CN216378008U - System for producing low-residual alcohol monoalkyl fatty tertiary amine - Google Patents
System for producing low-residual alcohol monoalkyl fatty tertiary amine Download PDFInfo
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- CN216378008U CN216378008U CN202123096313.6U CN202123096313U CN216378008U CN 216378008 U CN216378008 U CN 216378008U CN 202123096313 U CN202123096313 U CN 202123096313U CN 216378008 U CN216378008 U CN 216378008U
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Abstract
The utility model discloses a system for producing low-residual alcohol monoalkyl fatty tertiary amine, which comprises an amination kettle, an amination tower, a multistage condensing device, an oil-water separator, a dimethylamine recovery device and a compression buffer device, wherein an outlet of the amination kettle is connected with the amination tower, the amination tower is circularly connected with the multistage condensing device, and the multistage condensing device is connected with a feed inlet of the amination kettle through the compression buffer device to form a circulating loop; the multistage condensing device is connected with the oil-water separator, a water outlet at the lower end of the oil-water separator is connected with the dimethylamine recovery device, and the dimethylamine recovery device is connected with a feed inlet of the amination kettle through the compression buffer device to form another circulation loop. The multistage condensation device is arranged to realize fractional condensation of alcohol, tertiary amine and water, so that energy consumption is reduced, and the dimethylamine recovery device is arranged to realize cyclic utilization of materials and reduce environmental pollution.
Description
Technical Field
The utility model belongs to the technical field of organic synthesis, and particularly relates to a system for producing low-residual alcohol monoalkyl fatty tertiary amine.
Background
The device for preparing the monoalkyl fatty tertiary amine by the conventional alcohol method adopts primary condensation, circulating gas is directly condensed to low temperature and then subjected to water oil separation, a water layer is collected, and an oil layer flows back to a reaction kettle for reaction. The development of the process requires further improvement of the purity of the product prepared by the process and reduction of energy consumption, the alcohol content of the product prepared by the conventional method is less than 1%, and the recovery rate of amine in the production process is not high.
SUMMERY OF THE UTILITY MODEL
In order to improve the recovery utilization rate of energy in the process of preparing the monoalkyl fatty tertiary amine by an alcohol method and reduce the alcohol content of a final product, the utility model aims to provide a system for producing the monoalkyl fatty tertiary amine with low residual alcohol.
In order to achieve the purpose, the following technical scheme is provided:
a system for producing low-residual alcohol monoalkyl fatty tertiary amine comprises an amination kettle, an amination tower, a multi-stage condensing device, an oil-water separator, a dimethylamine recovery device and a compression buffer device, wherein an outlet of the amination kettle is connected with the amination tower, the amination tower is circularly connected with the multi-stage condensing device, and the multi-stage condensing device is connected with a feed inlet of the amination kettle through the compression buffer device to form a circulating loop; the multistage condensing device is connected with the oil-water separator, a water outlet at the lower end of the oil-water separator is connected with the dimethylamine recovery device, and the dimethylamine recovery device is connected with a feed inlet of the amination kettle through the compression buffer device to form another circulation loop.
Further, the multistage condensing device comprises a first-stage condenser and a second-stage condenser, the outlet of the amination tower is connected with the feed inlet of the first-stage condenser, the bottom discharge port of the first-stage condenser is connected with the side line of the amination tower through a pipeline, the top discharge port of the first-stage condenser is connected with the feed inlet of the second-stage condenser through a pipeline, the bottom discharge port of the second-stage condenser is connected with the oil-water separator through a pipeline, the top discharge port of the oil-water separator and the bottom outlet pipeline of the first-stage condenser are converged into a pipeline and then connected with the side line of the amination tower, the top discharge port of the second-stage condenser is connected with the compression buffer device, the first-stage condenser is used for cooling alcohol and tertiary amine, the second-stage condenser is used for cooling water, if the first-stage condensing method is adopted, the area of the cooler needs to be large due to large cooling capacity, and simultaneously, the water, the fatty alcohol and the tertiary amine are all cooled to the same low temperature and pass through the oil-water separator, the unreacted fatty alcohol and tertiary amine on the upper layer return to the amination tower, the large-flow cold charge flows back, the rising air flow (containing water, alcohol and tertiary amine) is met, part of the rising air flow is cooled and returns to the kettle, the energy consumption is increased, the evaporation generated water is not facilitated to be taken out of a reaction system, the copper-nickel catalyst can be partially inactivated after the rising air flow returns to the kettle, the reaction is slowed down, the production efficiency is reduced, the unit consumption of the catalyst can be increased, the sectional condensation is realized, compared with the one-time condensation, the condensation energy consumption is reduced, the reaction efficiency is improved, and the alcohol and the tertiary amine are effectively separated from the water.
Furthermore, the compression buffering device comprises a buffering tank before the pump, an amine compressor and a buffering tank after the pump, a discharge port at the top of the secondary condenser is connected with the buffering tank after the pump, the buffering tank after the pump is sequentially connected with the amine compressor and the buffering tank before the pump, the discharge port of the buffering tank before the pump is divided into two branches, one branch is connected with the rectifying kettle, and the other branch is connected with a feed inlet of the amination kettle.
Further, dimethylamine recovery unit includes amine recovery cauldron, amine recovery tower and amine recovery condenser, and oil water separator's lower extreme delivery port passes through the pipeline and is connected with amine recovery cauldron, and amine recovery cauldron connects gradually amine recovery tower and amine recovery condenser, and the air intake pipe of amine recovery condenser and preceding buffer tank of pump joins in marriage and is connected, and the air intake pipe is used for letting in nitrogen gas, hydrogen and dimethylamine.
Furthermore, a feed inlet of the amination kettle is connected with a feed pipe, the feed pipe extends to the bottom of the amination kettle, the feed pipe extends to the bottom, gas enters from the bottom to play a role in bubbling reaction, the reaction efficiency is improved, and a reaction product is pressed into the rectification kettle by utilizing the pressure of the amination kettle and the gas inlet pipe extending to the bottom.
Furthermore, automatic regulating valves are arranged on cold source feeding and discharging pipelines of the first-stage condenser and the second-stage condenser and used for controlling the flow of the cold source.
Furthermore, an automatic cut-off valve is arranged on a branch of the buffer tank in front of the pump connected with the rectifying kettle, an automatic cut-off valve is arranged on a pipeline of the amine recovery condenser connected with the air inlet pipe, and the automatic cut-off valve can be used as a material to be introduced into the amination kettle after the dimethylamine is recovered.
The utility model has the beneficial effects that:
1) the multistage condensing device is adopted for sectional condensation, so that the energy consumption is effectively reduced, and the reaction efficiency is improved;
2) dimethylamine in the circulating gas is recycled, so that the unit consumption of dimethylamine materials is improved, and the environmental pollution is reduced;
3) the reaction efficiency of the amination kettle is improved by adopting a bubbling feeding mode.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention;
in the figure: 1. an amination kettle; 2. an amination tower; 3. a first-stage condenser; 4. a secondary condenser; 5. an oil-water separator; 6. a pump front buffer tank; 7. an amine compressor; 8. a post-pump buffer tank; 9. an amine recovery kettle; 10. an amine recovery column; 11. an amine recovery condenser; 12. an automatic regulating valve; 13. an automatic shut-off valve.
Detailed Description
The utility model will be further described with reference to the drawings attached to the description, but the scope of the utility model is not limited thereto.
A system for producing low residual alcohol monoalkyl fatty tertiary amine comprises an amination kettle 1, an amination tower 2, a primary condenser 3, a secondary condenser 4, an oil-water separator 5, a buffer tank 6 before a pump, an amine compressor 7, a buffer tank 8 after the pump, an amine recovery kettle 9, an amine recovery tower 10 and an amine recovery condenser 11, wherein an outlet of the amination kettle 1 is connected with an inlet of the amination tower 2, a top outlet of the amination tower 2 is connected with a feed inlet of the primary condenser 3, a bottom discharge port of the primary condenser 3 is connected with a lateral line of the amination tower 2 through a pipeline, a top discharge port of the primary condenser 3 is connected with a feed inlet of the secondary condenser 4 through a pipeline, a bottom discharge port of the secondary condenser 4 is connected with the oil-water separator 5 through a pipeline, a top discharge port of the oil-water separator 5 and a bottom outlet pipeline of the primary condenser 3 are converged into a pipeline and then connected with the lateral line of the amination tower 2, a discharge port at the top of the secondary condenser 4 is connected with a post-pump buffer tank 8, the post-pump buffer tank 8 is sequentially connected with an amine compressor 7 and a pre-pump buffer tank 6, a discharge port of the pre-pump buffer tank 6 is divided into two branches, one branch is connected with the rectifying still, the other branch is connected with a feed port of the amination still 1, the feed port of the amination still 1 is connected with a feed pipe, the feed pipe extends to the bottom of the amination still 1, a water outlet at the lower end of the oil-water separator 5 is connected with an amine recovery still 9 through a pipeline, the amine recovery still 9 is sequentially connected with an amine recovery tower 10 and an amine recovery condenser 11, the amine recovery condenser 11 is connected with an air inlet pipe of the pre-pump buffer tank 6 in a converging manner, and the air inlet pipe is used for introducing nitrogen, hydrogen and dimethylamine; automatic regulating valves 12 are arranged on cold source feeding and discharging pipelines of the first-stage condenser 3 and the second-stage condenser 4 and used for controlling the flow of the cold source, automatic cut-off valves 13 are arranged on branches of the buffer tank 6 in front of the pump and the rectifying still, and automatic cut-off valves 13 are arranged on pipelines of the amine recovery condenser 11 and the air inlet pipe.
A process for producing low residual alcohol monoalkyl fatty tertiary amine comprises the following specific implementation modes: putting fatty alcohol and a catalyst into an amination kettle 1 in advance, then introducing hydrogen and nitrogen, heating, reducing the catalyst, introducing dimethylamine after reduction, heating the amination kettle 1, adjusting an automatic adjusting valve 12 to ensure that the temperature of circulating gas condensed by a primary condenser 3 is 120-140 ℃, the temperature of circulating gas condensed by a secondary condenser 4 is 30-50 ℃, heating the amination kettle 1 in stages for amination reaction, condensing the circulating gas in the reaction process by the primary condenser 3 and the secondary condenser 4 respectively, cooling and refluxing the fatty alcohol and the tertiary amine into the amination kettle 1 by the primary condenser 3, condensing water by the secondary condenser 4, introducing the water and uncondensed substances into an oil-water separator 5 for water-oil separation, wherein an upper oil layer is mainly the fatty alcohol and the tertiary amine and reflows into the amination kettle 1, and a lower layer is mainly a water layer containing the dimethylamine, and (3) the obtained product enters an amine recovery kettle 9 for recovering dimethylamine, the recovered dimethylamine flows back to an amination kettle 1, and the prepared crude product enters a rectifying kettle for refining.
Claims (7)
1. A system for producing low residual alcohol monoalkyl fatty tertiary amine is characterized by comprising an amination kettle (1), an amination tower (2), a multi-stage condensing device, an oil-water separator (5), a dimethylamine recovery device and a compression buffering device, wherein an outlet of the amination kettle (1) is connected with the amination tower (2), the amination tower (2) is circularly connected with the multi-stage condensing device, and the multi-stage condensing device is connected with a feeding hole of the amination kettle (1) through the compression buffering device to form a circulating loop; the multistage condensing device is connected with the oil-water separator (5), a water outlet at the lower end of the oil-water separator (5) is connected with the dimethylamine recovery device, and the dimethylamine recovery device is connected with a feed inlet of the amination kettle (1) through the compression buffer device to form another circulation loop.
2. The system for producing the low residual alcohol monoalkyl fatty tertiary amine according to claim 1, wherein the multistage condensing device comprises a first-stage condenser (3) and a second-stage condenser (4), the outlet of the amination tower (2) is connected with the feed inlet of the first-stage condenser (3), the bottom discharge outlet of the first-stage condenser (3) is connected with the side line of the amination tower (2) through a pipeline, the top discharge outlet of the first-stage condenser (3) is connected with the feed inlet of the second-stage condenser (4) through a pipeline, the bottom discharge outlet of the second-stage condenser (4) is connected with the oil-water separator (5) through a pipeline, the top discharge outlet of the oil-water separator (5) and the bottom outlet pipeline of the first-stage condenser (3) are converged into a pipeline and then connected with the side line of the amination tower (2), and the top discharge outlet of the second-stage condenser (4) is connected with the compression buffer device.
3. The system for producing the low residual alcohol monoalkyl fatty tertiary amine according to claim 2, wherein the compression buffering device comprises a pre-pump buffering tank (6), an amine compressor (7) and a post-pump buffering tank (8), a discharge port at the top of the secondary condenser (4) is connected with the post-pump buffering tank (8), the post-pump buffering tank (8) is sequentially connected with the amine compressor (7) and the pre-pump buffering tank (6), a discharge port of the pre-pump buffering tank (6) is divided into two branches, one branch is connected with the rectifying still, and the other branch is connected with a feed port of the amination still (1).
4. The system for producing the low residual alcohol monoalkyl fatty tertiary amine according to claim 3, wherein the dimethylamine recovery device comprises an amine recovery kettle (9), an amine recovery tower (10) and an amine recovery condenser (11), a water outlet at the lower end of the oil-water separator (5) is connected with the amine recovery kettle (9) through a pipeline, the amine recovery kettle (9) is sequentially connected with the amine recovery tower (10) and the amine recovery condenser (11), the amine recovery condenser (11) is connected with an air inlet pipe of the buffer tank (6) in front of the pump in a converging manner, and the air inlet pipe is used for introducing nitrogen, hydrogen and dimethylamine.
5. The system for producing low residual alcohol monoalkyl fatty tertiary amine according to claim 3, wherein the feed port of the amination kettle (1) is connected with a feed pipe, and the feed pipe extends to the bottom of the amination kettle (1).
6. The system for producing the tertiary amine with low residual alcohol monoalkyl fatty acid as claimed in claim 2, wherein the cold source inlet and outlet pipes of the primary condenser (3) and the secondary condenser (4) are provided with automatic regulating valves (12) for controlling the flow of the cold source.
7. The system for producing the low residual alcohol monoalkyl fatty tertiary amine according to claim 4, wherein an automatic cut-off valve (13) is arranged on a branch of the buffer tank (6) before the pump connected with the rectifying still, and an automatic cut-off valve (13) is arranged on a pipeline of the amine recovery condenser (11) connected with the air inlet pipe.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202123096313.6U CN216378008U (en) | 2021-12-10 | 2021-12-10 | System for producing low-residual alcohol monoalkyl fatty tertiary amine |
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| CN202123096313.6U CN216378008U (en) | 2021-12-10 | 2021-12-10 | System for producing low-residual alcohol monoalkyl fatty tertiary amine |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114105777A (en) * | 2021-12-10 | 2022-03-01 | 江苏万盛大伟化学有限公司 | Preparation method of low-residual alcohol monoalkyl fatty tertiary amine |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114105777A (en) * | 2021-12-10 | 2022-03-01 | 江苏万盛大伟化学有限公司 | Preparation method of low-residual alcohol monoalkyl fatty tertiary amine |
| CN114105777B (en) * | 2021-12-10 | 2024-03-12 | 江苏万盛大伟化学有限公司 | Preparation method of low-residual alcohol mono-alkyl fatty tertiary amine |
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