳维信生物科技有限公司 | Solvent recovery and water removal device for sucralose production |
| CN103435451A (en) * | 2013-08-29 | 2013-12-11 | 张家港市三联化工科技有限公司 | Treatment device applied to recover excessive hydroquinone during DHPPA synthesis |
| CN204607887U (en) * | 2015-05-05 | 2015-09-02 | 临沂远博化工有限公司 | A kind of production unit extracting methyl alcohol from tail gas absorption liquid |
| CN205182224U (en) * | 2015-11-16 | 2016-04-27 | 山东宝源化工股份有限公司 | Nitromethane underpressure distillation system |
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| FR578306A (en) * | 1923-05-09 | 1924-09-23 | Ricard Allenet & Cie Soc | Continuous process and apparatus for the dehydration of organic liquids |
| CN101585519B (en) * | 2008-05-20 | 2011-07-27 | 上海化工研究院 | Method for preparing <15>N-hydroxylamine hydrochloride by hydrolyzing <15>N-nitromethane |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203030013U (en) * | 2012-12-26 | 2013-07-03 | 溧阳维信生物科技有限公司 | Solvent recovery and water removal device for sucralose production |
| CN103435451A (en) * | 2013-08-29 | 2013-12-11 | 张家港市三联化工科技有限公司 | Treatment device applied to recover excessive hydroquinone during DHPPA synthesis |
| CN204607887U (en) * | 2015-05-05 | 2015-09-02 | 临沂远博化工有限公司 | A kind of production unit extracting methyl alcohol from tail gas absorption liquid |
| CN205182224U (en) * | 2015-11-16 | 2016-04-27 | 山东宝源化工股份有限公司 | Nitromethane underpressure distillation system |
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