CN210261603U - N-methyldiethanolamine production device - Google Patents
N-methyldiethanolamine production device Download PDFInfo
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- CN210261603U CN210261603U CN201920772433.7U CN201920772433U CN210261603U CN 210261603 U CN210261603 U CN 210261603U CN 201920772433 U CN201920772433 U CN 201920772433U CN 210261603 U CN210261603 U CN 210261603U
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Abstract
The utility model discloses a N-methyldiethanolamine production device, including one-level blender, second grade blender, reactor, evaporate amine tower, dehydration tower, initiator jar, secondary amine tower and product refining tower. The utility model discloses the unit that exists to present N-methyldiethanolamine production technology is high, the separation process is complicated, product purity hangs down the scheduling problem, new apparatus for producing and refined technology have been developed, product N-methyldiethanolamine purity improves to 99.8% from 95%, ethylene oxide unit consumption falls to 0.75-0.8 from 0.95-1.0, monomethylamine unit consumption falls to 0.26-0.30 from 0.4-0.45, intermediate product and unreacted monomethylamine and a small amount of ethylene oxide that the in-process produced all recycle completely through the separation, the material consumption has been reduced, the waste liquid that has also significantly reduced is discharged.
Description
Technical Field
The utility model belongs to the technical field of petrochemical, concretely relates to N-methyldiethanolamine's apparatus for producing.
Background
N-Methyldiethanolamine (MDEA) is colorless or pale yellow oily liquid, is weakly alkaline, has excellent selectivity and thermal stability, and has low vapor pressure. When the acidic gas is treated, the gas phase loss is small, the corrosion to the device is slight, and the method is suitable for treating natural gas, synthesis gas, refinery gas, Claus sulfur tail gas and the like. Meanwhile, H2S can be selectively removed from H2S and CO2 gases, and the method is particularly suitable for treating gases with high volume ratio of CO2 to H2S, widely replaces other amine solutions frequently used in the field of gas purification, and has a very wide market prospect. MDEA is also useful as a pesticide, emulsifier, or pharmaceutical intermediate.
At present, the industrial production of N-methyldiethanolamine mainly adopts the reaction of ethylene oxide and excessive monomethylamine, and the ethylene oxide is relatively active and can easily react with monomethylamine. However, as the temperature rises, the selectivity and the byproducts of the reaction change along with the change of the temperature; on the one hand, the alcohol amine substance is generated to generate a byproduct by dehydration condensation, and on the other hand, the ethylene oxide is polymerized by itself. In addition, the prior art mostly adopts an alkaline catalyst, which causes difficulty in separation and purification of products.
SUMMERY OF THE UTILITY MODEL
Utility model purpose: the utility model aims to provide a production device of N-methyldiethanolamine against the deficiency of the prior art.
The technical scheme is as follows: the utility model relates to a production device of N-methyldiethanolamine, which comprises a primary mixer, a secondary mixer, a reactor, an amine steaming tower, a dehydrating tower, an initiator tank, a secondary amine tower and a product refining tower; the first-stage mixer is provided with a feed inlet and a discharge outlet, the second-stage mixer is provided with a feed inlet and a discharge outlet, the discharge outlet of the first-stage mixer is connected with the feed inlet of the second-stage mixer, the discharge outlet of the second-stage mixer is connected with the feed inlet of the reactor, the discharge outlet of the reactor is connected with the middle feed inlet of the amine steaming tower, the top of the amine steaming tower is provided with a tower top discharge outlet, the bottom of the amine steaming tower is provided with a tower bottom discharge outlet, the tower bottom of the amine steaming tower is provided with a tower bottom discharge outlet, the top of the amine steaming tower is connected with the middle feed inlet of the first-stage mixer, the bottom of the amine steaming tower is connected with the middle feed inlet of the dehydrating tower, the dehydrating tower is provided with a tower top discharge outlet and a tower bottom discharge outlet, the bottom, the device comprises a secondary amine tower, a dehydration tower, a secondary amine tower, a tower bottom discharge port, a tower top discharge port, a secondary amine tower, a tower bottom discharge port, a secondary amine tower, a dehydration tower, a side line extraction port, a tower top discharge port, a tower bottom discharge port and a product refining tower, wherein the tower bottom discharge port is connected with the middle feed port of the secondary amine tower.
Preferably, the reactor is a tubular reactor, the working temperature is 90-150 ℃, and the operating pressure is 2.5-5.0 MPa.
Preferably, the number of theoretical plates of the amine distillation tower is 10-15, and the operating pressure is 0.4-0.6 MPa.
Preferably, the number of theoretical plates of the dehydration tower is 10-15, and the operating pressure is 0.1-0.3 MPa.
Preferably, the number of theoretical plates of the secondary amine tower is 10-15, the side draw is 2-5 theoretical plates, and the operating pressure is 0-0.01 MPa.
Preferably, the number of theoretical plates of the product refining tower is 15-23, the side extraction outlet is at the 6 th-10 th theoretical plate, and the operating pressure is 0-0.01 MPa.
A production process for N-methyldiethanolamine by using the production device comprises the following steps:
1) liquefied monomethylamine and ethylene oxide enter a primary mixer from a feed inlet of the primary mixer, are mixed, are extracted from a discharge outlet of the primary mixer, and enter a feed inlet of a secondary mixer;
2) part of the materials extracted from the top of the dehydration tower and the materials extracted from the side line extraction outlet of the secondary amine tower enter the feed inlet of a secondary mixer through the discharge outlet of an initiator tank, are mixed with the materials extracted in the step 1), and are extracted from the discharge outlet of the secondary mixer;
3) feeding the material extracted from the discharge port of the secondary mixer in the step 2) into a reactor from a feed port of the reactor for reaction, and extracting the reacted material from the discharge port of the reactor;
4) feeding the material extracted in the step 3) into an amine evaporation tower from an amine evaporation tower feeding hole, performing reduced pressure rectification, extracting unreacted monomethylamine from an amine evaporation tower ejection material hole, returning to a first-stage mixer feeding hole after condensation, participating in reacting light components extracted from the amine evaporation tower ejection material hole again, wherein condensed noncondensable gas contains trace monomethylamine and ethylene oxide, and feeding the gas into an absorption working section for absorption post-treatment, wherein heavy components are extracted from an amine evaporation tower bottom material hole;
5) feeding the heavy components extracted in the step 4) into a dehydration tower from a feed inlet of the dehydration tower, performing reduced pressure rectification, extracting water and a small amount of undelivered monomethylamine from a discharge outlet at the top of the dehydration tower, feeding the majority of the water and the small amount of undelivered monomethylamine into an initiator tank from a feed inlet of the initiator tank, feeding the small amount of the water and the small amount of undelivered monomethylamine into an absorption section for absorbing trace monomethylamine and ethylene oxide in the non-condensable gas generated in the step 3), and extracting the heavy components from a discharge;
6) feeding the heavy component extracted in the step 5) into a secondary amine tower from a feeding hole of the secondary amine tower, performing reduced pressure rectification, extracting a small amount of N-methylethanolamine and water which is not completely removed in a dehydration tower from a top discharging hole of the secondary amine tower, feeding the small amount of N-methylethanolamine into an initiator tank from a feeding hole of the initiator tank, extracting a large amount of N-methylethanolamine from a side line extracting hole of the secondary amine tower, feeding the large amount of N-methylethanolamine into the initiator tank from the feeding hole of the initiator tank, feeding the small amount of N-methylethanolamine into an absorption working section for absorbing a small amount of monomethylamine and ethylene oxide in the non-condensable gas generated in the step 3;
7) and (3) introducing heavy components extracted in the step 6) into a product refining tower from a feed inlet of the product refining tower, after rectification under reduced pressure, extracting a small amount of N-methyldiethanolamine and N-methylethanolamine which is not completely removed in a secondary amine tower from a feed outlet of the product refining tower, returning the N-methyldiethanolamine to the secondary amine tower from the feed inlet of the secondary amine tower for continuous separation, extracting a large amount of N-methyldiethanolamine from a side line extraction outlet of the product refining tower, storing the large amount of N-methyldiethanolamine in a product tank, returning the small amount of N-methyldiethanolamine to the secondary amine tower from the feed inlet of the secondary amine tower for controlling the feeding composition of the secondary amine tower, and extracting a small.
Has the advantages that: (1) the reactor in the utility model adopts a tubular reactor and a series of rectifying towers which are connected in series, the reaction process can be controlled by adjusting the reaction temperature and the pressure, the side reaction is reduced, the yield of the target product is improved, the unreacted materials are recycled after being separated, and the unit consumption of raw materials is reduced; the purity of the product N-methyldiethanolamine is improved from 95 percent to 99.8 percent, the unit consumption of the ethylene oxide is reduced from 0.95 to 1.0 to 0.75 to 0.8, the unit consumption of the monomethylamine is reduced from 0.4 to 0.45 to 0.26 to 0.30, and the intermediate product generated in the process, the unreacted monomethylamine and a small amount of ethylene oxide are completely recycled by separation, so the material consumption is reduced, and the waste liquid discharge is greatly reduced;
(2) the utility model utilizes the intermediate product N-methylethanolamine as a catalyst and is matched with a small amount of water, the N-methylethanolamine produced in the reaction process is extracted through a top discharging port of a secondary amine tower, the water added in the primary reaction is extracted through a top discharging port of a dehydrating tower, and the N-methylethanolamine and the water enter a secondary mixer to participate in the reaction again after passing through an initiator tank in a circulating manner, thereby not only improving the utilization rate of raw materials, but also avoiding bringing in new substances, and reducing the energy consumption for separation and the equipment investment;
(3) the utility model discloses a set up the side draw mouth at the well upper portion of secondary amine tower, adopt a large amount of N-methyl ethanolamine to and upper portion sets up the side draw mouth in the product refining tower, adopts a large amount of N-methyl diethanolamine, and separates the few accessory substances that produce the reaction from the product, can obtain higher purity N-methyl diethanolamine.
Drawings
Fig. 1 is a schematic view of the process flow of the present invention.
In the figure, 1-a first-stage mixer, 2-a second-stage mixer, 3-a reactor, 4-an amine distilling tower, 5-a dehydrating tower, 6-an initiator tank, 7-a secondary amine tower and 8-a product refining tower.
Detailed Description
The technical solution of the present invention is described in detail below with reference to the accompanying drawings, but the scope of the present invention is not limited to the embodiments.
Example (b): a production device of N-methyldiethanolamine comprises a primary mixer 1, a secondary mixer 2, a reactor 3, an amine steaming tower 4, a dehydrating tower 5, an initiator tank 6, a secondary amine tower 7 and a product refining tower 8; the primary mixer 1 is provided with a feeding hole and a discharging hole, the secondary mixer 2 is provided with a feeding hole and a discharging hole, the discharging hole of the primary mixer 1 is connected with the feeding hole of the secondary mixer 2, the discharging hole of the secondary mixer 2 is connected with the feeding hole of the reactor 3, the reactor 3 is a tubular reactor 3, the working temperature is 90-150 ℃, the operating pressure is 2.5-5.0 MPa, the reactor 3 is provided with a discharging hole, the discharging hole of the reactor 3 is connected with the middle feeding hole of the amine steaming tower 4, the amine steaming tower 4 is provided with 10-15 theoretical plates, the operating pressure is 0.4-0.6 MPa, the top of the amine steaming tower 4 is provided with a top discharging hole, the bottom of the tower is provided with a bottom discharging hole, the top discharging hole of the amine steaming tower 4 is connected with the feeding hole of the primary mixer 1, the bottom discharging hole of the amine steaming tower 4 is connected with the middle feeding hole of the dehydrating tower 5, the dehydrating tower 5 is provided with 10-15 theoretical plates, the dehydration tower 5 is provided with a tower top discharge hole and a tower bottom discharge hole, the tower bottom discharge hole of the dehydration tower 5 is connected with a middle feed inlet of a secondary amine tower 7, the secondary amine tower 7 is provided with 10-15 theoretical plates, a side line extraction hole is arranged between 2 th theoretical plate and 5 th theoretical plate, the operation pressure is 0-0.01 MPa, the middle upper part of the secondary amine tower 7 is provided with a side line extraction hole, the tower top discharge hole is arranged at the tower top, the tower bottom discharge hole of the secondary amine tower 7 is connected with a middle feed inlet of a product refining tower 8, the tower top discharge hole of the secondary amine tower 7 and the tower top discharge hole of the dehydration tower 5 are connected with a top feed inlet of an initiator tank 6 together, the bottom discharge hole of the initiator tank 6 is connected with a feed inlet of a secondary mixer 2, the middle upper part of the product refining tower 8 is provided with a side, and in the product refining tower 8, the number of theoretical plates is 15-23, a lateral line extraction port is arranged on the 6 th-10 th theoretical plate, and the operating pressure is 0-0.01 MPa.
A production process for N-methyldiethanolamine by using the production device comprises the following steps:
a. liquefied monomethylamine and ethylene oxide are mixed in a first-stage mixer 1 according to the mass ratio of 1.5: 1.
b. N-methylethanolamine and water from the initiator tank 6 are used as reaction catalysts and enter the secondary mixer 2 together with reaction raw materials for mixing;
c. the mixed materials enter a reactor 3 from a feed inlet of the reactor 3 for reaction, the reactor 3 is a tubular reactor 3 consisting of a plurality of sections of straight pipes, the length of the pipe ensures that the residence time of the materials is 7-10min, each section of straight pipe is provided with a jacket, media such as steam, hot water and the like can be introduced to control the temperature in a segmented manner, the reaction temperature is controlled to be about 90 ℃, the pressure is 5.5MPa, the reaction time is 7.5min, the propylene oxide is completely reacted, the conversion rate of monomethylamine is 66.7%, the selectivity of N-methyldiethanolamine is 99.1%, and the materials after the reaction are extracted from a discharge outlet of the reactor;
d. feeding the reacted materials into an amine steaming tower 4, wherein the amine steaming tower 4 is a scattered pall ring packed tower, 10 theoretical plates are provided in total, the feeding position is a 5 th plate, the operating pressure is 0.5MPa, after reduced pressure rectification, unreacted monomethylamine is extracted from a discharge port at the top of the amine steaming tower 4, the unreacted monomethylamine is condensed and then returns to a feeding port of a first-stage mixer to participate in the reaction again, noncondensable gas is sent to an absorption working section to absorb trace monomethylamine and ethylene oxide in the unreacted monomethylamine, and heavy components are extracted from a discharge port at the bottom of the amine steaming tower 4;
e. heavy components extracted from an amine distillation tower 4 are sent into a dehydration tower 5, the dehydration tower 5 adopts pore plate corrugated packing, 12 theoretical plates are totally adopted, the feeding position is the 6 th plate, the operating pressure is 0.025MPa, after reduced pressure rectification, water generated by side reaction, water used as a catalyst, N-methylethanolamine and a small amount of undepleted monomethylamine are extracted from a discharge port at the top of the dehydration tower 5, most of condensed heavy components are sent into an initiator tank 6 and then returned to a secondary mixer 2 to continue to participate in the reaction, a small part of condensed heavy components are used as absorption liquid to enter an absorption working section, and heavy components are extracted from a discharge port at the bottom of the dehydration tower 5;
f. sending heavy components extracted by a dehydrating tower 5 into a secondary amine tower 7, wherein the secondary amine tower 7 adopts a pore plate corrugated packing, 12 theoretical plates are provided, the feeding position is the 8 th plate, the side line extraction outlet is the 4 th plate, the operation pressure is 0.001MPa, after reduced pressure rectification, a small amount of N-methylethanolamine and water which is not completely removed in the dehydrating tower 5 are extracted from a discharge hole at the top of the secondary amine tower 7, after condensation, the N-methylethanolamine is sent into an initiator tank 6 and then returned to a secondary mixer 2 to continue to participate in reaction, a large amount of N-methylethanolamine is extracted from the side line extraction outlet of the secondary amine tower 7, most of N-methylethanolamine is sent into the initiator tank 6 and then returned to the secondary mixer 2 to continue to participate in reaction, a small amount of N-methylethanolamine enters an absorption working section as absorption;
g. heavy components extracted from a secondary amine tower 7 are sent into a product refining tower 8, the product refining tower 8 adopts wire mesh corrugated packing, 15 theoretical plates are used totally, the feeding position is the 11 th plate, the lateral extraction port is the 8 th plate, the operating pressure is 0.001MPa, after reduced pressure rectification, a small amount of N-methyldiethanolamine and N-methylethanolamine which is not completely removed in the secondary amine tower 7 are extracted from a discharge port at the top of the product refining tower 8, the N-methyldiethanolamine returns to the secondary amine tower 7 to be continuously separated, a large amount of N-methyldiethanolamine is extracted from the lateral extraction port of the product refining tower 8, the purity can reach 99.8%, the majority of N-methyldiethanolamine is stored in a product tank, the minority of N-methyldiethanolamine returns to the secondary amine tower 7 to be used for adjusting the feeding composition of the secondary amine tower 7, and a small.
According to the embodiment, the production of N-methyldiethanolamine is carried out, the unit consumption of ethylene oxide is 0.75, the unit consumption of monomethylamine is 0.26, the conversion rate of ethylene oxide is close to 100%, the selectivity of N-methyldiethanolamine is 99.1%, the product purity can reach 99.8%, in the process, except a small amount of byproducts, the unreacted monomethylamine and N-methylethanolamine are recycled, and trace monomethylamine and ethylene oxide possibly existing in non-condensable gas can be recycled after being fully absorbed by an absorption section, so that waste gas is not generated.
As mentioned above, although the present invention has been shown and described with reference to certain preferred embodiments, it should not be construed as limiting the invention itself. Various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. A production device of N-methyldiethanolamine is characterized by comprising a primary mixer, a secondary mixer, a reactor, an amine steaming tower, a dehydrating tower, an initiator tank, a secondary amine tower and a product refining tower; the first-stage mixer is provided with a feed inlet and a discharge outlet, the second-stage mixer is provided with a feed inlet and a discharge outlet, the discharge outlet of the first-stage mixer is connected with the feed inlet of the second-stage mixer, the discharge outlet of the second-stage mixer is connected with the feed inlet of the reactor, the discharge outlet of the reactor is connected with the middle feed inlet of the amine steaming tower, the top of the amine steaming tower is provided with a tower top discharge outlet, the bottom of the amine steaming tower is provided with a tower bottom discharge outlet, the tower bottom of the amine steaming tower is provided with a tower bottom discharge outlet, the top of the amine steaming tower is connected with the middle feed inlet of the first-stage mixer, the bottom of the amine steaming tower is connected with the middle feed inlet of the dehydrating tower, the dehydrating tower is provided with a tower top discharge outlet and a tower bottom discharge outlet, the bottom, the device comprises a secondary amine tower, a dehydration tower, a secondary amine tower, a tower bottom discharge port, a tower top discharge port, a secondary amine tower, a tower bottom discharge port, a secondary amine tower, a dehydration tower, a side line extraction port, a tower top discharge port, a tower bottom discharge port and a product refining tower, wherein the tower bottom discharge port is connected with the middle feed port of the secondary amine tower.
2. The apparatus for producing N-methyldiethanolamine as claimed in claim 1, wherein the reactor is a tubular reactor, the working temperature is 90 ℃ to 150 ℃, and the operating pressure is 2.5MPa to 5.0 MPa.
3. The apparatus for producing N-methyldiethanolamine as claimed in claim 1, wherein the number of theoretical plates of the amine evaporation tower is 10-15, and the operating pressure is 0.4-0.6 MPa.
4. The apparatus for producing N-methyldiethanolamine as claimed in claim 1, wherein the number of theoretical plates of the dehydration tower is 10-15, and the operating pressure is 0.1-0.3 MPa.
5. The apparatus for producing N-methyldiethanolamine as claimed in claim 1, wherein the number of theoretical plates of the secondary amine tower is 10-15, the side draw is from 2 to 5 theoretical plates, and the operating pressure is 0-0.01 MPa.
6. The production device of N-methyldiethanolamine as claimed in claim 1, wherein the number of theoretical plates of the product refining tower is 15-23, the side draw is on the 6 th-10 th theoretical plate, and the operating pressure is 0-0.01 MPa.
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| CN201920772433.7U CN210261603U (en) | 2019-05-27 | 2019-05-27 | N-methyldiethanolamine production device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113185413A (en) * | 2021-04-28 | 2021-07-30 | 宁波乐维实业有限公司 | Processing technology of mixed amine |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113185413A (en) * | 2021-04-28 | 2021-07-30 | 宁波乐维实业有限公司 | Processing technology of mixed amine |
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