CN209836043U - Continuous production device for diethanol monoisopropanolamine - Google Patents

Continuous production device for diethanol monoisopropanolamine Download PDF

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CN209836043U
CN209836043U CN201920316731.5U CN201920316731U CN209836043U CN 209836043 U CN209836043 U CN 209836043U CN 201920316731 U CN201920316731 U CN 201920316731U CN 209836043 U CN209836043 U CN 209836043U
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liquid tank
pipeline
straight line
absorption tower
line section
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曾曼华
尹述柏
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HUBEI XIANLIN CHEMICAL INDUSTRY Co Ltd
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HUBEI XIANLIN CHEMICAL INDUSTRY Co Ltd
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Abstract

The utility model discloses a diethanol monoisopropanolamine continuous production device, including a jacket tubular reactor and a tail gas absorption tower, which is characterized in that the jacket tubular reactor is provided with a straight line section and a backflow section, the tail end of the straight line section is communicated with the head end of the backflow section, the head end of the backflow section is communicated with the head end of the straight line section through a control valve and forms an annular pipeline, the head end of the straight line section is provided with an axial flow propeller, and the straight line section is also provided with a diethanol amine inlet and an oxypropylene inlet; the jacketed tubular reactor is connected with a vacuum flash packed tower through a mass flow meter, and the top of the vacuum flash packed tower is connected with a vacuum ejector through the mass flow meter; the vacuum ejector is connected with the injection liquid tank; the mixed liquid outlet in the jet liquid tank is connected with the absorption liquid tank in the tail gas absorption tower through a pipeline. The utility model discloses guaranteed that diethanol monoisopropanolamine continuous production and to the yield and the purity of diethanol monoisopropanolamine all can reach higher requirement, production flexible operation, very big reduction workman intensity of labour, do benefit to extensive industrial production.

Description

Continuous production device for diethanol monoisopropanolamine
Technical Field
The utility model relates to a diethanol monoisopropanolamine chemical engineering technical field especially relates to an industrial diethanol monoisopropanolamine continuous production technology.
Background
Diethanol monoisopropanolamine, also known as 1- [ N, N-bis (2-hydroxyethyl) amino ] propan-2-ol, DEIPA for short, is a colorless or light yellow transparent viscous liquid with ammonia odor stimulation, and has stable properties at normal temperature and normal pressure.
The method is mainly used for industrially producing the diethanol monoisopropanolamine in a large scale in 2011 in China, the consumption field is mostly concentrated on a cement grinding aid, and the diethanol monoisopropanolamine is favored by grinding aids and concrete admixture enterprises in China due to the advantages of better adaptability and obvious strength enhancement in early and later periods of cement. The existing production process of diethanol monoisopropanolamine mainly has three routes: (1) a reaction route of ammonia with an epoxy olefin; (2) MIPA and EO reaction routes; (3) DEA and PO reaction route. Two preceding reaction routes need a lot of to throw material, purification many times because it needs a lot of to be reacted in series, its midway, and the equipment drops into big and the product quality that production obtained does not have the assurance, the utility model discloses a third kind route, but current industry DEA and PO reaction route production diethanol monoisopropanolamine adopt intermittent type formula production technology method more, and to the product quality uncontrollable that produces, operation workman's intensity of labour is great, can't guarantee the continuous stable production of product, and the final finished product purity that obtains is not high.
Disclosure of Invention
The utility model aims at providing a technology of the continuous large-scale production of diethanol monoisopropanolamine in industry to prior art's not enough, this production technology can be continuous stable going on, product quality is high, and the accessory substance is few, very big reduction workman intensity of labour, and the purity of the final diethanol monoisopropanolamine who obtains is up to more than 98%, does benefit to the large-scale production of industrialization.
The purpose of the utility model is realized through the following technical scheme: a continuous production device of diethanol monoisopropanolamine comprises a loop-clamping tube reactor and a tail gas absorption tower, and is characterized in that the loop-clamping tube reactor is provided with a straight line section and a backflow section, the tail end of the straight line section is communicated with the head end of the backflow section, the head end of the backflow section is communicated with the head end of the straight line section through a control valve and forms an annular pipeline, the head end of the straight line section is provided with an axial flow propeller, and the straight line section is also provided with a diethanol amine inlet and; the jacketed tubular reactor is connected with a vacuum flash packed tower through a mass flow meter, a diethanolamine monoisopropanolamine product outlet is arranged at the bottom of the vacuum flash packed tower, and the top of the vacuum flash packed tower is connected with a vacuum ejector through the mass flow meter; the vacuum ejector is connected with the injection liquid tank; the mixed liquid outlet in the jet liquid tank is connected with the absorption liquid tank in the tail gas absorption tower through a pipeline.
Preferably, the tail gas absorption tower comprises an absorption liquid tank and an absorption tower body, the top of the absorption liquid tank is connected with the bottom of the absorption tower body, a first-stage spray head and a second-stage spray head are arranged in the absorption tower, and the second-stage spray head is positioned below the first-stage spray head.
Preferably, an outlet at the bottom of the absorption liquid tank is connected with an inlet of a second conveying pump through a pipeline, an outlet of the second conveying pump is connected with a second-stage spray header in the tail gas absorption tower through a pipeline, an outlet at the bottom of the jet liquid tank is connected with an inlet of a third conveying pump through a pipeline, and an outlet of the third conveying pump is connected with a first-stage spray header in the tail gas absorption tower through a pipeline.
Preferably, the bottom outlet of the injection liquid tank is connected with the inlet of a first delivery pump through a pipeline, and the outlet of the first delivery pump is connected with a vacuum ejector through a pipeline.
Preferably, the tail gas absorption tower is internally provided with an absorption liquid collector, and the absorption liquid collector is connected with a reflux port of the injection liquid tank through a pipeline.
Borrow by above-mentioned scheme, the utility model discloses there is following advantage at least:
1) the jacket loop reactor is adopted, the heat exchange area of the jacket is large, the temperature of circulating water in the jacket is regulated in a segmented mode, and the segmented reaction temperature can be accurately controlled.
2) The loop reactor is formed by assembling and welding pipelines, has high pressure resistance, and is safe and reliable compared with a kettle reactor.
3) The reactor is fed and discharged continuously, accurate batching under DCS control can be realized, and compared with intermittent kettle type operation, the labor intensity is greatly reduced.
4) An axial flow propeller is arranged in the loop reactor, materials flow in an axial horizontal pushing mode, and a plurality of static mixers are arranged to ensure sufficient radial mixing. Compared with kettle type operation, the axial back mixing is less, and the side reaction is relatively reduced. Compared with a straight-through tubular reactor, the operation is more flexible.
5) The reaction temperature is controlled in a segmented mode, the temperature of the front section is low, the temperature of the rear section is high, side reactions can be reduced compared with kettle type operation, and the overall reaction speed is improved.
6) Vacuum flash evaporation and multi-stage absorption ensure that the surplus propylene oxide in the ingredients can be recycled.
Drawings
FIG. 1 is a schematic view of the process flow of the continuous production device for diethanol monoisopropanolamine in the production of the utility model.
Detailed Description
As shown in fig. 1, the apparatus for continuously producing diethanol monoisopropanolamine comprises a jacketed tubular reactor 3, a tail gas absorption column 13, and the like.
Wherein, a plurality of static mixers 4 are arranged in the jacket loop reactor 3, and an axial flow propeller 5 is arranged in the jacket loop reactor. The working principle of the static mixer is that fluid flows in a pipeline to impact various plate elements, the velocity gradient of laminar motion of the fluid is increased or turbulent flow is formed, the laminar flow is divided, moved and recombined, and in the turbulent flow, the fluid can generate violent vortex in the cross section direction besides the three conditions, and strong shearing force acts on the fluid to further divide and mix the fluid, and finally the fluid is mixed to form the required emulsion. So called "static" mixers, means that there are no moving parts in the pipe, only static elements.
The jacketed tubular reactor 3 allows the materials to be fully mixed, flow and react. The jacket loop reactor 3 is provided with a straight line section 3A and a backflow section 3B, the tail end of the straight line section 3A is communicated with the head end of the backflow section 3B, the head end of the backflow section is communicated with the head end of the straight line section 3A through a control valve 33 and forms an annular pipeline, the head end of the straight line section 3A is provided with an axial flow propeller 5, and the straight line section is further provided with a diethanolamine inlet 31 and an oxypropylene inlet 32.
And the diethanol amine is continuously metered by a mass flow meter 1, and the propylene oxide is continuously metered by a mass flow meter 2 and then flows into a double-ring pipe reactor 3. The liquid phase discharge port at the bottom of the vacuum flash packed tower 7 is connected with a mass flow meter 9. The liquid phase discharge is the diethanolamine monoisopropanolamine product, and can be removed to a product intermediate tank.
The jacketed tubular reactor is connected with a vacuum flash packed tower 7 through a mass flow meter 6, and a liquid diethanolamine monoisopropanolamine product is collected at an outlet at the bottom of the vacuum flash packed tower 7. The top of the vacuum flash packed tower 7 is connected with a vacuum ejector 11 through a mass flow meter 8. The vacuum ejector 11 is connected to an ejection liquid tank 12. The mixed liquid outlet of the injection liquid tank 12 is connected with the top of the absorption liquid tank 15A of the tail gas absorption tower 15 through a pipeline. And the unabsorbed residual gas phase in the mixed liquid is exhausted after being absorbed by the tail gas absorption tower 15 in two stages.
The tail gas absorption tower 15 comprises an absorption liquid tank 15A and an absorption tower body 15B, the top of the absorption liquid tank is connected with the bottom of the absorption tower body, a first-stage spray header 151 and a second-stage spray header 152 are arranged in the absorption tower, and the second-stage spray header is positioned below the first-stage spray header 151.
The tail gas absorption tower can also be provided with a leak tray-shaped absorption liquid collector 153 or other diversion trench-shaped collectors 153, the absorption liquid collector 153 collects part of absorption liquid, the absorption liquid collector is connected with the reflux port of the injection liquid tank 12 through a pipeline, and the pipeline is provided with a valve which can limit the reflux quantity according to actual needs.
The outlet at the bottom of the absorption liquid tank 15A is connected with the inlet of the second delivery pump 102 through a pipeline, and the outlet of the second delivery pump 102 is connected with the second-stage spray header 152 in the tail gas absorption tower through a pipeline. The liquid in the recovered absorption liquid tank can be used for preparing diethanolamine.
An outlet at the bottom of the injection liquid tank 12 is connected with an inlet of a third delivery pump 103 through a pipeline, and an outlet of the third delivery pump 103 is connected with a first-stage spray header 151 in the tail gas absorption tower through a pipeline. The first-stage spray header 151 on the top of the absorption tower can also be connected with other pipelines to inject deionized water. The bottom outlet of the injection liquid tank 12 is also connected with the inlet of a first delivery pump 101 through a pipeline, and the outlet of the first delivery pump 101 is connected with the vacuum ejector 11 through a pipeline.
The following examples and comparative descriptions of the process of the present invention
Examples 1 to 7
The method comprises the steps of preheating diethanolamine to 70-80 ℃ before entering a reactor, continuously metering the diethanolamine by a mass flowmeter 1, continuously metering propylene oxide by a mass flowmeter 2, flowing into a jacketed tubular reactor 3, wherein the molar ratio of the diethanolamine to the propylene oxide is 1:1.0-1.2, passing through internal parts such as a static mixer 4 and an axial flow propeller 5 in the jacketed tubular reactor 3, fully mixing, flowing and reacting materials, controlling the reaction temperature to be 75 ℃ at the front section, 95 ℃ at the rear section, and controlling the pressure to be 1.8-2 MPa. The reaction materials are pushed by an axial flow propeller 5 to circularly flow in the loop reactor, part of the reaction materials flow into a vacuum flash packed tower 7 after being measured by a mass flow meter 6, the liquid phase discharged from the bottom of the vacuum flash packed tower 7 is a diethanolamine monoisopropanolamine product, and the diethanolamine monoisopropanolamine product is removed from a product intermediate tank.
The gas phase discharged from the top of the vacuum flash packed tower 7 is mainly propylene oxide and water, and is intensively mixed with the injection liquid in the vacuum ejector 11, most of the injection liquid is absorbed and falls into the injection liquid tank 12 along with the injection liquid, and the unabsorbed residual gas phase is subjected to two-stage absorption in the tail gas absorption tower 15 and then is evacuated.
The absorption liquid can be used for preparing diethanolamine, and additional deionized water enters from the top of the absorption tower. By changing the molar ratio of the diethanolamine to the propylene oxide, the temperature of the circulating water in the jacket of the fixed-clamp loop reactor is kept constant, and the finished product of diethanolamine monoisopropanolamine is obtained. The test results are shown in table 1:
it can be seen from Table 1 that the yield and purity of the final product are changed with the change of the molar ratio of diethanolamine to propylene oxide, while the yield and purity are higher when the ratio is 1: 1.02-1.05.
Examples 8 to 14
Preheating diethanolamine to 70-80 ℃ before entering a reactor, continuously metering the diethanolamine by a mass flowmeter 1, continuously metering propylene oxide by a mass flowmeter 2, flowing into a jacketed tubular reactor 3, wherein the molar ratio of the diethanolamine to the propylene oxide is 1:1.02, fully mixing, flowing and reacting materials by internal components such as a static mixer 4, an axial flow propeller 5 and the like in the jacketed tubular reactor 3, controlling the reaction temperature to be 60-100 ℃, wherein the reaction temperature is 70-80 ℃ at the front section and 90-100 ℃ at the rear section. The pressure intensity is 1.8-2 MPa. The reaction materials are pushed by an axial flow propeller 5 to circularly flow in the loop reactor, part of the reaction materials flow into a vacuum flash packed tower 7 after being measured by a mass flow meter 6, the liquid phase discharged from the bottom of the vacuum flash packed tower 7 is a diethanolamine monoisopropanolamine product, and the diethanolamine monoisopropanolamine product is removed from a product intermediate tank. The gas phase discharged from the top of the vacuum flash packed tower 7 is mainly propylene oxide and water, and is intensively mixed with the injection liquid in the vacuum ejector 11, most of the injection liquid is absorbed and falls into the injection liquid tank 12 along with the injection liquid, and the unabsorbed residual gas phase is subjected to two-stage absorption in the tail gas absorption tower 15 and then is evacuated. The absorption liquid can be used for preparing diethanolamine, and additional deionized water enters from the top of the absorption tower. And controlling the temperature of circulating water in a jacket of the jacket loop reactor to change the temperature of the front end and the rear end of the circulating water so as to obtain a finished product of diethanolamine monoisopropanolamine. The test results are shown in Table 2
It can be seen from table 2 that the yield and purity of the final product vary with the temperature of the front and rear sections of the jacketed tubular reactor, and the yield and purity of the final product do not reach 90% when the temperature of the front section is lower than 70 ℃, but decrease when the temperature of the front section is higher than 80 ℃. It also drops when the back end temperature is below 90 ℃. Therefore, the yield and purity of the product can be judged to be higher when the front section is 70-80 ℃ and the rear section is 90-100 ℃.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although some descriptions are made with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (5)

1. A continuous production device of diethanol monoisopropanolamine comprises a loop-clamping tube reactor and a tail gas absorption tower, and is characterized in that the loop-clamping tube reactor is provided with a straight line section and a backflow section, the tail end of the straight line section is communicated with the head end of the backflow section, the head end of the backflow section is communicated with the head end of the straight line section through a control valve and forms an annular pipeline, the head end of the straight line section is provided with an axial flow propeller, and the straight line section is also provided with a diethanol amine inlet and; the jacketed tubular reactor is connected with a vacuum flash packed tower through a mass flow meter, a diethanolamine monoisopropanolamine product outlet is arranged at the bottom of the vacuum flash packed tower, and the top of the vacuum flash packed tower is connected with a vacuum ejector through the mass flow meter; the vacuum ejector is connected with the injection liquid tank; the mixed liquid outlet in the jet liquid tank is connected with the absorption liquid tank in the tail gas absorption tower through a pipeline.
2. The apparatus for continuously producing diethanol monoisopropanolamine according to claim 1, characterized in that: the tail gas absorption tower comprises an absorption liquid tank and an absorption tower body, the top of the absorption liquid tank is connected with the bottom of the absorption tower body, a first-stage spray head and a second-stage spray head are arranged in the absorption tower, and the second-stage spray head is located below the first-stage spray head.
3. The apparatus for continuously producing diethanol monoisopropanolamine according to claim 1, characterized in that: the bottom outlet of the absorption liquid tank is connected with the inlet of a second conveying pump through a pipeline, the outlet of the second conveying pump is connected with a second-stage spray head in the tail gas absorption tower through a pipeline, the bottom outlet of the jet liquid tank is connected with the inlet of a third conveying pump through a pipeline, and the outlet of the third conveying pump is connected with a first-stage spray head in the tail gas absorption tower through a pipeline.
4. The apparatus for continuously producing diethanol monoisopropanolamine according to claim 1, characterized in that: and an outlet at the bottom of the injection liquid tank is connected with an inlet of a first conveying pump through a pipeline, and an outlet of the first conveying pump is connected with a vacuum ejector through a pipeline.
5. The apparatus for continuously producing diethanol monoisopropanolamine according to claim 1, characterized in that: and an absorption liquid collector is arranged in the tail gas absorption tower and is connected with a reflux port of the injection liquid tank through a pipeline.
CN201920316731.5U 2019-03-13 2019-03-13 Continuous production device for diethanol monoisopropanolamine Active CN209836043U (en)

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Application Number Priority Date Filing Date Title
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PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of utility model: A continuous production device of diethanol monoisopropanolamine

Effective date of registration: 20220125

Granted publication date: 20191224

Pledgee: Bank of China Limited Xiantao branch

Pledgor: HUBEI XIANLIN CHEMICAL CO.,LTD.

Registration number: Y2022420000029

PE01 Entry into force of the registration of the contract for pledge of patent right