CN217568079U - Propionyl chloride production tail gas processing apparatus - Google Patents
Propionyl chloride production tail gas processing apparatus Download PDFInfo
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- CN217568079U CN217568079U CN202221257952.8U CN202221257952U CN217568079U CN 217568079 U CN217568079 U CN 217568079U CN 202221257952 U CN202221257952 U CN 202221257952U CN 217568079 U CN217568079 U CN 217568079U
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Abstract
The utility model relates to a propionyl chloride production technical field, concretely relates to propionyl chloride tail gas treatment separator. The propionyl chloride production tail gas treatment device comprises a reaction kettle and a distillation kettle which are sequentially connected, a reaction kettle primary condenser and a reaction kettle secondary condenser which are sequentially connected with the top of the reaction kettle, a distillation kettle primary condenser and a distillation kettle secondary condenser which are sequentially connected with the top of the distillation kettle, a water absorption tower and an alkali absorption tower; the coolant inlet of the reaction kettle second-stage condenser and the coolant inlet of the distillation kettle second-stage condenser are both connected with a coolant inlet pipe, the coolant outlet of the reaction kettle first-stage condenser and the distillation kettle first-stage condenser are respectively connected with a coolant inlet, and the coolant outlet of the reaction kettle first-stage condenser and the distillation kettle first-stage condenser is both connected with a coolant outlet pipe. The utility model discloses reduced the remaining of propionyl chloride, propionic acid in the noncondensable gas, improved the product yield, reduced tail gas treatment pressure, improved condenser operating stability simultaneously.
Description
Technical Field
The utility model relates to a propionyl chloride production technical field, concretely relates to propionyl chloride production tail gas processing apparatus.
Background
Propionyl chloride is used as an intermediate of ibuprofen, clethodim and propanil serving as pesticides and is an important chemical raw material. The current common production methods of propionyl chloride comprise: phosphorus trichloride process, phosphorus pentachloride process, and thionyl chloride process. The phosphorus trichloride method is characterized in that propionic acid and phosphorus trichloride react to generate propionyl chloride and phosphorous acid, then the propionyl chloride and the phosphorous acid are separated through sedimentation separation, the propionyl chloride is distilled, and fractions at 80 ℃ are collected to obtain the propionyl chloride.
The phosphorus trichloride method is the most common propionyl chloride production method at present, and when propionic acid and phosphorus trichloride are reacted and propionyl chloride is distilled, tail gas is generally treated by cooling refrigerating fluid of a condenser and separating gas from liquid. Because the propionyl chloride has a low boiling point (77-79 ℃), although condensation is carried out, 8-10% of propionyl chloride non-condensable gas enters an absorption system, the product yield is low, the recovered hydrochloric acid impurities are more, and the VOCs in tail gas emission is high, so that the tail gas treatment pressure is high; and the tail gas has higher temperature, is directly cooled by refrigerating fluid of the condenser, has larger temperature difference, and easily causes the fluctuation of a heat exchange tube of the condenser in a quenching state by gas to cause the fault of the condenser.
SUMMERY OF THE UTILITY MODEL
The to-be-solved technical problem of the utility model is: the utility model provides a propionyl chloride production tail gas processing apparatus adopts the two-stage condensation to carry out progressively cooling recovery to tail gas, has reduced the residue of propionyl chloride, propionic acid in the noncondensable gas, has improved the product yield, has reduced tail gas treatment pressure, has improved condenser operating stability simultaneously.
The propionyl chloride production tail gas treatment device comprises a reaction kettle and a distillation kettle which are connected in sequence, a reaction kettle primary condenser and a reaction kettle secondary condenser which are connected in sequence with the top of the reaction kettle, a distillation kettle primary condenser and a distillation kettle secondary condenser which are connected in sequence with the top of the distillation kettle, a water absorption tower and an alkali absorption tower; cooling medium inlets of the reaction kettle secondary condenser and the distillation kettle secondary condenser are both connected with a cooling liquid inlet pipe, cooling medium outlets of the reaction kettle primary condenser and the distillation kettle primary condenser are respectively connected with a cooling medium inlet of the reaction kettle primary condenser and a cooling medium outlet of the distillation kettle primary condenser are both connected with a cooling liquid outlet pipe; and the non-condensable gas outlets of the reaction kettle secondary condenser and the distillation kettle secondary condenser are sequentially connected with the water absorption tower and the alkali absorption tower.
Preferably, the condensate of the second-stage condenser of the reaction kettle enters the reaction kettle after passing through the first-stage condenser of the reaction kettle. When tail gas generated in the production process of the reaction kettle is condensed, the temperature of a cooling liquid of a secondary condenser of the reaction kettle is between-15 and-20 ℃, the temperature is reduced to about 10 to 15 ℃ after heat exchange, and the cooling liquid is used as the cooling liquid of a primary condenser of the reaction kettle; the tail gas of the reaction kettle is primarily cooled by cooling liquid at about 10-15 ℃ in a first-stage condenser of the reaction kettle, is deeply cooled by cooling liquid at about-15 to-20 ℃ in a second-stage condenser of the reaction kettle, and is fully condensed with propylene and propionyl chloride contained in the tail gas and then returns to the reaction kettle for production; firstly, the cooling capacity contained in the cooling liquid is fully utilized; secondly, the problem that the heat exchange tube of the condenser fluctuates due to large temperature difference when the gas enters the condenser is avoided by gradual cooling; and thirdly, the tail gas containing low-boiling-point raw materials and products is fully condensed and recovered, so that the product yield is improved, and the tail gas treatment pressure is reduced.
Preferably, the condensate of the secondary condenser of the distillation still enters the distillation still after passing through the primary condenser of the distillation still. When tail gas generated in the distillation process of the distillation kettle is condensed, the temperature of cooling liquid of a secondary condenser of the distillation kettle is between-15 and-20 ℃, the temperature is reduced to about 10 to 15 ℃ after heat exchange, and then the cooling liquid is used as cooling liquid of a primary condenser of the distillation kettle; the distilled gas in the distillation kettle is primarily cooled by cooling liquid at about 10-15 ℃ in a first-stage condenser of the distillation kettle, is deeply cooled by cooling liquid at about-15 to-20 ℃ in a second-stage condenser of the distillation kettle, and is returned to the distillation kettle after propionyl chloride contained in the distilled gas is fully condensed.
Preferably, the bottom of the still is connected to a propionyl chloride product line. The propionyl chloride after the hydrogen chloride gas is distilled out is discharged.
Preferably, an absorption liquid inlet of the water absorption tower is connected with an absorption water pipeline, an absorption liquid outlet is connected with a hydrochloric acid storage tank, and a tail gas outlet is connected with an alkali absorption tower inlet. The tail gas treated by the two-stage condenser mainly contains hydrogen chloride gas, the part of the tail gas is introduced into a water absorption tower and is absorbed by water, and the obtained hydrochloric acid is discharged into a hydrochloric acid storage tank from the bottom of the tower and is used as a byproduct.
Preferably, an absorption liquid outlet of the alkali absorption tower is connected with an alkali liquor circulating tank, and the alkali liquor circulating tank is respectively connected with an absorption liquid inlet and an alkali liquor discharge pipe of the alkali absorption tower after passing through an alkali liquor circulating pump. The tail gas absorbed by the water absorption tower also contains trace hydrogen chloride gas, and the hydrogen chloride gas is discharged after being absorbed by alkali liquor in the alkali absorption tower, so that the hydrogen chloride gas contained in the tail gas is completely removed. The alkali liquor in the alkali absorption tower can be circularly used for tail gas absorption, when the salt concentration is increased after the absorption, the alkali liquor is discharged from an alkali liquor discharge pipe for treatment, and fresh alkali liquor is added into an alkali liquor circulation tank.
Further, a tail gas outlet of the alkali absorption tower is connected with a pipeline going to a tail gas treatment system. After absorption by the alkali absorption tower, the tail gas has extremely low content of VOCs and is sent to a tail gas treatment system for treatment.
The working process of the propionyl chloride production tail gas treatment device is as follows:
when the phosphorus trichloride method is used for producing propionyl chloride, tail gas generated in the synthesis process of a reaction kettle mainly comprises unreacted propionic acid, hydrogen chloride and propionyl chloride generated by reaction, the tail gas is primarily cooled by cooling liquid at about 10-15 ℃ in a first-stage condenser of the reaction kettle, then is deeply cooled by cooling liquid at about-15 to-20 ℃ in a second-stage condenser of the reaction kettle, and propylene and propionyl chloride contained in the tail gas are fully condensed and then are returned to the reaction kettle for production; after the reaction is finished, carrying out precipitation and layering on generated phosphorous acid and propionyl chloride, discharging the propionyl chloride into a distillation still for distillation and refining, wherein tail gas generated in the distillation process of the distillation still mainly comprises hydrogen chloride and a small amount of propionyl chloride, carrying out primary cooling on the part of the tail gas by cooling liquid at about 10-15 ℃ in a primary condenser of the distillation still, carrying out deep cooling on the part of the tail gas by cooling liquid at about-15 to-20 ℃ in a secondary condenser of the distillation still, fully condensing the propionyl chloride contained in the tail gas and then returning the tail gas to the distillation still; the tail gas treated by the two-stage condenser mainly contains hydrogen chloride gas, the tail gas is introduced into a water absorption tower and is absorbed by water, and the obtained hydrochloric acid is discharged into a hydrochloric acid storage tank from the bottom of the tower and is used as a byproduct; the tail gas absorbed by the water absorption tower also contains trace hydrogen chloride gas, and the hydrogen chloride gas is discharged after being absorbed by alkali liquor in the alkali absorption tower, so that the hydrogen chloride gas in the tail gas is completely removed, wherein the alkali liquor in the alkali absorption tower can be circularly used for tail gas absorption, when the salt concentration is increased after the absorption, the alkali liquor is discharged by an alkali liquor discharge pipe for treatment, and fresh alkali liquor is added into an alkali liquor circulation tank; after absorption by the alkali absorption tower, the tail gas has extremely low content of VOCs and is sent to a tail gas treatment system for treatment.
Compared with the prior art, the utility model discloses following beneficial effect has:
the propionyl chloride production tail gas treatment device adopts two-stage condensation to treat tail gas generated in the production process and tail gas generated in the distillation process, and adopts cooling liquid discharged by the second-stage condenser as cooling liquid of the first-stage condenser, so that firstly, the cooling capacity contained in the cooling liquid is fully utilized; secondly, the problem that the heat exchange tube of the condenser fluctuates because the temperature difference is large when the gas enters the condenser is avoided by gradual cooling; and thirdly, the tail gas containing low boiling point raw materials and products is fully condensed and recovered, so that the product yield is improved, the impurity content in the hydrochloric acid as a byproduct is reduced, the content of VOCs in the tail gas is also reduced, and the tail gas treatment pressure is reduced.
Drawings
FIG. 1 is a schematic structural view of the propionyl chloride production tail gas treatment device of the utility model;
in the figure: 1. a reaction kettle; 2. a first-stage condenser of the reaction kettle; 3. a secondary condenser of the reaction kettle; 4. a second-stage condenser of the distillation kettle; 5. a first-stage condenser of the distillation kettle; 6. a distillation kettle; 7. a propionyl chloride product line; 8. a coolant outlet pipe; 9. a cooling liquid inlet pipe; 10. an absorption water line; 11. a water absorption tower; 12. a hydrochloric acid storage tank; 13. to a tail gas treatment system pipeline; 14. an alkali absorption tower; 15. an alkali liquor circulating tank; 16. an alkali liquor circulating pump; 17. and an alkali liquor discharge pipe.
Detailed Description
The following will describe in detail specific embodiments of the present invention. Well-known structures or functions may not be described in detail in the following embodiments in order to avoid unnecessarily obscuring the details. Approximating language, as used herein in the following examples, may be applied to identify quantitative representations that could permissibly vary in number without resulting in a change in the basic function. Unless defined otherwise, technical and scientific terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
Example 1
As shown in figure 1, the propionyl chloride production tail gas treatment device of the utility model comprises a reaction kettle 1 and a distillation kettle 6 which are connected in sequence, a reaction kettle first-stage condenser 2 and a reaction kettle second-stage condenser 3 which are connected in sequence with the top of the reaction kettle 1, a distillation kettle first-stage condenser 5 and a distillation kettle second-stage condenser 4 which are connected in sequence with the top of the distillation kettle 6, a water absorption tower 11 and an alkali absorption tower 14; cooling medium inlets of the reaction kettle secondary condenser 3 and the distillation kettle secondary condenser 4 are both connected with a cooling liquid inlet pipe 9, cooling medium outlets are respectively connected with cooling medium inlets of the reaction kettle primary condenser 2 and the distillation kettle primary condenser 5, and cooling medium outlets of the reaction kettle primary condenser 2 and the distillation kettle primary condenser 5 are both connected with a cooling liquid outlet pipe 8; and the non-condensable gas outlets of the reaction kettle secondary condenser 3 and the distillation kettle secondary condenser 4 are sequentially connected with a water absorption tower 11 and an alkali absorption tower 14.
Preferably, the condensate of the second-stage condenser 3 of the reaction kettle enters the reaction kettle 1 after passing through the first-stage condenser 2 of the reaction kettle. When tail gas generated in the production process of the reaction kettle 1 is condensed, the temperature of a cooling liquid of the secondary condenser 3 of the reaction kettle is between 15 ℃ below zero and 20 ℃ below zero, the temperature is reduced to between 10 ℃ and 15 ℃ after heat exchange, and the cooling liquid is used as a cooling liquid of the primary condenser 2 of the reaction kettle; the tail gas of the reaction kettle 1 is primarily cooled by cooling liquid at about 10-15 ℃ in a first-stage condenser 2 of the reaction kettle, is deeply cooled by cooling liquid at about-15 to-20 ℃ in a second-stage condenser 3 of the reaction kettle, and is fully condensed with propylene and propionyl chloride contained in the tail gas and then returns to the reaction kettle 1 for production; firstly, the cooling capacity contained in the cooling liquid is fully utilized; secondly, the problem that the heat exchange tube of the condenser fluctuates due to large temperature difference when the gas enters the condenser is avoided by gradual cooling; and thirdly, the raw materials and products with low boiling points in the tail gas are fully condensed and recovered, so that the product yield is improved, and the tail gas treatment pressure is reduced.
Preferably, the condensate of the distillation still secondary condenser 4 enters the distillation still 6 after passing through the distillation still primary condenser 5. When tail gas generated in the distillation process of the distillation kettle 6 is condensed, the temperature of a cooling liquid of a secondary condenser 4 of the distillation kettle is about-15 to-20 ℃, the temperature is reduced to about 10 to 15 ℃ after heat exchange, and the cooling liquid is used as a cooling liquid of a primary condenser 5 of the distillation kettle; the distilled gas of the distillation kettle 6 is primarily cooled by cooling liquid at about 10-15 ℃ in the first-stage condenser 5 of the distillation kettle, is deeply cooled by cooling liquid at about-15 to-20 ℃ in the second-stage condenser 4 of the distillation kettle, and is fully condensed and then returned to the distillation kettle 6.
Preferably, the bottom of the distillation still 6 is connected with a propionyl chloride product line 7. The propionyl chloride after the hydrogen chloride gas is distilled out is discharged.
Preferably, an absorption liquid inlet of the water absorption tower 11 is connected with an absorption water pipeline 10, an absorption liquid outlet is connected with a hydrochloric acid storage tank 12, and a tail gas outlet is connected with an inlet of an alkali absorption tower 14. The tail gas treated by the two-stage condenser mainly contains hydrogen chloride gas, the tail gas is introduced into a water absorption tower 11 and is absorbed by water, and the obtained hydrochloric acid is discharged into a hydrochloric acid storage tank 12 from the bottom of the tower to be used as a byproduct.
Preferably, an absorption liquid outlet of the alkali absorption tower 14 is connected with an alkali liquid circulation tank 15, and the alkali liquid circulation tank 15 is connected with an absorption liquid inlet and an alkali liquid discharge pipe 17 of the alkali absorption tower 14 respectively after passing through an alkali liquid circulation pump 16. The tail gas absorbed by the water absorption tower 11 also contains trace hydrogen chloride gas, and the hydrogen chloride gas is discharged after being absorbed by the alkali liquor in the alkali absorption tower 14, so that the hydrogen chloride gas contained in the tail gas is completely removed. The alkali liquor in the alkali absorption tower 14 can be recycled for tail gas absorption, when the salt concentration is increased after the absorption, the alkali liquor is discharged from an alkali liquor discharge pipe 17 for treatment, and fresh alkali liquor is added into an alkali liquor circulation tank 15.
Further, a tail gas outlet of the alkali absorption tower 14 is connected with a tail gas processing system pipeline 13. After being absorbed by the alkali absorption tower 14, the tail gas has extremely low content of VOCs and is sent to a tail gas treatment system for treatment.
The working process of the propionyl chloride production tail gas treatment device is as follows:
when the phosphorus trichloride method is used for producing propionyl chloride, tail gas generated in the synthesis process of a reaction kettle 1 mainly comprises unreacted propionic acid, hydrogen chloride and propionyl chloride generated by reaction, the tail gas is primarily cooled by cooling liquid at about 10-15 ℃ in a first-stage condenser 2 of the reaction kettle, then is deeply cooled by cooling liquid at about-15 to-20 ℃ in a second-stage condenser 3 of the reaction kettle, and propylene and propionyl chloride contained in the tail gas are fully condensed and then return to the reaction kettle 1 for production; after the reaction is finished, the generated phosphorous acid and propionyl chloride are precipitated and layered, the propionyl chloride is discharged into a distillation still 6 for distillation and refining, the tail gas generated in the distillation process of the distillation still 6 is mainly hydrogen chloride and a small amount of propionyl chloride, the part of the tail gas is primarily cooled by cooling liquid at about 10-15 ℃ in a first-stage condenser 5 of the distillation still, then is deeply cooled by cooling liquid at about-15 to-20 ℃ in a second-stage condenser 4 of the distillation still, and the propionyl chloride contained in the tail gas is fully condensed and then returns to the distillation still 6; the tail gas treated by the two-stage condenser mainly contains hydrogen chloride gas, the part of the tail gas is led into a water absorption tower 11 and is absorbed by water, and the obtained hydrochloric acid is discharged into a hydrochloric acid storage tank 12 from the bottom of the tower and is used as a byproduct; the tail gas absorbed by the water absorption tower 11 also contains trace hydrogen chloride gas, and the hydrogen chloride gas is discharged after being absorbed by alkali liquor in the alkali absorption tower 14, so that the hydrogen chloride gas in the tail gas is completely removed, wherein the alkali liquor in the alkali absorption tower 14 can be recycled for tail gas absorption, and after the alkali liquor is absorbed and the salt concentration is increased, the alkali liquor is discharged from an alkali liquor discharge pipe 17 for treatment, and fresh alkali liquor is added into an alkali liquor circulation tank 15; after being absorbed by the alkali absorption tower 14, the tail gas has extremely low content of VOCs and is sent to a tail gas treatment system for treatment.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described above, or equivalents may be substituted for elements thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. The utility model provides a propionyl chlorine production tail gas processing apparatus which characterized in that: comprises a reaction kettle (1) and a distillation kettle (6) which are connected in sequence, a reaction kettle first-stage condenser (2) and a reaction kettle second-stage condenser (3) which are connected with the top of the reaction kettle (1) in sequence, a distillation kettle first-stage condenser (5) and a distillation kettle second-stage condenser (4) which are connected with the top of the distillation kettle (6) in sequence, a water absorption tower (11) and an alkali absorption tower (14); cooling medium inlets of the reaction kettle secondary condenser (3) and the distillation kettle secondary condenser (4) are both connected with a cooling liquid inlet pipe (9), cooling medium outlets are respectively connected with cooling medium inlets of the reaction kettle primary condenser (2) and the distillation kettle primary condenser (5), and cooling medium outlets of the reaction kettle primary condenser (2) and the distillation kettle primary condenser (5) are both connected with a cooling liquid outlet pipe (8); and the non-condensable gas outlets of the reaction kettle secondary condenser (3) and the distillation kettle secondary condenser (4) are sequentially connected with a water absorption tower (11) and an alkali absorption tower (14).
2. The apparatus for treating the tail gas from propionyl chloride production of claim 1, characterized in that: and the condensate of the reaction kettle secondary condenser (3) enters the reaction kettle (1) after passing through the reaction kettle primary condenser (2).
3. The apparatus for treating the tail gas from propionyl chloride production of claim 1, characterized in that: and the condensate of the distillation kettle secondary condenser (4) enters the distillation kettle (6) after passing through the distillation kettle primary condenser (5).
4. The apparatus for treating the tail gas from propionyl chloride production of claim 1, characterized in that: the bottom of the distillation still (6) is connected with a propionyl chloride product pipeline (7).
5. The propionyl chloride production tail gas processing apparatus of claim 1, characterized in that: an absorption liquid inlet of the water absorption tower (11) is connected with an absorption water pipeline (10), an absorption liquid outlet is connected with a hydrochloric acid storage tank (12), and a tail gas outlet is connected with an alkali absorption tower (14) inlet.
6. The propionyl chloride production tail gas processing apparatus of claim 1, characterized in that: an absorption liquid outlet of the alkali absorption tower (14) is connected with an alkali liquid circulating tank (15), and the alkali liquid circulating tank (15) is respectively connected with an absorption liquid inlet and an alkali liquid discharge pipe (17) of the alkali absorption tower (14) after passing through an alkali liquid circulating pump (16).
7. The apparatus for treating the tail gas from propionyl chloride production of claim 6, characterized in that: the tail gas outlet of the alkali absorption tower (14) is connected with a pipeline (13) leading to a tail gas treatment system.
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| CN202221257952.8U CN217568079U (en) | 2022-05-24 | 2022-05-24 | Propionyl chloride production tail gas processing apparatus |
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| CN202221257952.8U CN217568079U (en) | 2022-05-24 | 2022-05-24 | Propionyl chloride production tail gas processing apparatus |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116020259A (en) * | 2022-12-15 | 2023-04-28 | 莒南国泰化工有限公司 | Sulfonyl chloride synthesis tail gas treatment device and method |
| CN119390563A (en) * | 2025-01-02 | 2025-02-07 | 新华制药（寿光）有限公司 | Continuous synthesis process of propionyl chloride |
-
2022
- 2022-05-24 CN CN202221257952.8U patent/CN217568079U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116020259A (en) * | 2022-12-15 | 2023-04-28 | 莒南国泰化工有限公司 | Sulfonyl chloride synthesis tail gas treatment device and method |
| CN119390563A (en) * | 2025-01-02 | 2025-02-07 | 新华制药（寿光）有限公司 | Continuous synthesis process of propionyl chloride |
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