CN107823908B - Acyl chloride vacuum rectification device and method - Google Patents
Acyl chloride vacuum rectification device and method Download PDFInfo
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- CN107823908B CN107823908B CN201711241086.7A CN201711241086A CN107823908B CN 107823908 B CN107823908 B CN 107823908B CN 201711241086 A CN201711241086 A CN 201711241086A CN 107823908 B CN107823908 B CN 107823908B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/58—Preparation of carboxylic acid halides
- C07C51/64—Separation; Purification; Stabilisation; Use of additives
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to an acyl chloride vacuum rectification device and method. The device comprises an acyl chloride rectifying device and a vacuum unit, wherein a vacuum buffer tank, a cyclone separator and an acyl chloride material collecting device are sequentially connected between the acyl chloride rectifying device and the vacuum unit; the acyl chloride material collecting device comprises a spray tower, a mist catcher and a collecting tank; the top of the spray tower is communicated with a mist catcher, and the mist catcher is communicated with a vacuum unit; the bottom of the mist catcher is connected with a circulating medium collecting tank. The acyl chloride vacuum rectification device and method provided by the invention are reasonable in design and simple in method, and can prevent acyl chloride materials from entering a vacuum unit, so that the production efficiency is improved, the labor intensity of workers in maintenance is reduced, and the service life of the vacuum unit is effectively prolonged.
Description
Technical Field
The invention relates to an acyl chloride vacuum rectification device and method, and belongs to the field of tail gas treatment.
Background
The acyl chloride is a compound containing a-C (O) Cl functional group, belongs to the acyl halide class, has corrosiveness, and is a carboxylic acid derivative formed by replacing hydroxyl in carboxylic acid with chlorine. Common acid chlorides are: m/p-phthaloyl chloride, p-nitrobenzoyl chloride, chloroacetyl chloride.
At present, production enterprises in China mainly adopt a thionyl chloride method or a phosgene method to produce acyl chloride, the refining process in the acyl chloride production process needs to be carried out under a high vacuum working condition, and a roots pump and a water injection pump are generally adopted to form a vacuum unit to provide the high vacuum working condition needed by the acyl chloride refining process. When the vacuum unit operates, the gas extracted from the rectifying device still contains a small amount of acyl chloride materials, particularly m/p-phthaloyl chloride/p-nitrobenzoyl chloride with a higher boiling point, and the materials are finally accumulated in the pump cavity and the rotor of the roots pump, so that the clearance of the rotor is continuously reduced, and the locking of the rotor of the roots pump and the abrasion of an anticorrosive coating on the surface of the rotor are finally caused. In actual production, the maintenance and cleaning period of the roots pump is half a month, and the problems that the production progress is influenced, the labor intensity of workers for maintenance is high and the service life of a vacuum unit is short when acyl chloride materials enter the vacuum unit exist.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the acyl chloride vacuum rectification device which can prevent acyl chloride materials from entering a vacuum unit, thereby improving the production efficiency, reducing the labor intensity of workers in maintenance and prolonging the service life of the vacuum unit; meanwhile, a rectification method is provided, which is simple and easy to implement.
The invention relates to an acyl chloride vacuum rectification device which comprises an acyl chloride rectification device and a vacuum unit, wherein a vacuum buffer tank, a cyclone separator and a collection device are sequentially connected between the acyl chloride rectification device and the vacuum unit; the collecting device comprises a spray tower, a mist catcher and a circulating medium collecting tank; the top of the spray tower is communicated with a mist catcher, and the mist catcher is communicated with a vacuum unit; the bottom of the mist catcher is connected with a circulating medium collecting tank.
The acyl chloride rectifying device comprises an acyl chloride rectifying tower, a condenser and a gas-liquid separator, wherein the top of the acyl chloride rectifying tower is connected with the top of the condenser, and the bottom of the condenser is communicated with the top of the gas-liquid separator; the gas-liquid separator is communicated with the top of the vacuum buffer tank.
The collecting device also comprises a circulating tank, a filter, a first circulating pump and a second circulating pump; the circulation tank is divided into a first chamber and a second chamber by a partition plate; the bottom of the spraying tower is communicated with the top of a first chamber, the first chamber is communicated with the top of a second chamber through a first circulating pump through a pipeline, and a filter is arranged on the pipeline; the second chamber is communicated with the spray tower through a second circulating pump.
Preferably, the upper part and the middle part of the spray tower are respectively provided with a nozzle, and the tower is not filled with filler.
Preferably, the filter is a bag filter.
The bottom of the gas-liquid separator is communicated with the acyl chloride rectifying tower.
The vacuum buffer tank, the cyclone separator and the circulating tank are all provided with cooling jackets for introducing chilled water.
A vacuum rectification method of acyl chloride comprises the following steps:
1) condensing the material from the acyl chloride rectifying tower by a condenser, then feeding the condensed material into a gas-liquid separator for gas-liquid separation, feeding the liquid-phase material into the acyl chloride rectifying tower, feeding the gas-phase material into a cyclone separator through a vacuum buffer tank to remove part of the entrained acyl chloride material, and obtaining a secondary gas-phase material;
2) and the secondary gas-phase material in the cyclone separator enters a spray tower, the entrained acyl chloride material is leached into a first chamber in a circulating tank, the residual secondary gas-phase material after the acyl chloride material is removed enters a mist catcher to catch the entrained circulating medium, the caught circulating medium enters a circulating medium collecting tank, and the residual gas-phase material enters a vacuum unit.
And the circulating medium with the acyl chloride material in the first cavity of the circulating tank enters the second cavity of the circulating tank after entering the filter through the first circulating pump and enters the spray tower through the second circulating pump for recycling.
The temperature in the vacuum buffer tank, the cyclone separator and the circulating tank is 0-10 ℃.
The circulating medium in the circulating tank is liquid with saturated vapor pressure lower than 3kpa at normal temperature.
Preferably, the circulating medium in the circulating tank is sulfuric acid with a concentration of 90% -98%.
Compared with the prior art, the invention has the following advantages:
the acyl chloride vacuum rectification device and method provided by the invention are reasonable in design and simple in method, and can prevent acyl chloride materials from entering a vacuum unit, so that the production efficiency is improved, the labor intensity of workers for overhauling is reduced, the service life of the vacuum unit is effectively prolonged, and the overhaul period of the Roots pump is prolonged from half a month to six months.
Drawings
FIG. 1 is a schematic structural diagram of an acid chloride vacuum rectification device of the present invention.
In the figure: 1. an acyl chloride rectifying tower; 2. a condenser; 3. a gas-liquid separator; 4. a vacuum buffer tank; 5. a cyclone separator; 6. a spray tower; 7. a circulation tank; 8. a first circulation pump; 9. a filter; 10. a second circulation pump; 11. a mist catcher; 12. a circulating medium collection tank; 13. and (4) a vacuum unit.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
Referring to the attached drawing 1, the acyl chloride vacuum rectification device of the embodiment comprises an acyl chloride rectification device and a vacuum unit 13, wherein a vacuum buffer tank 4, a cyclone separator 5 and a collection device are sequentially connected between the acyl chloride rectification device and the vacuum unit 13; the collecting device comprises a spray tower 6, a mist catcher 11 and a circulating medium collecting tank 12; the top of the spray tower 6 is communicated with a mist catcher 11, and the mist catcher 11 is communicated with a vacuum unit 13; the bottom of the mist catcher 11 is connected with a circulating medium collecting tank 12; the acyl chloride rectifying device comprises an acyl chloride rectifying tower 1, a condenser 2 and a gas-liquid separator 3, wherein the top of the acyl chloride rectifying tower 1 is connected with the top of the condenser 2, and the bottom of the condenser 2 is communicated with the top of the gas-liquid separator 3; the gas-liquid separator 3 is communicated with the top of the vacuum buffer tank 4; the collecting device also comprises a circulating tank 7, a filter 9, a first circulating pump 8 and a second circulating pump 10; the circulation tank 7 is divided into a first chamber and a second chamber by a partition; the bottom of the spray tower 6 is communicated with the top of a first chamber, the first chamber is communicated with the top of a second chamber through a first circulating pump 8 through a pipeline, and a filter 9 is arranged on the pipeline; the second chamber is communicated with the spray tower 6 through a second circulating pump 10; the bottom of the gas-liquid separator 3 is communicated with the acyl chloride rectifying tower 1.
A vacuum rectification method of acyl chloride comprises the following steps:
1) condensing the material from the acyl chloride rectifying tower 1 by a condenser 2, then feeding the condensed material into a gas-liquid separator 3 for gas-liquid separation, feeding the liquid-phase material into the acyl chloride rectifying tower 1, feeding the gas-phase material into a cyclone separator 5 through a vacuum buffer tank 4 to remove part of the entrained acyl chloride material, and obtaining a secondary gas-phase material; the temperature of the vacuum buffer tank 4 and the cyclone separator 5 is controlled at 0 ℃ by cooling water through a jacket;
2) the secondary gas-phase material in the cyclone separator 5 enters a spray tower 6, the entrained acyl chloride material is leached into a first chamber of a circulating tank 7, the temperature of the circulating tank 7 is 0 ℃, and the circulating medium is 90% sulfuric acid; the residual secondary gas-phase material after the acyl chloride material is removed enters a mist catcher 11 to catch the entrained circulating medium, the caught circulating medium enters a circulating medium collecting tank 12, and the residual gas-phase material enters a vacuum unit 13;
after a circulating medium with acyl chloride materials in a first cavity of the circulating tank 7 is pressurized by the first circulating pump 8 and enters the filter 9, the acyl chloride materials are left on the surface of the filter bag, and the filtered circulating medium enters a second cavity and enters the spray tower 6 through the second circulating pump 10 for recycling.
Example 2
This example is different from example 1 only in that the temperature of the vacuum buffer tank 4, the cyclone 5 and the circulation tank 7 was 5 ℃ and the sulfuric acid concentration in the circulation tank 7 was controlled to 95%.
Example 3
This example is different from example 1 only in that the temperature of the vacuum buffer tank 4, the cyclone 5 and the circulation tank 7 was 10 ℃ and the sulfuric acid concentration in the circulation tank 7 was controlled to 98%.
Claims (10)
1. The utility model provides an acyl chloride vacuum distillation device, includes acyl chloride distillation device and vacuum unit (13), its characterized in that: a vacuum buffer tank (4), a cyclone separator (5) and a collecting device are sequentially connected between the acyl chloride rectifying device and the vacuum unit (13); the collecting device comprises a spray tower (6), a mist catcher (11) and a circulating medium collecting tank (12); the top of the spray tower (6) is communicated with a mist catcher (11), and the mist catcher (11) is communicated with a vacuum unit (13); the bottom of the mist catcher (11) is connected with a circulating medium collecting tank (12).
2. An acid chloride vacuum rectification apparatus as claimed in claim 1, characterized in that: the acyl chloride rectifying device comprises an acyl chloride rectifying tower (1), a condenser (2) and a gas-liquid separator (3), wherein the top of the acyl chloride rectifying tower (1) is connected with the top of the condenser (2), and the bottom of the condenser (2) is communicated with the top of the gas-liquid separator (3); the gas-liquid separator (3) is communicated with the top of the vacuum buffer tank (4).
3. An acid chloride vacuum rectification apparatus as claimed in claim 1, characterized in that: the collecting device also comprises a circulating tank (7), a filter (9), a first circulating pump (8) and a second circulating pump (10); the circulation tank (7) is divided into a first chamber and a second chamber by a partition plate; the bottom of the spray tower (6) is communicated with the top of the first chamber, the first chamber is communicated with the top of the second chamber through a first circulating pump (8) through a pipeline, and a filter (9) is arranged on the pipeline; the second chamber is communicated with the spray tower (6) through a second circulating pump (10).
4. An acid chloride vacuum rectification apparatus as claimed in claim 2, characterized in that: the bottom of the gas-liquid separator (3) is communicated with the acyl chloride rectifying tower (1).
5. An acid chloride vacuum rectification apparatus as claimed in claim 1, characterized in that: the vacuum buffer tank (4) and the cyclone separator (5) are both provided with cooling jackets for introducing chilled water.
6. An acid chloride vacuum rectification apparatus as claimed in claim 3, characterized in that: the circulating tank (7) is provided with a cooling jacket for introducing chilled water.
7. The vacuum rectification method of acyl chloride is characterized by comprising the following steps: the method comprises the following steps:
1) condensing the material from the acyl chloride rectifying tower (1) by a condenser (2), then feeding the condensed material into a gas-liquid separator (3) for gas-liquid separation, feeding the liquid-phase material into the acyl chloride rectifying tower (1), feeding the gas-phase material into a cyclone separator (5) through a vacuum buffer tank (4) to remove part of entrained acyl chloride material, and obtaining a secondary gas-phase material;
2) and the secondary gas-phase material in the cyclone separator (5) enters a spray tower (6), the entrained acyl chloride material is leached into a first chamber in a circulating tank (7), the residual secondary gas-phase material after the acyl chloride material is removed enters a mist catcher (11) to capture the entrained circulating medium, the captured circulating medium enters a circulating medium collecting tank (12), and the residual gas-phase material enters a vacuum unit (13).
8. A method for the vacuum distillation of acid chloride according to claim 7, wherein: and a circulating medium with an acyl chloride material in a first chamber of the circulating tank (7) enters a second chamber of the circulating tank (7) after entering a filter (9) through a first circulating pump (8) and enters the spray tower (6) through a second circulating pump (10) for recycling.
9. A method for the vacuum distillation of acid chloride according to claim 7, wherein: the temperature in the vacuum buffer tank (4), the cyclone separator (5) and the circulating tank (7) is 0-10 ℃.
10. A method for the vacuum distillation of acid chloride according to claim 7, wherein: the circulating medium in the circulating tank (7) is liquid with saturated vapor pressure lower than 3kpa at normal temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711241086.7A CN107823908B (en) | 2017-11-30 | 2017-11-30 | Acyl chloride vacuum rectification device and method |
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| CN201711241086.7A CN107823908B (en) | 2017-11-30 | 2017-11-30 | Acyl chloride vacuum rectification device and method |
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| Publication Number | Publication Date |
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| CN107823908A CN107823908A (en) | 2018-03-23 |
| CN107823908B true CN107823908B (en) | 2020-04-07 |
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| CN115155088B (en) * | 2022-06-16 | 2024-04-30 | 安徽广信农化股份有限公司 | Rectifying device for KL540 crystallization processing and application method thereof |
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| RU2188224C2 (en) * | 2000-11-13 | 2002-08-27 | Цегельский Валерий Григорьевич | Plant for oil product distillation |
| CN2585995Y (en) * | 2002-12-17 | 2003-11-12 | 金持中 | Aerated water jetting vacuum extractor for tech of urea prodn. |
| US8747622B2 (en) * | 2011-06-28 | 2014-06-10 | Uop Llc | Aromatics-recovery process |
| CN107840858A (en) * | 2017-10-28 | 2018-03-27 | 南通江山农药化工股份有限公司 | The continuous rectification under vacuum technique of Trimethyl phosphite |
| CN207755798U (en) * | 2017-11-30 | 2018-08-24 | 山东凯盛新材料股份有限公司 | Acyl chlorides vacuum rectifying apparatus |
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