CN112619588A - Tertiary amine production device and production method thereof - Google Patents
Tertiary amine production device and production method thereof Download PDFInfo
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- CN112619588A CN112619588A CN202011386022.8A CN202011386022A CN112619588A CN 112619588 A CN112619588 A CN 112619588A CN 202011386022 A CN202011386022 A CN 202011386022A CN 112619588 A CN112619588 A CN 112619588A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/26—Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D45/00—Separating dispersed particles from gases or vapours by gravity, inertia, or centrifugal forces
- B01D45/04—Separating dispersed particles from gases or vapours by gravity, inertia, or centrifugal forces by utilising inertia
- B01D45/08—Separating dispersed particles from gases or vapours by gravity, inertia, or centrifugal forces by utilising inertia by impingement against baffle separators
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/04—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups
- C07C209/14—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups by substitution of hydroxy groups or of etherified or esterified hydroxy groups
- C07C209/16—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups by substitution of hydroxy groups or of etherified or esterified hydroxy groups with formation of amino groups bound to acyclic carbon atoms or to carbon atoms of rings other than six-membered aromatic rings
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/86—Separation
Abstract
The invention discloses a production device of tertiary amine, which comprises an evaporator, a circulating pump, an amination reactor, a gas-liquid separator, a cooler A, a cooler B, an oil-water separator, a buffer tank, a recovery kettle and a heat exchanger; according to the invention, a gas-liquid separator filled with metal corrugated filler is arranged on a circulating gas pipeline of an amination reactor, oil phase separated in an oil-water separator is sprayed above the gas-liquid separator and carries out reverse heat exchange with gas phase in the gas-liquid separator, heavy component oil phase is condensed and flows back to the reactor, and uncondensed gas continuously passes through a cooler A and a cooler B. The invention also provides a method for producing tertiary amine by using the device. The production device and the production method of the tertiary amine have the advantages of good oil-water separation effect, shortened reaction time and improved yield.
Description
Technical Field
The invention relates to the technical field of tertiary amine production, in particular to a production device and a production method of tertiary amine.
Background
The single long-chain alkyl tertiary amine is an important aliphatic alcohol amine, particularly the tertiary amine with the carbon chain length of C8-C18, is mainly used for producing raw materials of cationic surfactants, zwitterionic surfactants and amine oxide, and has irreplaceable effects in the fields of sterilization, fabric softening, washing, foam increasing, static resistance, metal slow release and the like. In the prior art, the production method of tertiary amine mainly comprises the following steps: halogenated amination method and fatty alcohol catalytic amination method, the halogenated amination method has the problems of equipment corrosion, environmental pollution and the like, the product quality is not high, and the method is basically eliminated.
The process for preparing tertiary amine by directly catalyzing and aminating fatty alcohol is widely applied due to the advantages of short process route, less equipment investment, basically no three-waste discharge, high product quality and the like. The reaction equation for this reaction is:
the fatty alcohol catalyzes the amination reaction to produce tertiary amine and water. The reaction is endothermic and requires continuous removal of water generated in the system to promote equilibrium of the reaction to the right. The water generated in the reaction needs to be taken out and separated by the circulating gas in the system in the production.
The conventional tertiary amine production system is shown in fig. 2, wherein a mixed gas of tertiary amine, water and the like generated by the reaction of the amination reactor 100 enters the recycle gas heat exchanger 200 through a gas phase pipeline for heat exchange, most of the tertiary amine in the gas phase is condensed and enters the tertiary amine separator 400 together with the mixed gas, the condensed tertiary amine flows back to the amination reactor 100 along a pipeline at the bottom of the tertiary amine separator 400, the uncondensed mixed gas enters the recycle gas cooler 800 through the gas phase pipeline for cooling by cooling water and then enters the oil-water separator 500, the fatty alcohol, the tertiary amine and the water vapor in the mixed gas are substantially condensed and are layered up and down in the oil-water separator 500 (the water is at the lower oil layer), the lower reaction water flows into the reaction water metering tank 600 through an overflow pipe depending on the design of the process pipeline, and the upper oil phase flows back to the bottom of the amination reactor 100 through the overflow pipe. The reaction water metering tank 600 has steam heating energy to evaporate the dimethylamine dissolved in the reaction water, and the reaction water metering tank 600 has a cooler to condense the volatilized water vapor, so as to prevent the water vapor from entering the system. The evaporated dimethylamine and fresh dimethylamine (vaporized by dimethylamine vaporizer 700) enter into the circulating gas heat exchanger 200 together for heat exchange and temperature rise, then enter into the circulating gas preheater 300 for heating to the temperature required by the reaction, and then enter into the amination reactor 100 for reaction.
The existing tertiary amine production system has the following defects:
(1) the mixed gas in the oil-water separation process contains materials seriously, so that the liquid level of the amination reactor 100 is reduced;
(2) the pressure of the amination reactor 100 is high, and as the pressure of the circulating gas is gradually reduced by condensation, pressure difference exists, so that liquid phases separated by the tertiary amine separator 400 and the oil-water separator 500 cannot smoothly flow back to the amination reactor 100, and the liquid levels of the tertiary amine separator 400 and the oil-water separator 500 are continuously increased;
(3) the mixed gas condensate enters the oil-water separator 500 from the upper part, and an oil-water mixture entering the oil-water separator 500 is automatically layered depending on the density of the oil-water mixture, so that the efficiency is low, the layering is not thorough, and a large amount of materials are contained in the separated water;
(4) the amination reactor 100 catalyzed by the fatty alcohol adopts a stirred tank reactor, and mass transfer obstacles between gas phase, liquid phase and solid phase exist. Poor mass transfer results in long reaction times and poor reaction quality.
Therefore, the liquid level of the reactor is reduced due to the fact that a large amount of fatty alcohol and tertiary amine are carried in circulating gas of the existing tertiary amine reaction system, the positive reaction is influenced due to poor water separation effect, byproducts are increased due to low reaction efficiency due to poor catalyst effect, and the production quality and efficiency of the tertiary amine are seriously influenced. Therefore, a reaction device and a production method with good oil-water separation effect, high yield and high quality of produced tertiary amine are needed to overcome the defects.
Disclosure of Invention
In order to solve the problems, the invention provides a production device and a production method of tertiary amine, which have the advantages of good oil-water separation effect, shortened reaction time and improved yield.
In order to achieve the purpose, the invention adopts the technical scheme that: a production device of tertiary amine comprises an evaporator, a circulating pump, an amination reactor, a gas-liquid separator, a cooler A, a cooler B, an oil-water separator, a buffer tank, a recovery kettle and a heat exchanger;
a feeding port of the evaporator is communicated with a dimethylamine input pipeline, dimethylamine is evaporated in the evaporator to form dimethylamine steam, and a gas outlet of the evaporator is communicated with a dimethylamine steam output pipeline;
the material inlet of the amination reactor is communicated with an aliphatic alcohol input pipeline, a Venturi tube is arranged in the amination reactor, a nozzle above the Venturi tube is communicated with a material outlet of a heat exchanger through a pipeline, the material inlet of the heat exchanger is communicated with a material outlet of a circulating pump through a pipeline, a material outlet at the bottom of the amination reactor is communicated with a material inlet of the circulating pump through a pipeline, a material outlet at the side end of the amination reactor is communicated with a tertiary amine finished product output pipeline, a gas outlet at the top of the amination reactor is communicated with a gas inlet of a gas-liquid separator through a pipeline, a material outlet at the bottom of the gas-liquid separator is communicated with the material inlet at the top of the amination reactor through a pipeline, a gas outlet at the top of the gas-liquid separator is communicated with a gas inlet of a cooler A through a pipeline, a gas, the side gas outlet of buffer tank is equipped with noncondensable gas output line, noncondensable gas output line with dimethylamine steam output line assembles the back with amination reactor's venturi inhales the chamber and is linked together, noncondensable gas output line and dimethylamine steam output line are linked together with nitrogen gas input pipeline and hydrogen input pipeline in addition simultaneously, the bottom discharge mouth of buffer tank pass through the pipeline with it is linked together to retrieve the cauldron, cooler A and cooler B's bottom discharge mouth respectively through condensed liquid output line with oil water separator side pan feeding mouth is linked together, the discharge gate on oil water separator top with the pan feeding mouth on gas water separator top passes through the pipeline and is linked together, oil water separator's bottom discharge mouth with it is linked together through the pipeline to retrieve the pan feeding mouth on cauldron top.
Further, retrieve the inside of cauldron and be equipped with heating coil, heat the water in retrieving the cauldron, and the bottom air inlet of retrieving the cauldron is linked together with vapor input pipeline, lets in vapor in retrieving the cauldron, heats the water in retrieving the cauldron, and the discharge gate is linked together with comdenstion water output pipeline, with comdenstion water discharge, retrieves the cauldron top and is equipped with the water cooler, prevents that vapor from volatilizing, water cooler top gas outlet through dimethylamine recovery pipeline with not condensed gas output pipeline is linked together.
Furthermore, the cooler A, the cooler B and the water cooler are respectively communicated with the cooling water inlet pipeline and the cooling water outlet pipeline simultaneously.
Further, a valve A is arranged between a discharge hole at the bottom of the amination reactor and an inlet of the circulating pump.
Further, a valve B is arranged between the circulating pump and the heat exchanger.
Furthermore, the gas-liquid separator is filled with a metal corrugated filler for realizing oil-water separation.
Further, the positions of the coolers A and B are higher than the gas-liquid separator.
The present invention further provides a process for producing a tertiary amine using the apparatus for producing a tertiary amine, which comprises the steps of:
mixing fatty alcohol and catalyst in a proportioning tank, pumping into an amination reactor from a fatty alcohol input pipeline, starting a circulating pump to establish self circulation of the amination reactor, heating an evaporator by hot water to vaporize dimethylamine to generate dimethylamine steam, forming local vacuum when the fatty alcohol and the catalyst flow through a Venturi tube above the amination reactor to suck the vaporized dimethylamine steam into the amination reactor and take part in reaction, feeding tertiary amine and the water steam generated by the reaction into a gas-liquid separator filled with metal corrugated filler through a pipeline to perform gas-liquid separation, feeding the liquid separated by condensation back to the amination reactor through a pipeline below the gas-liquid separator, feeding the gas which is not condensed into a cooler A through a pipeline, further condensing the gas, feeding the gas which is not condensed into a cooler B through a pipeline, condensing the gas again, feeding the gas which is not condensed into a buffer tank, returning to the upper part of the amination reactor through an uncondensed gas output pipeline, and sucking the gas above the amination reactor together with dimethylamine steam into the amination reactor; the condensed liquids in the cooler A and the cooler B are respectively converged together through a condensed liquid output pipeline and flow into an oil-water separation tank for oil-water separation, the oil is on the upper layer, the water is on the lower layer, the water flows out from the bottom of the oil-water separation tank to a recovery kettle, the recovery kettle is heated by water vapor, dimethylamine dissolved in the water is separated from the water after being heated, the evaporated dimethylamine condenses the volatilized water vapor through a water cooler, and the separated dimethylamine returns to an amination reactor through a dimethylamine recovery pipeline to continuously participate in the reaction;
meanwhile, the oil in the oil-water separator is sprayed above the gas-liquid separator after being pressed to the gas-liquid separator, and carries out reverse heat exchange with the gas phase in the gas-liquid separator, and the heavy component oil phase is condensed and flows back to the amination reactor. The tertiary amine finished product is continuously generated along with the addition of the fatty alcohol and the dimethylamine and overflows from an output pipeline of the tertiary amine finished product of the amination reactor.
Further, the adding amount of the catalyst is 3 per mill of the mass of the fatty alcohol.
Further, the catalyst adopts Cu-Ca-Zn-Mg, and the mass percentage of the Cu-Ca-Zn-Mg is as follows: 18%, Ca: 25%, Zn: 5%, Mg: 0.9 percent.
Further, the amination reactorThe reaction temperature T1 is 210 ℃, the reaction pressure P is 0.1-0.3 MPa, and the liquid circulation amount F2 is 300m3The flow rate of dimethylamine F1 is 210-240 m3H, circulating gas flow F3 of 900m3The condensate temperature T2 of the cooler A is 80 ℃, the condensate temperature T3 of the cooler B is 40 ℃ and the liquid level L of the oil-water separator is 50%.
The invention has the advantages that: according to the invention, the gas-liquid separator filled with the metal corrugated filler is arranged on the circulating gas pipeline of the amination reactor, the oil phase separated in the oil-water separator is sprayed above the gas-liquid separator and carries out reverse heat exchange with the gas phase in the gas-liquid separator, the heavy component oil phase is condensed and flows back to the reactor, and the uncondensed gas continuously passes through the cooler A and the cooler B, so that the problem of material entrainment of the circulating gas is effectively solved; condensate condensed by the cooler A and the cooler B flows into the oil-water layer in the oil-water separating tank from the side surface of the oil-water separating tank along the pipeline, so that the oil-water in the condensate can be separated quickly. Under the condition of the same production capacity, the consumption of a single batch of the catalyst can be reduced by at least 33.33%, and the generation of byproducts can be reduced by at least 57.14%. Meanwhile, the amination reactor adopts an external circulation heating jet reactor, improves the mass transfer process, shortens the reaction time by 50 percent compared with a stirring kettle device under the same catalyst, improves the reaction selectivity by 1 percent, and has obvious economic benefit.
Drawings
FIG. 1 is a schematic view of a production apparatus for a tertiary amine according to the present invention;
FIG. 2 is a schematic diagram showing the structure of a tertiary amine production system in the prior art.
The reference numerals include:
in fig. 1: 1-evaporator, 2-circulating pump, 3-amination reactor, 31-venturi tube, 4-gas-liquid separator, 5-cooler A, 6-cooler B, 7-oil-water separator, 8-inlet buffer tank, 9-recovery kettle, 91-heating coil, 10-heat exchanger, 11-dimethylamine input pipeline, 12-dimethylamine steam output pipeline, 13-fatty alcohol input pipeline, 14-tertiary amine finished product output pipeline, 15-uncondensed gas output pipeline, 16-nitrogen input pipeline, 17-condensed liquid output pipeline, 18-water cooler, 19-hydrogen input pipeline, 20-cooling water inlet pipeline, 21-cooling water outlet pipeline, 22-valve A, 23-valve B, etc, 24-steam input pipeline, 25-condensed water output pipeline and 26-dimethylamine recovery pipeline.
In fig. 2: the system comprises a 100-amination reactor, a 200-recycle gas heat exchanger, a 300-recycle gas preheater, a 400-tertiary amine separator, a 500-oil-water separator, a 600-reaction water metering tank, a 700-dimethylamine vaporizer and a 800-recycle gas cooler.
Detailed Description
In order to make the purpose, technical solution and advantages of the present technical solution more clear, the present technical solution is further described in detail below with reference to specific embodiments. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present teachings.
As shown in figure 1, a tertiary amine production device comprises an evaporator 1, a circulating pump 2, an amination reactor 3, a gas-liquid separator 4, a cooler A5, a cooler B6, an oil-water separator 7, a buffer tank 8, a recovery kettle 9 and a heat exchanger 10;
a feeding port of the evaporator 1 is communicated with a dimethylamine input pipeline 11, dimethylamine is evaporated in the evaporator 1 to form dimethylamine steam, and an air outlet of the evaporator 1 is communicated with a dimethylamine steam output pipeline 12;
the material inlet of an amination reactor 3 is communicated with an aliphatic alcohol input pipeline 13, a venturi tube is arranged in the amination reactor 3, a nozzle above the venturi tube is communicated with the material outlet of a heat exchanger 10 through a pipeline, the material inlet of the heat exchanger 10 is communicated with the material outlet of a circulating pump 2 through a pipeline, the material outlet at the bottom of the amination reactor 3 is communicated with the material inlet of the circulating pump 2 through a pipeline, the material outlet at the side end of the amination reactor 3 is communicated with a tertiary amine finished product output pipeline 14, the gas outlet at the top of the amination reactor 3 is communicated with the gas inlet of a gas-liquid separator 4 through a pipeline, the material outlet at the bottom of the gas-liquid separator 4 is communicated with the material inlet at the top of the amination reactor 3 through a pipeline, the gas outlet at the top of the gas-liquid separator 4 is communicated with the gas inlet, cooler B6's side gas outlet is linked together through the air inlet of pipeline with buffer tank 8, and buffer tank 8's side gas outlet is equipped with noncondensable gas output line 15, noncondensable gas output line 15 with dimethylamine steam output line 12 assemble the back with amination reactor 3's venturi inhales the chamber and is linked together, noncondensable gas output line 15 and dimethylamine steam output line 12 are linked together with nitrogen gas input pipeline 16 and hydrogen input pipeline 19 in addition simultaneously, buffer tank 8's bottom discharge gate pass through the pipeline with retrieve cauldron 9 and be linked together, cooler A5 and cooler B6's bottom discharge gate respectively through condensation liquid output line 17 with oil water separator 7 side pan feeding mouth is linked together, the discharge gate on oil water separator 7 top with the pan feeding mouth on gas liquid separator 4 top passes through the pipeline and is linked together, oil water separator 7's bottom discharge gate with the pan feeding mouth on retrieve cauldron 9 top is linked together through the pipeline.
The cooler A5, the cooler B6 and the water cooler 18 are respectively communicated with the cooling water inlet pipeline 20 and the cooling water outlet pipeline 21 at the same time.
A valve A22 is arranged between the discharge hole at the bottom of the amination reactor 3 and the inlet of the circulating pump 2.
A valve B23 is arranged between the circulating pump 2 and the heat exchanger 10.
And a metal corrugated filler is arranged in the gas-liquid separator 4 and is used for realizing oil-water separation.
The coolers A5 and B6 are located at a higher position than the gas-liquid separator 4.
The present invention further provides a process for producing a tertiary amine using the apparatus for producing a tertiary amine, which comprises the steps of:
mixing fatty alcohol and catalyst in a proportioning tank, pumping into an amination reactor 3 from a fatty alcohol input pipeline 13, starting a circulating pump 2 to establish self circulation of the amination reactor 3, heating an evaporator 1 by hot water to vaporize dimethylamine to generate dimethylamine steam, forming partial vacuum when the fatty alcohol and the catalyst flow through a Venturi tube above the amination reactor 3 to suck the vaporized dimethylamine steam into the amination reactor 3 and participate in reaction, leading tertiary amine and the water steam generated by the reaction to enter a gas-liquid separator 4 filled with metal corrugated packing through a pipeline for gas-liquid separation, leading the condensed and separated liquid to flow back to the amination reactor 3 through a pipeline below the gas-liquid separator 4, leading the uncondensed gas to enter a cooler A5 through a pipeline, further condensing the gas, leading the uncondensed gas to enter a cooler B6 through a pipeline, condensing the gas again, leading the uncondensed gas to enter a buffer tank 8, and returned to the upper part of the amination reactor 3 via the uncondensed gas outlet line 15 to be sucked into the amination reactor 3 together with the dimethylamine vapour. The condensed liquids in the cooler A5 and the cooler B6 are respectively gathered together through a condensed liquid output pipeline 17 and flow into an oil-water separation tank 7 for oil-water separation, oil (fatty alcohol, tertiary amine and the like) is in the lower layer of water at the upper layer, the water flows out from the bottom of the oil-water separation tank 7 to a recovery kettle 9, the recovery kettle 9 is heated by water vapor, dimethylamine dissolved in the water is separated from the water after being heated, the evaporated dimethylamine condenses the volatilized water vapor through a water cooler 18, and the separated dimethylamine returns to the amination reactor 3 through a dimethylamine recovery pipeline 26 to continuously participate in the reaction;
meanwhile, the oil in the oil-water separator 7 is pressed to the gas-liquid separator 4 and then sprayed above the gas-liquid separator 4 to perform reverse heat exchange with the gas phase in the gas-liquid separator 4, and the heavy component oil phase is condensed and flows back to the amination reactor 3. The tertiary amine finished product is continuously generated along with the addition of the fatty alcohol and the dimethylamine and overflows from a tertiary amine finished product output pipeline 14 of the amination reactor 3.
The adding amount of the catalyst is 3 per mill of the mass of the fatty alcohol.
The catalyst adopts Cu-Ca-Zn-Mg, and the weight percentage composition of the Cu-Ca-Zn-Mg is as follows: 18%, Ca: 25%, Zn: 5%, Mg: 0.9 percent. The invention improves the Cu mass percentage from 16% to 18% to improve the activity and selectivity of the catalyst.
The reaction temperature T1 of the amination reactor is 210 ℃, the reaction pressure P is 0.1-0.3 MPa, and the liquid circulation quantity F2 is 300m3The flow rate of dimethylamine F1 is 210-240 m3H, circulating gas flow F3 of 900m3The condensate temperature T2 of the cooler A is 80 ℃, the condensate temperature T3 of the cooler B is 40 ℃ and the liquid level L of the oil-water separator is 50%.
According to the invention, a gas phase pipeline is provided with the gas-liquid separator 4, most of liquid is condensed and separated and flows back to the amination reactor 3, and the condition that the liquid level of the amination reactor 3 is reduced can not occur;
in the invention, the positions of the cooler A5 and the cooler B6 are higher than the gas-liquid separator 4, and the oil phase in the oil-water separator 4 is pressed into the gas-liquid separator 4 by gravity, and then flows back to the reactor after being subjected to reverse heat exchange with the gas phase in the reactor.
In the invention, the bottom discharge ports of the cooler A5 and the cooler B6 are respectively communicated with the side end feeding port of the oil-water separator 7 through the condensed liquid output pipeline 17, the oil-water mixture can be directly inserted into an oil-water layering interface, and the oil-water mixture can be rapidly layered after entering the oil-water separator 7.
The tertiary amine is produced by adopting the production device of the invention and the prior art, and the production comparison results of the two processes are shown in the table 1.
TABLE 1 comparison of Tertiary amine production Performance of the present invention versus the prior art
As can be seen from Table 1, compared with the prior art, the production device and the production method of the invention not only improve the color, the tertiary amine content and the main component content, inhibit the side reaction, but also shorten the reaction time and have obvious economic benefit.
The foregoing is only a preferred embodiment of the present invention, and many variations in the specific embodiments and applications of the invention may be made by those skilled in the art without departing from the spirit of the invention, which falls within the scope of the claims of this patent.
Claims (10)
1. A production device of tertiary amine is characterized by comprising an evaporator, a circulating pump, an amination reactor, a gas-liquid separator, a cooler A, a cooler B, an oil-water separator, a buffer tank, a recovery kettle and a heat exchanger;
a feeding port of the evaporator is communicated with a dimethylamine input pipeline, dimethylamine is evaporated in the evaporator to form dimethylamine steam, and a gas outlet of the evaporator is communicated with a dimethylamine steam output pipeline;
the material inlet of the amination reactor is communicated with an aliphatic alcohol input pipeline, a Venturi tube is arranged in the amination reactor, a nozzle above the Venturi tube is communicated with a material outlet of a heat exchanger through a pipeline, the material inlet of the heat exchanger is communicated with a material outlet of a circulating pump through a pipeline, a material outlet at the bottom of the amination reactor is communicated with a material inlet of the circulating pump through a pipeline, a material outlet at the side end of the amination reactor is communicated with a tertiary amine finished product output pipeline, a gas outlet at the top of the amination reactor is communicated with a gas inlet of a gas-liquid separator through a pipeline, a material outlet at the bottom of the gas-liquid separator is communicated with the material inlet at the top of the amination reactor through a pipeline, a gas outlet at the top of the gas-liquid separator is communicated with a gas inlet of a cooler A through a pipeline, a gas, the side gas outlet of buffer tank is equipped with noncondensable gas output line, noncondensable gas output line with dimethylamine steam output line assembles the back with amination reactor's venturi inhales the chamber and is linked together, noncondensable gas output line and dimethylamine steam output line are linked together with nitrogen gas input pipeline and hydrogen input pipeline in addition simultaneously, the bottom discharge mouth of buffer tank pass through the pipeline with it is linked together to retrieve the cauldron, cooler A and cooler B's bottom discharge mouth respectively through condensed liquid output line with oil water separator side pan feeding mouth is linked together, the discharge gate on oil water separator top with the pan feeding mouth on gas water separator top passes through the pipeline and is linked together, oil water separator's bottom discharge mouth with it is linked together through the pipeline to retrieve the pan feeding mouth on cauldron top.
2. The apparatus for producing a tertiary amine according to claim 1, wherein the recovery still has a heating coil inside to heat water in the recovery still, and a bottom inlet of the recovery still is connected to a steam inlet line to introduce steam into the recovery still to heat water in the recovery still, and a discharge outlet is connected to a condensed water outlet line to discharge condensed water, a water cooler is provided above the recovery still to prevent evaporation of steam, and a gas outlet above the water cooler is connected to the uncondensed gas outlet line through a dimethylamine recovery line.
3. The apparatus for producing a tertiary amine according to claim 1, wherein said cooler A, said cooler B and said water cooler are simultaneously connected to a cooling water inlet line and a cooling water outlet line, respectively.
4. The apparatus for producing a tertiary amine according to claim 1, wherein a valve A is provided between the outlet of the bottom of the amination reactor and the inlet of the circulation pump.
5. An apparatus for producing a tertiary amine according to claim 1, wherein a valve B is provided between said circulation pump and said heat exchanger.
6. The apparatus for producing a tertiary amine according to claim 1, wherein said gas-liquid separator contains a metal corrugated packing for effecting oil-water separation.
7. The apparatus for producing a tertiary amine according to claim 1, wherein said coolers A and B are located at a higher position than the gas-liquid separator.
8. A production method using the apparatus for producing a tertiary amine according to any one of claims 1 to 7, characterized by specifically comprising the steps of:
mixing fatty alcohol and catalyst in a proportioning tank, pumping into an amination reactor from a fatty alcohol input pipeline, starting a circulating pump to establish self circulation of the amination reactor, heating an evaporator by hot water to vaporize dimethylamine to generate dimethylamine steam, forming local vacuum when the fatty alcohol and the catalyst flow through a Venturi tube above the amination reactor to suck the vaporized dimethylamine steam into the amination reactor and take part in reaction, feeding tertiary amine and the water steam generated by the reaction into a gas-liquid separator filled with metal corrugated filler through a pipeline to perform gas-liquid separation, feeding the liquid separated by condensation back to the amination reactor through a pipeline below the gas-liquid separator, feeding the gas which is not condensed into a cooler A through a pipeline, further condensing the gas, feeding the gas which is not condensed into a cooler B through a pipeline, condensing the gas again, feeding the gas which is not condensed into a buffer tank, returning to the upper part of the amination reactor through an uncondensed gas output pipeline, and sucking the gas above the amination reactor together with dimethylamine steam into the amination reactor; the condensed liquids in the cooler A and the cooler B are respectively converged together through a condensed liquid output pipeline and flow into an oil-water separation tank for oil-water separation, the oil is on the upper layer, the water is on the lower layer, the water flows out from the bottom of the oil-water separation tank to a recovery kettle, the recovery kettle is heated by water vapor, dimethylamine dissolved in the water is separated from the water after being heated, the evaporated dimethylamine condenses the volatilized water vapor through a water cooler, and the separated dimethylamine returns to an amination reactor through a dimethylamine recovery pipeline to continuously participate in the reaction;
meanwhile, the oil in the oil-water separator is sprayed above the gas-liquid separator after being pressed to the gas-liquid separator, and carries out reverse heat exchange with the gas phase in the gas-liquid separator, and the heavy component oil phase is condensed and flows back to the amination reactor. The tertiary amine finished product is continuously generated along with the addition of the fatty alcohol and the dimethylamine and overflows from an output pipeline of the tertiary amine finished product of the amination reactor.
9. The method for producing a tertiary amine according to claim 8, wherein the amount of the catalyst added is 3% by mass of the fatty alcohol; the catalyst adopts Cu-Ca-Zn-Mg, and the weight percentage composition of the Cu-Ca-Zn-Mg is as follows: 18%, Ca: 25%, Zn: 5%, Mg: 0.9 percent.
10. The method for producing a tertiary amine according to claim 8, wherein the amination reactor has a reaction temperature T1 of 210 ℃, a reaction pressure P of 0.1 to 0.3MPa, and a liquid circulation F2 of 300m3The flow rate of dimethylamine F1 is 210-240 m3H, circulating gas flow F3 of 900m3The condensate temperature T2 of the cooler A is 80 ℃, the condensate temperature T3 of the cooler B is 40 ℃ and the liquid level L of the oil-water separator is 50%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006312624A (en) * | 2005-04-07 | 2006-11-16 | Kao Corp | Method for producing tertiary amine |
| CN101538205A (en) * | 2008-03-17 | 2009-09-23 | 株洲珊林科技有限公司 | Process system and method for continuously preparing long chain alkyl dimethyl tertiary amine |
| CN103071444A (en) * | 2013-01-30 | 2013-05-01 | 北京工商大学 | Gas-liquid reaction device |
| CN203128459U (en) * | 2012-12-18 | 2013-08-14 | 天津天智精细化工有限公司 | Preparation system of tertiary amine |
| CN203582768U (en) * | 2013-11-07 | 2014-05-07 | 灯塔北方化工有限公司 | Continuous tertiary amine production device for fixed bed |
-
2020
- 2020-12-02 CN CN202011386022.8A patent/CN112619588B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006312624A (en) * | 2005-04-07 | 2006-11-16 | Kao Corp | Method for producing tertiary amine |
| CN101538205A (en) * | 2008-03-17 | 2009-09-23 | 株洲珊林科技有限公司 | Process system and method for continuously preparing long chain alkyl dimethyl tertiary amine |
| CN203128459U (en) * | 2012-12-18 | 2013-08-14 | 天津天智精细化工有限公司 | Preparation system of tertiary amine |
| CN103071444A (en) * | 2013-01-30 | 2013-05-01 | 北京工商大学 | Gas-liquid reaction device |
| CN203582768U (en) * | 2013-11-07 | 2014-05-07 | 灯塔北方化工有限公司 | Continuous tertiary amine production device for fixed bed |
Non-Patent Citations (1)
| Title |
|---|
| 梅金龙等: "醇一步法催化胺化制叔胺生产工艺概述", 《中国洗涤用品工业》 * |
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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