CN109748805A - The method of liquid ammonia process for caustic soda purification production isopropanolamine - Google Patents
The method of liquid ammonia process for caustic soda purification production isopropanolamine Download PDFInfo
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Abstract
The problems such as the present invention relates to a kind of methods of liquid ammonia process for caustic soda purification production isopropanolamine, mainly solve in the prior art using water as catalyst, high, dehydration energy is high, product by-product is more so as to cause plant investment.This method uses anhydrous liquid ammonia and propylene oxide for reaction raw materials; calandria type fixed bed reactor and heat-insulating fixed bed reactors are set; ensure that propylene oxide converts completely; calandria type fixed bed reactor passes through circulating hot water cooling; cooling hot water preheats the reaction product after reaction raw materials and decompression; recyclable overwhelming majority reaction heat; reaction product recycles most ammonia by flash tank; remaining ammonia is recycled by the aminoacid stripping tower that tower top configures compressor; this method by-product is few; equipment investment and plant energy consumption can be reduced, can be used in the industrial production of isopropanolamine.
Description
Technical field
The present invention relates to isopropanolamine production fields, it particularly relates to which a kind of make original with anhydrous liquid ammonia and propylene oxide
The method for expecting to produce isopropanolamine under adhesiveless ZSM-5 zeolite molecular sieve catalyst catalytic action.
Background technique
Isopropanolamine includes monoisopropanolamine (1- amino -2- propyl alcohol, abbreviation MIPA), diisopropanolamine (DIPA) (2,2 '-dihydroxy
Di-n-propylamine, abbreviation DIPA) and three kinds of homologue products of triisopropanolamine (1,1,1 '-nitrilo-, three -2- propyl alcohol, abbreviation TIPA).
Isopropanolamine is a kind of amphoteric compound, due in molecule simultaneously there is amino and hydroxyl, both can be carried out the typical reaction of amine,
Also it can be carried out the typical reaction of alcohols, to synthesize a series of useful derivatives.These derivatives, which are widely used in producing, to be washed
Wash agent, polyurethane cross-linking agent, textile finshing agent, printing and dyeing softening agent, soap, cosmetics, antirust agent, metal cutting coolant, tan
Remove from office agent, coating, wax work and agrochemical.The aqueous solution of diisopropanolamine (DIPA) or the mixing water that it is constituted together with other solvents
Solution is widely used as industrially desulfurized dose.Since its physical property is similar to ethanol amine, so the occasion of all ethanol amines application, isopropanol
Amido originally has similar application.Isopropanolamine self property makes its application in some aspects better than ethanol amine, increasingly causes
The concern of people, application range are growing, and become one kind organic chemical industry excellent, with broad prospects for development and fine chemistry industry
Product.
It is a thtee-stage shiplock reaction, master by Material synthesis one, two, the reaction of triisopropanolamine of ammonia and propylene oxide
Want reaction equation as follows:
The reaction heat of three reactions is respectively -125.698kJ/mol, -136.692kJ/mol, -151.056kJ/mol, is
Strong exothermal reaction.With the difference of ammonia and propylene oxide molar ratio (ammonia alkane ratio), the ratio of three kinds of products be will be different.Ammonia alkane
Than bigger, shared ratio is bigger in the product for monoisopropanolamine, diisopropanolamine (DIPA), and on the contrary then triisopropanolamine is in the product
Ratio is bigger.If ammonia alkane, than too small, excessive propylene oxide and triisopropanolamine reaction generate triisopropanolamine propoxyl group ether:
Even if above-mentioned reaction is at high temperature under high pressure, reaction speed is also extremely slow, need to there is acid, alkali, alcohol, ion exchange resin or water
Isoreactivity group could accelerate reaction to catalytic action has been reacted, and wherein water is preferred cheap catalyst, prepare with raw material ammonia
It puts into and reacts at ammonium hydroxide.In general, the ammonia concn used is lower, i.e. when the amount of catalyst water is more, synthetic reaction condition
Milder, reaction pressure is lower (when ammonia concn is lower than 25wt%, reaction pressure is lower than 1MPa), and reaction speed is faster.
But a series of problems will be brought as catalyst using water, water promotes secondary anti-while promoting main reaction to occur
Ring-opening reaction will occur with propylene oxide and generate propylene glycol and propylene glycol propoxyl group ether for the reaction answered, water:
Water as catalyst needs to be separated with product in process of production, and dehydration need to consume a large amount of thermal energy, meanwhile, greatly
The presence of amount water can promote the generation of (5), (6) two side reactions, cause the decline of isopropanolamine purity, not only separate rectifying
Process complications, and energy consumption increases.
It is single although product purity is low it can be seen that mild as the technique reaction condition of raw material using low concentration ammonia aqueous solution
Position energy consumption is high.
External to mostly use the high strength ammonia aqueous solution of 60-90wt% as raw material greatly, reaction pressure is controlled in 6-8MPa, ammonia
And propylene oxide ratio is between 10~40:1.Due to reducing water, dehydration energy can decline by a relatively large margin, and high pressure is sudden strain of a muscle again
It steams deamination and provides condition, recovery ammonia energy consumption also decreases.But technique, still using water as catalyst, the pair of (4), (5) two formulas is anti-
It should still remain, product purity is still centainly influenced.
Summary of the invention
The technical problem to be solved by the present invention is to existing in the prior art using water as catalyst, so as to cause device throwing
The problems such as money is high, dehydration energy is high, product by-product is more provides a kind of method of new liquid ammonia process for caustic soda purification production isopropanolamine, the present invention
The technical solution taken is as follows: a kind of method of liquid ammonia process for caustic soda purification production isopropanolamine, comprising the following steps:
A) fresh anhydrous liquid ammonia and circulation liquefied ammonia are mixed into liquefied ammonia charging, are mixed into charging after preheating with propylene oxide feed
Mixture；
B) incoming mixture is sent into calandria type fixed bed reactor, and first order reaction product stream is obtained after reaction；
C) calandria type fixed bed reactor passes through circulating hot water cooling；
D) the first order reaction product stream enters heat-insulating fixed bed reactors, and the mixing containing ammonia is obtained after the reaction was continued
Isopropanolamine product；
E) the mixing isopropanolamine product containing ammonia depressurizes first, then after the heat exchange of reacted device cooling hot water, send first
Enter flash tank, flash drum overhead gas is condensed into condensation liquefied ammonia, is recycled back to reaction member, and flash tank bottom is obtained containing a small amount of ammonia
Mix isopropanolamine product；
F) the mixing isopropanolamine product containing a small amount of ammonia is sent into aminoacid stripping tower, and tower top obtains ammonia steam, and tower reactor obtains
The mixing isopropanolamine product for removing ammonia, is sent to subsequent separation process；
G) the ammonia steam is condensed into compression condensation liquefied ammonia through compressor three stage compression, is recycled back to reaction member.
In above-mentioned technical proposal, it is preferable that reactant in calandria type fixed bed reactor and heat-insulating fixed bed reactors
The flow direction of material is upper entering and lower leaving, and wherein calandria type fixed bed reactor tube side walks reaction mass, and shell side walks circulating hot water.
In above-mentioned technical proposal, it is preferable that calandria type fixed bed reactor reaction pressure be 7~10MPa, temperature be 80~
120℃。
In above-mentioned technical proposal, it is preferable that heat-insulating fixed bed reactors reaction pressure be 7~10MPa, temperature be 85~
130℃。
In above-mentioned technical proposal, it is preferable that the molar ratio of fresh liquefied ammonia and propylene oxide is 5:1~12:1.
In above-mentioned technical proposal, it is preferable that in the circulating hot water and tube side in calandria type fixed bed reactor in shell side
It is identical that reaction mass flows direction, continuously withdraws from reaction heat, makes temperature≤120 DEG C of the reaction mass in tube side, and pressure≤
10MPa。
Reactor cooling hot water exchanges heat with logistics cold in technique, is to recycle a kind of maximally efficient mode of reaction heat,
In above-mentioned technical proposal, it is preferable that after circulating hot water goes out calandria type fixed bed reactor, all with the mixing isopropyl containing ammonia
The heat exchange of hydramine product enters calandria type fixed bed reactor after cooling down using cooler.
In above-mentioned technical proposal, it is preferable that after circulating hot water goes out calandria type fixed bed reactor, it is divided into two parts, one
Divide and exchange heat with liquefied ammonia charging, a part of and described mixing isopropanolamine product heat exchange containing ammonia is cooling using cooler
Enter calandria type fixed bed reactor afterwards.
In above-mentioned technical proposal, it is preferable that the temperature difference≤6 DEG C of circulating hot water disengaging calandria type fixed bed reactor.
In above-mentioned technical proposal, it is preferable that the flash tank is level-one, second level or multistage, it is also possible to which rectifying column replaces.
Isopropanolamine is heat-sensitive substance, is easy to happen pyrolytic under high temperature and influences product coloration and quality, on
It states in technical solution, it is preferable that aminoacid stripping tower tower top pressure≤0.13MPa, bottom temperature≤180 DEG C.
Aminoacid stripping tower tower top pressure is lower, and compression energy consumption is bigger, in above-mentioned technical proposal, it is preferable that aminoacid stripping tower tower top
0.11~0.13MPa of pressure.
To use cheap cooling water as the cooling ammonia steam after compression pressurization of cooling medium, compression should be improved
Machine outlet pressure makes cold solidifying Wen Du≤35 DEG C of ammonia steam under this pressure, but hypertonia, easily causes the waste of energy, above-mentioned
In technical solution, it is preferable that Chu mouthfuls of Ya Li≤1.4MPa of the Ya contracting machine.
In above-mentioned technical proposal, it is preferable that the compressor delivery pressure is 1.4MPa.
In above-mentioned technical proposal, it is preferable that be equipped with cooler and gas-liquid separation between stage compressor and split-compressor
Subsequent separation process is sent in device, the extraction of gas-liquid separator liquid phase.
In above-mentioned technical proposal, it is preferable that be equipped with cooler and gas-liquid separation between split-compressor and three-stage blower
Subsequent separation process is sent in device, the extraction of gas-liquid separator liquid phase.
In above-mentioned technical proposal, it is preferable that the compressor can also for one stage of compression, two-stage compression, level Four compression or more
Multi-stage compression.
The excessively high conversion ratio that will affect reaction of fresh anhydrous liquid ammonia impurity content and selectivity, shorten catalyst life, because
This, can move to fresh anhydrous liquid ammonia feed entrance point at technique other positions, first pass around purification, then pass through circulation liquefied ammonia pipeline
Send reactor back to and participate in reaction, in above-mentioned technical proposal, it is preferable that fresh anhydrous liquid ammonia can in heat-insulating fixed bed reactors and
Any position is added between flash tank, can also be added at aminoacid stripping tower feed entrance point.
Adhesiveless ZSM-5 zeolite molecules are filled in present invention process shell and tube reactor and heat-insulating fixed bed reactors
Sieve catalyst substitutes in traditional handicraft using water as catalyst, can reduce a series of side reactions caused by water, improves product quality,
Save dehydration energy.Shell and tube reactor outlet material enters heat-insulating fixed bed reactors, guarantees that propylene oxide converts completely,
Propylene oxide is avoided to penetrate the safety accident and equipment fault that may cause.Shell and tube reactor and heat-insulating fixed bed reactors
Concatenated structure can reduce shell and tube catalytic ammoniation main reactor volume, and main reactor cooling is convenient, reaction is mild, pass through tune
It saves hot water input and hot water inlet's temperature carries out temperature control, have the characteristics that reaction temperature is controllable, safe and reliable.Shell and tube is solid
60~99% reaction heat can be recycled for preheating liquefied ammonia charging and reaction product in the circulation cooling hot water of fixed bed reactor.Reaction
More than 90% ammonia by flash tank circulation and stress in product, 10% or less ammonia is recycled by aminoacid stripping tower, aminoacid stripping tower tower top ammonia
Steam first compresses to be condensed again, can reduce device overall power consumption.The environmental friendly safety of isopropanolamine, product structure is adjustable, energy
Enough inhibit by-product, product purity is high easily separated, it can be achieved that long-term operation and reduction production cost.
Using the method for the present invention, product isopropanolamine (including monoisopropanolamine, diisopropanolamine (DIPA) and monoisopropanolamine)
Yield >=99.6%, the content of the ethers such as triisopropanolamine propoxyl group ether is only 0.1~0.4% in product, and catalyst uses the longevity
Life is 12 months, achieves preferable technical effect.
Detailed description of the invention
Fig. 1 is the process flow chart that liquid ammonia process for caustic soda purification of the present invention produces isopropanolamine.
In Fig. 1, R-101 is calandria type fixed bed reactor, and R-102 is heat-insulating fixed bed reactors, and E-101 is charging
Preheater, E-102 are circulating hot water cooler, and E-103 is reaction product cooler, and E-104 is liquefied ammonia condenser, and E-105 is
One stage of compression cooler, E-106 are two-stage compression cooler, and E-107 is three stage compression cooler, and D-101 is flash tank, D-
102 be one stage of compression knockout drum, and D-103 is two-stage compression knockout drum, and T-101 is aminoacid stripping tower, and C-101 is level-one
Compressor, C-102 are split-compressor, and C-103 is three-stage blower.1 is propylene oxide feed, and 2 be fresh anhydrous liquid ammonia, 3
It is fed for liquefied ammonia charging, 4 for high temperature liquefied ammonia, 5 be first order reaction product, and 6 be Depressor response product, and 7 feed for flash tank, and 8 are
The discharging of flash tank gas phase, 9 feed for condensation liquefied ammonia, 10 for aminoacid stripping tower, and 11 be ammonia steam, and 12 discharge for aminoacid stripping tower tower reactor,
13 discharge for one stage of compression knockout drum liquid phase, and 14 discharge for two-stage compression knockout drum liquid phase, and 15 be the different of removing ammonia
Propanolamine product, 16 be compression condensation liquefied ammonia.
In Fig. 1, fresh anhydrous liquid ammonia 1 is mixed into liquefied ammonia charging 3 with condensation liquefied ammonia 9 and compression condensation liquefied ammonia 16, through feeding
High temperature liquefied ammonia charging 4 is obtained after preheater E-101 preheating, high temperature liquefied ammonia charging 4 is mixed with propylene oxide feed 1, and mixture is sent
At the top of toward calandria type fixed bed reactor R-101, first order reaction product 5 is obtained in the bottom R-101 after reaction, R-101 is used and followed
Ring hot water cooling, circulating hot water upper entering and lower leaving are forward flowed with reaction mass, and the circulating hot water after cooling is divided into two strands, one
For preheating liquefied ammonia charging 3 in E-101, one is used to preheat Depressor response product 6 in reaction product cooler E-103,
Calandria type fixed bed reactor R-101 is sent back to after circulating hot water cooler E-102 is cooling；First order reaction product 5 is sent into insulation
Formula fixed bed reactors R-102 continues to react, and remaining propylene oxide is converted completely, and the outlet R-102 is subtracted
Reaction product 6 is pressed, Depressor response product 6 is preheated in reaction product cooler E-103 through circulating hot water first, exported
Flash tank D-101 is sent into flash tank charging 7, and 8 feeding liquefied ammonia condenser E-104 of flash tank gas phase discharging is condensed into condensation liquefied ammonia 9,
Condensation liquefied ammonia 9 is recycled to reaction member, and the discharging of flash tank liquid phase is aminoacid stripping tower charging 10, aminoacid stripping tower T-101 tower overhead gas
Ammonia steam 11 is sent to one stage of compression knockout drum after stage compressor C-101, one stage of compression cooler E-105 compression are cooling
The discharging of D-102, D-102 gas phase continues to be sent to split-compressor C-102, two-stage compression cooler E-106 compression cooling, second level pressure
The discharging of contracting knockout drum D-103 gas phase is sent to three-stage blower C-103, three stage compression cooler E-107 compression cooling and is obtained
Compression condensation liquefied ammonia 16 is recycled to reaction member, and D-102 liquid phase discharging 13 and D-103 liquid phase discharging 14 goes out with aminoacid stripping tower tower reactor
Material 12 is mixed into the isopropanolamine product 15 of removing ammonia, is sent into subsequent separation process.
The present invention will be further described below by way of examples, but these embodiments are not anyway to this hair
Bright range is construed as limiting.
Specific embodiment
[embodiment 1]
Fresh liquefied ammonia 2 is mixed into liquefied ammonia charging 3, preheated rear and epoxy third with condensation liquefied ammonia 9 and compression condensation liquefied ammonia 16
Calandria type fixed bed reactor R-101 is sent into 1 mixing of alkane charging, and first order reaction product 5 enters heat-insulating fixed bed reactors R-
Adhesiveless ZSM-5 zeolite molecular sieve catalyst is filled in 102, R-101 and R-102, the outlet R-102 decompression obtains logistics 6,
It is sent into flash tank D-101 after reacted device hot water preheating, D-101 overhead stream 8 is recycled to reaction member, bottoms after condensing
10 are sent into aminoacid stripping tower T-101, and T-101 overhead stream 11 is condensed into logistics 16 through three stage compression, is recycled to reaction member, level-one
Knockout drum D-102 and D-103, D-102 and D- are additionally provided between compression and two-stage compression, two-stage compression and three stage compression
103 liquid phase output streams 13 and logistics 14 and tower reactor output streams 12 are mixed into logistics 15, are sent into subsequent separation process.
The molar ratio of liquefied ammonia charging 3 and propylene oxide feed 1 is 8:1.
Calandria type fixed bed reactor reaction pressure is 9MPa, and outlet temperature is 110 DEG C.Heat-insulating fixed bed reactors are anti-
Answering pressure is 9MPa, and outlet temperature is 118 DEG C.
After 105 DEG C of circulating hot water enter calandria type fixed bed reactor shell sides, 110 DEG C are heated to from calandria type fixed bed
Reactor lower part outflow, is heated to 98 DEG C for Depressor response product stream 6, is cooled to 105 DEG C using circulating hot water cooler
Into calandria type fixed bed reactor shell side.The temperature difference that circulating hot water passes in and out calandria type fixed bed reactor is 5 DEG C.
Calandria type fixed bed reactor reaction heat 93% is recycled, and reduces process energy consumption.
95% ammonia is recycled by flash tank D-101 in logistics 6, and 5% ammonia enters aminoacid stripping tower T-101.
Aminoacid stripping tower T-101 tower top pressure 0.13MPa, 180 DEG C of bottom temperature, three stage compression compressor delivery pressure
1.4MPa, the temperature of compression condensation logistics 16 are 40 DEG C.
The yield of product isopropanolamine (including monoisopropanolamine, diisopropanolamine (DIPA) and monoisopropanolamine) is 99.6%, is produced
The content of the ethers such as triisopropanolamine propoxyl group ether is 0.15% in product, and the service life of catalyst is 12 months, regeneration week
Phase is 3~6 months.
[embodiment 2]
Fresh liquefied ammonia 2 is mixed into liquefied ammonia charging 3, preheated rear and epoxy third with condensation liquefied ammonia 9 and compression condensation liquefied ammonia 16
Calandria type fixed bed reactor R-101 is sent into 1 mixing of alkane charging, and first order reaction product 5 enters heat-insulating fixed bed reactors R-
Adhesiveless ZSM-5 zeolite molecular sieve catalyst is filled in 102, R-101 and R-102, the outlet R-102 decompression obtains logistics 6,
It is sent into flash tank D-101 after reacted device hot water preheating, D-101 overhead stream 8 is recycled to reaction member, bottoms after condensing
10 are sent into aminoacid stripping tower T-101, and T-101 overhead stream 11 is condensed into logistics 16 through three stage compression, is recycled to reaction member, level-one
Knockout drum D-102 and D-103, D-102 and D- are additionally provided between compression and two-stage compression, two-stage compression and three stage compression
103 liquid phase output streams 13 and logistics 14 and tower reactor output streams 12 are mixed into logistics 15, are sent into subsequent separation process.
The molar ratio of liquefied ammonia charging 3 and propylene oxide feed 1 is 9:1.
Calandria type fixed bed reactor reaction pressure is 9.5MPa, and outlet temperature is 115 DEG C.Heat-insulating fixed bed reactors
Reaction pressure is 9.5MPa, and outlet temperature is 122 DEG C.
After 110 DEG C of circulating hot water enter calandria type fixed bed reactor shell sides, 115 DEG C are heated to from calandria type fixed bed
Reactor lower part outflow, is heated to 86 DEG C for Depressor response product stream 6, is cooled to 110 DEG C using circulating hot water cooler
Into calandria type fixed bed reactor shell side.The temperature difference that circulating hot water passes in and out calandria type fixed bed reactor is 5 DEG C.
Calandria type fixed bed reactor reaction heat 99% is recycled, and reduces process energy consumption.
94% ammonia is recycled by flash tank D-101 in logistics 6, and 6% ammonia enters aminoacid stripping tower T-101.
Aminoacid stripping tower T-101 tower top pressure 0.13MPa, 180 DEG C of bottom temperature, three stage compression compressor delivery pressure
1.4MPa, the temperature of compression condensation logistics 16 are 40 DEG C.
The yield of product isopropanolamine (including monoisopropanolamine, diisopropanolamine (DIPA) and monoisopropanolamine) is 99.6%, is produced
The content of the ethers such as triisopropanolamine propoxyl group ether is 0.17% in product, and the service life of catalyst is 12 months, regeneration week
Phase is 3~6 months.
[embodiment 3]
Fresh liquefied ammonia 2 is mixed into liquefied ammonia charging 3, preheated rear and epoxy third with condensation liquefied ammonia 9 and compression condensation liquefied ammonia 16
Calandria type fixed bed reactor R-101 is sent into 1 mixing of alkane charging, and first order reaction product 5 enters heat-insulating fixed bed reactors R-
Adhesiveless ZSM-5 zeolite molecular sieve catalyst is filled in 102, R-101 and R-102, the outlet R-102 decompression obtains logistics 6,
It is sent into flash tank D-101 after reacted device hot water preheating, D-101 overhead stream 8 is recycled to reaction member, bottoms after condensing
10 are sent into aminoacid stripping tower T-101, and T-101 overhead stream 11 is condensed into logistics 16 through three stage compression, is recycled to reaction member, level-one
Knockout drum D-102 and D-103, D-102 and D- are additionally provided between compression and two-stage compression, two-stage compression and three stage compression
103 liquid phase output streams 13 and logistics 14 and tower reactor output streams 12 are mixed into logistics 15, are sent into subsequent separation process.
The molar ratio of liquefied ammonia charging 3 and propylene oxide feed 1 is 10:1.
Calandria type fixed bed reactor reaction pressure is 10MPa, and outlet temperature is 120 DEG C.Heat-insulating fixed bed reactors
Reaction pressure is 10MPa, and outlet temperature is 126 DEG C.
After 110 DEG C of circulating hot water enter calandria type fixed bed reactor shell sides, 115 DEG C are heated to from calandria type fixed bed
Reactor lower part outflow, is heated to 71 DEG C for Depressor response product stream 6, is cooled to 110 DEG C using circulating hot water cooler
Into calandria type fixed bed reactor shell side.The temperature difference that circulating hot water passes in and out calandria type fixed bed reactor is 5 DEG C.
Calandria type fixed bed reactor reaction heat 99% is recycled, and reduces process energy consumption.
93% ammonia is recycled by flash tank D-101 in logistics 6, and 7% ammonia enters aminoacid stripping tower T-101.
Aminoacid stripping tower T-101 tower top pressure 0.13MPa, 180 DEG C of bottom temperature, three stage compression compressor delivery pressure
1.4MPa, the temperature of compression condensation logistics 16 are 40 DEG C.
The yield of product isopropanolamine (including monoisopropanolamine, diisopropanolamine (DIPA) and monoisopropanolamine) is 99.6%, is produced
The content of the ethers such as triisopropanolamine propoxyl group ether is 0.19% in product, and the service life of catalyst is 12 months, regeneration week
Phase is 3~6 months.
[embodiment 4]
Fresh liquefied ammonia 2 is mixed into liquefied ammonia charging 3, preheated rear and epoxy third with condensation liquefied ammonia 9 and compression condensation liquefied ammonia 16
Calandria type fixed bed reactor R-101 is sent into 1 mixing of alkane charging, and first order reaction product 5 enters heat-insulating fixed bed reactors R-
Adhesiveless ZSM-5 zeolite molecular sieve catalyst is filled in 102, R-101 and R-102, the outlet R-102 decompression obtains logistics 6,
It is sent into flash tank D-101 after reacted device hot water preheating, D-101 overhead stream 8 is recycled to reaction member, bottoms after condensing
10 are sent into aminoacid stripping tower T-101, and T-101 overhead stream 11 is condensed into logistics 16 through three stage compression, is recycled to reaction member, level-one
Knockout drum D-102 and D-103, D-102 and D- are additionally provided between compression and two-stage compression, two-stage compression and three stage compression
103 liquid phase output streams 13 and logistics 14 and tower reactor output streams 12 are mixed into logistics 15, are sent into subsequent separation process.
The molar ratio of liquefied ammonia charging 3 and propylene oxide feed 1 is 11:1.
Calandria type fixed bed reactor reaction pressure is 10MPa, and outlet temperature is 120 DEG C.Heat-insulating fixed bed reactors
Reaction pressure is 10MPa, and outlet temperature is 125 DEG C.
After 110 DEG C of circulating hot water enter calandria type fixed bed reactor shell sides, 115 DEG C are heated to from calandria type fixed bed
Reactor lower part outflow, is heated to 69 DEG C for Depressor response product stream 6, is cooled to 110 DEG C using circulating hot water cooler
Into calandria type fixed bed reactor shell side.The temperature difference that circulating hot water passes in and out calandria type fixed bed reactor is 5 DEG C.
Calandria type fixed bed reactor reaction heat 99% is recycled, and reduces process energy consumption.
92% ammonia is recycled by flash tank D-101 in logistics 6, and 8% ammonia enters aminoacid stripping tower T-101.
Aminoacid stripping tower T-101 tower top pressure 0.13MPa, 180 DEG C of bottom temperature, three stage compression compressor delivery pressure
1.4MPa, the temperature of compression condensation logistics 16 are 40 DEG C.
The yield of product isopropanolamine (including monoisopropanolamine, diisopropanolamine (DIPA) and monoisopropanolamine) is 99.6%, is produced
The content of the ethers such as triisopropanolamine propoxyl group ether is 0.19% in product, and the service life of catalyst is 12 months, regeneration week
Phase is 3~6 months.
[embodiment 5]
Fresh liquefied ammonia 2 is mixed into liquefied ammonia charging 3, preheated rear and epoxy third with condensation liquefied ammonia 9 and compression condensation liquefied ammonia 16
Calandria type fixed bed reactor R-101 is sent into 1 mixing of alkane charging, and first order reaction product 5 enters heat-insulating fixed bed reactors R-
Adhesiveless ZSM-5 zeolite molecular sieve catalyst is filled in 102, R-101 and R-102, the outlet R-102 decompression obtains logistics 6,
It is sent into flash tank D-101 after reacted device hot water preheating, D-101 overhead stream 8 is recycled to reaction member, bottoms after condensing
10 are sent into aminoacid stripping tower T-101, and T-101 overhead stream 11 is condensed into logistics 16 through three stage compression, is recycled to reaction member, level-one
Knockout drum D-102 and D-103, D-102 and D- are additionally provided between compression and two-stage compression, two-stage compression and three stage compression
103 liquid phase output streams 13 and logistics 14 and tower reactor output streams 12 are mixed into logistics 15, are sent into subsequent separation process.
The molar ratio of liquefied ammonia charging 3 and propylene oxide feed 1 is 12:1.
Calandria type fixed bed reactor reaction pressure is 10MPa, and outlet temperature is 120 DEG C.Heat-insulating fixed bed reactors
Reaction pressure is 10MPa, and outlet temperature is 125 DEG C.
After 110 DEG C of circulating hot water enter calandria type fixed bed reactor shell sides, 115 DEG C are heated to from calandria type fixed bed
Reactor lower part outflow, is heated to 60 DEG C for Depressor response product stream 6, is cooled to 110 DEG C using circulating hot water cooler
Into calandria type fixed bed reactor shell side.The temperature difference that circulating hot water passes in and out calandria type fixed bed reactor is 5 DEG C.
Calandria type fixed bed reactor reaction heat 99% is recycled, and reduces process energy consumption.
91% ammonia is recycled by flash tank D-101 in logistics 6, and 9% ammonia enters aminoacid stripping tower T-101.
Aminoacid stripping tower T-101 tower top pressure 0.13MPa, 180 DEG C of bottom temperature, three stage compression compressor delivery pressure
1.4MPa, the temperature of compression condensation logistics 16 are 40 DEG C.
The yield of product isopropanolamine (including monoisopropanolamine, diisopropanolamine (DIPA) and monoisopropanolamine) is 99.6%, is produced
The content of the ethers such as triisopropanolamine propoxyl group ether is 0.19% in product, and the service life of catalyst is 12 months, regeneration week
Phase is 3~6 months.
[embodiment 6]
Fresh liquefied ammonia 2 is mixed into liquefied ammonia charging 3, reacted device hot water preheating with condensation liquefied ammonia 9 and compression condensation liquefied ammonia 16
It is mixed afterwards with propylene oxide feed 1 and is sent into calandria type fixed bed reactor R-101, first order reaction product 5 is fixed into heat-insulating
Adhesiveless ZSM-5 zeolite molecular sieve catalyst, the outlet R-102 decompression are filled in bed reactor R-102, R-101 and R-102
Logistics 6 is obtained, is sent into flash tank D-101 after reacted device hot water preheating, D-101 overhead stream 8 is recycled to reaction after condensing single
Member, bottoms 10 are sent into aminoacid stripping tower T-101, and T-101 overhead stream 11 is condensed into logistics 16 through three stage compression, are recycled to anti-
Unit is answered, knockout drum D-102 and D-103 are additionally provided between one stage of compression and two-stage compression, two-stage compression and three stage compression,
The liquid phase output streams 13 and logistics 14 and tower reactor output streams 12 of D-102 and D-103 are mixed into logistics 15, are sent into subsequent point
From process.
The molar ratio of liquefied ammonia charging 3 and propylene oxide feed 1 is 7:1.
Calandria type fixed bed reactor reaction pressure is 8.5MPa, and outlet temperature is 105 DEG C.Heat-insulating fixed bed reactors
Reaction pressure is 8.5MPa, and outlet temperature is 114 DEG C.
After 100 DEG C of circulating hot water enter calandria type fixed bed reactor shell sides, 105 DEG C are heated to from calandria type fixed bed
Reactor lower part outflow, is heated to 86 DEG C for Depressor response product stream 6, liquefied ammonia charging 3 is heated to 80 DEG C, using circulation
Hot water cooler is cooled to 100 DEG C and enters calandria type fixed bed reactor shell side.Circulating hot water passes in and out calandria type fixed bed reaction
The temperature difference of device is 5 DEG C.
Calandria type fixed bed reactor reaction heat 24% feeds 3 pre- heat utilizations by liquefied ammonia, and 75% is depressurized reaction product 6 in advance
Heat utilization, calandria type fixed bed reactor reaction heat 99% are recycled, and reduce process energy consumption.
91% ammonia is recycled by flash tank D-101 in logistics 6, and 9% ammonia enters aminoacid stripping tower T-101.
Aminoacid stripping tower T-101 tower top pressure 0.13MPa, 180 DEG C of bottom temperature, three stage compression compressor delivery pressure
1.4MPa, the temperature of compression condensation logistics 16 are 40 DEG C.
The yield of product isopropanolamine (including monoisopropanolamine, diisopropanolamine (DIPA) and monoisopropanolamine) is 99.6%, is produced
The content of the ethers such as triisopropanolamine propoxyl group ether is 0.14% in product, and the service life of catalyst is 12 months, regeneration week
Phase is 3~6 months.
[embodiment 7]
Fresh liquefied ammonia 2 is mixed into liquefied ammonia charging 3, reacted device hot water preheating with condensation liquefied ammonia 9 and compression condensation liquefied ammonia 16
It is mixed afterwards with propylene oxide feed 1 and is sent into calandria type fixed bed reactor R-101, first order reaction product 5 is fixed into heat-insulating
Adhesiveless ZSM-5 zeolite molecular sieve catalyst, the outlet R-102 decompression are filled in bed reactor R-102, R-101 and R-102
Logistics 6 is obtained, is sent into flash tank D-101 after reacted device hot water preheating, D-101 overhead stream 8 is recycled to reaction after condensing single
Member, bottoms 10 are sent into aminoacid stripping tower T-101, and T-101 overhead stream 11 is condensed into logistics 16 through three stage compression, are recycled to anti-
Unit is answered, knockout drum D-102 and D-103 are additionally provided between one stage of compression and two-stage compression, two-stage compression and three stage compression,
The liquid phase output streams 13 and logistics 14 and tower reactor output streams 12 of D-102 and D-103 are mixed into logistics 15, are sent into subsequent point
From process.
The molar ratio of liquefied ammonia charging 3 and propylene oxide feed 1 is 6:1.
Calandria type fixed bed reactor reaction pressure is 8MPa, and outlet temperature is 100 DEG C.Heat-insulating fixed bed reactors are anti-
Answering pressure is 8MPa, and outlet temperature is 110 DEG C.
After 95 DEG C of circulating hot water enter calandria type fixed bed reactor shell sides, 100 DEG C are heated to from calandria type fixed bed
Reactor lower part outflow, is heated to 95 DEG C for Depressor response product stream 6, liquefied ammonia charging 3 is heated to 80 DEG C, using circulation
Hot water cooler is cooled to 95 DEG C and enters calandria type fixed bed reactor shell side.Circulating hot water passes in and out calandria type fixed bed reactor
The temperature difference be 5 DEG C.
Calandria type fixed bed reactor reaction heat 20.4% feeds 3 pre- heat utilizations by liquefied ammonia, and 71.5%, which is depressurized reaction, produces
The pre- heat utilization of object 6, calandria type fixed bed reactor reaction heat 91.9% are recycled, and reduce process energy consumption.
93% ammonia is recycled by flash tank D-101 in logistics 6, and 7% ammonia enters aminoacid stripping tower T-101.
Aminoacid stripping tower T-101 tower top pressure 0.13MPa, 180 DEG C of bottom temperature, three stage compression compressor delivery pressure
1.4MPa, the temperature of compression condensation logistics 16 are 40 DEG C.
The yield of product isopropanolamine (including monoisopropanolamine, diisopropanolamine (DIPA) and monoisopropanolamine) is 99.6%, is produced
The content of the ethers such as triisopropanolamine propoxyl group ether is 0.13% in product, and the service life of catalyst is 12 months, regeneration week
Phase is 3~6 months.
[embodiment 8]
Fresh liquefied ammonia 2 is mixed into liquefied ammonia charging 3, reacted device hot water preheating with condensation liquefied ammonia 9 and compression condensation liquefied ammonia 16
It is mixed afterwards with propylene oxide feed 1 and is sent into calandria type fixed bed reactor R-101, first order reaction product 5 is fixed into heat-insulating
Adhesiveless ZSM-5 zeolite molecular sieve catalyst, the outlet R-102 decompression are filled in bed reactor R-102, R-101 and R-102
Logistics 6 is obtained, is sent into flash tank D-101 after reacted device hot water preheating, D-101 overhead stream 8 is recycled to reaction after condensing single
Member, bottoms 10 are sent into aminoacid stripping tower T-101, and T-101 overhead stream 11 is condensed into logistics 16 through three stage compression, are recycled to anti-
Unit is answered, knockout drum D-102 and D-103 are additionally provided between one stage of compression and two-stage compression, two-stage compression and three stage compression,
The liquid phase output streams 13 and logistics 14 and tower reactor output streams 12 of D-102 and D-103 are mixed into logistics 15, are sent into subsequent point
From process.
The molar ratio of liquefied ammonia charging 3 and propylene oxide feed 1 is 5:1.
Calandria type fixed bed reactor reaction pressure is 7MPa, and outlet temperature is 90 DEG C.Heat-insulating fixed bed reactors are anti-
Answering pressure is 7MPa, and outlet temperature is 103 DEG C.
After 85 DEG C of circulating hot water enter calandria type fixed bed reactor shell sides, 90 DEG C are heated to from calandria type fixed bed anti-
It answers device lower part to flow out, Depressor response product stream 6 is heated to 85 DEG C, liquefied ammonia charging 3 is heated to 80 DEG C, using cycling hot
Water cooler is cooled to 85 DEG C and enters calandria type fixed bed reactor shell side.Circulating hot water passes in and out calandria type fixed bed reactor
The temperature difference is 5 DEG C.
Calandria type fixed bed reactor reaction heat 16.3% feeds 3 pre- heat utilizations by liquefied ammonia, and 46.9%, which is depressurized reaction, produces
The pre- heat utilization of object 6, calandria type fixed bed reactor reaction heat 63.2% are recycled, and reduce process energy consumption.
90% ammonia is recycled by flash tank D-101 in logistics 6, and 10% ammonia enters aminoacid stripping tower T-101.
Aminoacid stripping tower T-101 tower top pressure 0.13MPa, 180 DEG C of bottom temperature, three stage compression compressor delivery pressure
1.4MPa, the temperature of compression condensation logistics 16 are 40 DEG C.
The yield of product isopropanolamine (including monoisopropanolamine, diisopropanolamine (DIPA) and monoisopropanolamine) is 99.6%, is produced
The content of the ethers such as triisopropanolamine propoxyl group ether is 0.12% in product, and the service life of catalyst is 12 months, regeneration week
Phase is 3~6 months.
[embodiment 9]
Fresh liquefied ammonia 2 is mixed into liquefied ammonia charging 3, preheated rear and epoxy third with condensation liquefied ammonia 9 and compression condensation liquefied ammonia 16
Calandria type fixed bed reactor R-101 is sent into 1 mixing of alkane charging, and first order reaction product 5 enters heat-insulating fixed bed reactors R-
Adhesiveless ZSM-5 zeolite molecular sieve catalyst is filled in 102, R-101 and R-102, the outlet R-102 decompression obtains logistics 6,
It is sent into flash tank D-101 after reacted device hot water preheating, D-101 overhead stream 8 is recycled to reaction member, bottoms after condensing
10 are sent into aminoacid stripping tower T-101, and T-101 overhead stream 11 is condensed into logistics 16 through three stage compression, is recycled to reaction member, level-one
Knockout drum D-102 and D-103, D-102 and D- are additionally provided between compression and two-stage compression, two-stage compression and three stage compression
103 liquid phase output streams 13 and logistics 14 and tower reactor output streams 12 are mixed into logistics 15, are sent into subsequent separation process.
The molar ratio of liquefied ammonia charging 3 and propylene oxide feed 1 is 8:1.
Calandria type fixed bed reactor reaction pressure is 9MPa, and outlet temperature is 80 DEG C.Heat-insulating fixed bed reactors are anti-
Answering pressure is 9MPa, and outlet temperature is 89 DEG C.
After 75 DEG C of circulating hot water enter calandria type fixed bed reactor shell sides, 80 DEG C are heated to from calandria type fixed bed anti-
It answers device lower part to flow out, Depressor response product stream 6 is heated to 75 DEG C, is cooled to 75 DEG C of entrance using circulating hot water cooler
Calandria type fixed bed reactor shell side.The temperature difference that circulating hot water passes in and out calandria type fixed bed reactor is 5 DEG C.
Calandria type fixed bed reactor reaction heat 90.7% is recycled, and reduces process energy consumption.
93% ammonia is recycled by flash tank D-101 in logistics 6, and 7% ammonia enters aminoacid stripping tower T-101.
Aminoacid stripping tower T-101 tower top pressure 0.13MPa, 180 DEG C of bottom temperature, three stage compression compressor delivery pressure
1.4MPa, the temperature of compression condensation logistics 16 are 40 DEG C.
The yield of product isopropanolamine (including monoisopropanolamine, diisopropanolamine (DIPA) and monoisopropanolamine) is 99.6%, is produced
The content of the ethers such as triisopropanolamine propoxyl group ether is 0.13% in product, and the service life of catalyst is 12 months, regeneration week
Phase is 3~6 months.
[embodiment 10]
Fresh liquefied ammonia 2 is mixed into liquefied ammonia charging 3, preheated rear and epoxy third with condensation liquefied ammonia 9 and compression condensation liquefied ammonia 16
Calandria type fixed bed reactor R-101 is sent into 1 mixing of alkane charging, and first order reaction product 5 enters heat-insulating fixed bed reactors R-
Adhesiveless ZSM-5 zeolite molecular sieve catalyst is filled in 102, R-101 and R-102, the outlet R-102 decompression obtains logistics 6,
It is sent into flash tank D-101 after reacted device hot water preheating, D-101 overhead stream 8 is recycled to reaction member, bottoms after condensing
10 are sent into aminoacid stripping tower T-101, and T-101 overhead stream 11 is condensed into logistics 16 through three stage compression, is recycled to reaction member, level-one
Knockout drum D-102 and D-103, D-102 and D- are additionally provided between compression and two-stage compression, two-stage compression and three stage compression
103 liquid phase output streams 13 and logistics 14 and tower reactor output streams 12 are mixed into logistics 15, are sent into subsequent separation process.
The molar ratio of liquefied ammonia charging 3 and propylene oxide feed 1 is 8:1.
Calandria type fixed bed reactor reaction pressure is 9MPa, and outlet temperature is 95 DEG C.Heat-insulating fixed bed reactors are anti-
Answering pressure is 9MPa, and outlet temperature is 89 DEG C.
After 90 DEG C of circulating hot water enter calandria type fixed bed reactor shell sides, 95 DEG C are heated to from calandria type fixed bed anti-
It answers device lower part to flow out, Depressor response product stream 6 is heated to 90 DEG C, is cooled to 90 DEG C of entrance using circulating hot water cooler
Calandria type fixed bed reactor shell side.The temperature difference that circulating hot water passes in and out calandria type fixed bed reactor is 5 DEG C.
Calandria type fixed bed reactor reaction heat 88.7% is recycled, and reduces process energy consumption.
94% ammonia is recycled by flash tank D-101 in logistics 6, and 6% ammonia enters aminoacid stripping tower T-101.
Aminoacid stripping tower T-101 tower top pressure 0.13MPa, 180 DEG C of bottom temperature, three stage compression compressor delivery pressure
1.4MPa, the temperature of compression condensation logistics 16 are 40 DEG C.
The yield of product isopropanolamine (including monoisopropanolamine, diisopropanolamine (DIPA) and monoisopropanolamine) is 99.6%, is produced
The content of the ethers such as triisopropanolamine propoxyl group ether is 0.14% in product, and the service life of catalyst is 12 months, regeneration week
Phase is 3~6 months.
[comparative example 1]
Isopropanolamine is produced using the method for the prior art, duct length reaches 550 meters, and wherein first-stage reactor is tubular type
500 meters of reactor (casing, hot water cooling), second reactor is 50 meters of tubular reactor (insulation), using water as catalyst, operation
Pressure is 4~10MPa, 60~120 DEG C of reaction temperature, reacts 110~120 DEG C of outlet temperature.
The yield of product isopropanolamine be 96~98%, wherein the content of the ethers such as triisopropanolamine propoxyl group ether be 0.5~
2%.
Claims (16)
1. a kind of method of liquid ammonia process for caustic soda purification production isopropanolamine, comprising the following steps:
A) fresh anhydrous liquid ammonia and circulation liquefied ammonia are mixed into liquefied ammonia charging, are mixed into charging with propylene oxide feed after preheating and mix
Object；
B) incoming mixture is sent into calandria type fixed bed reactor, and first order reaction product stream is obtained after reaction；
C) calandria type fixed bed reactor passes through circulating hot water cooling；
D) the first order reaction product stream enters heat-insulating fixed bed reactors, and the mixing isopropyl containing ammonia is obtained after the reaction was continued
Hydramine product；
E) the mixing isopropanolamine product containing ammonia depressurizes first, then after the heat exchange of reacted device cooling hot water, is first fed into sudden strain of a muscle
Steaming pot, flash drum overhead gas are condensed into condensation liquefied ammonia, are recycled to reaction member, and flash tank bottom obtains the mixing containing a small amount of ammonia
Isopropanolamine product；
F) the mixing isopropanolamine product containing a small amount of ammonia is sent into aminoacid stripping tower, and tower top obtains ammonia steam, and tower reactor is removed
The mixing isopropanolamine product of ammonia, is sent to subsequent separation process；
G) the ammonia steam is condensed into compression condensation liquefied ammonia through compressor three stage compression, is recycled to reaction member.
2. the method for liquid ammonia process for caustic soda purification production isopropanolamine according to claim 1, it is characterised in that calandria type fixed bed reactor
Flow direction with reaction mass in heat-insulating fixed bed reactors is upper entering and lower leaving, wherein calandria type fixed bed reactor reaction mass
Tube side is walked, circulating hot water walks shell side.
3. the method for liquid ammonia process for caustic soda purification production isopropanolamine according to claim 1, it is characterised in that calandria type fixed bed reactor
Reaction pressure is 7~10MPa, and temperature is 80~120 DEG C.
4. the method for liquid ammonia process for caustic soda purification production isopropanolamine according to claim 1, it is characterised in that heat-insulating fixed bed reactors
Reaction pressure is 7~10MPa, and temperature is 85~130 DEG C.
5. the method for liquid ammonia process for caustic soda purification production isopropanolamine according to claim 1, it is characterised in that fresh liquefied ammonia and propylene oxide
Molar ratio be (5:1)~(12:1).
6. the method for liquid ammonia process for caustic soda purification production isopropanolamine according to claim 1, it is characterised in that calandria type fixed bed reactor
Circulating hot water in middle shell side is identical as the reaction mass flowing direction in tube side, continuously withdraws from reaction heat, makes anti-in tube side
Answer temperature≤120 DEG C of material, pressure≤10MPa.
7. the method for liquid ammonia process for caustic soda purification production isopropanolamine according to claim 1, it is characterised in that it is solid that circulating hot water goes out shell and tube
It exchanges heat after fixed bed reactor with the mixing isopropanolamine product containing ammonia, is fixed using after cooler cooling into shell and tube
Bed reactor.
8. the method for liquid ammonia process for caustic soda purification production isopropanolamine according to claim 1, it is characterised in that it is solid that circulating hot water goes out shell and tube
It exchanges heat after fixed bed reactor with liquefied ammonia charging and the mixing isopropanolamine product containing ammonia, after cooler cooling
Into calandria type fixed bed reactor.
9. the method for liquid ammonia process for caustic soda purification production isopropanolamine according to claim 1, it is characterised in that circulating hot water passes in and out shell and tube
The temperature difference≤6 DEG C of fixed bed reactors.
10. according to claim 1 liquid ammonia process for caustic soda purification production isopropanolamine method, it is characterised in that the flash tank be level-one,
Second level or multistage, it is also possible to which rectifying column replaces.
11. the method for liquid ammonia process for caustic soda purification production isopropanolamine according to claim 1, it is characterised in that aminoacid stripping tower tower top pressure≤
0.13MPa, bottom temperature≤180 DEG C；0.11~0.13Mpa of preferred aminoacid stripping tower tower top pressure.
12. the method for liquid ammonia process for caustic soda purification production isopropanolamine according to claim 1, it is characterised in that the compressor delivery pressure
≧1.4MPa。
13. the method for liquid ammonia process for caustic soda purification production isopropanolamine according to claim 1, it is characterised in that stage compressor and second level pressure
Cooler and gas-liquid separator are equipped between contracting machine, subsequent separation process is sent in the extraction of gas-liquid separator liquid phase.
14. the method for liquid ammonia process for caustic soda purification production isopropanolamine according to claim 1, it is characterised in that split-compressor and three-level pressure
Cooler and gas-liquid separator are equipped between contracting machine, subsequent separation process is sent in the extraction of gas-liquid separator liquid phase.
15. the method for liquid ammonia process for caustic soda purification production isopropanolamine according to claim 1, it is characterised in that the compressor can also be one
Grade compression, two-stage compression, level Four compression or more compression.
16. the method for liquid ammonia process for caustic soda purification production isopropanolamine according to claim 1, it is characterised in that fresh anhydrous liquid ammonia can be exhausted
Any position is added between hot type fixed bed reactors and flash tank, can also be added at aminoacid stripping tower feed entrance point.
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| CN110327967A (en) * | 2019-07-26 | 2019-10-15 | 山东达民化工股份有限公司 | The peaceful production. art of the isopropanol of catalyst and preparation method and application catalyst |
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| WO2021099456A1 (en) * | 2019-11-20 | 2021-05-27 | Basf Se | Zeolite catalyzed process for the amination of propylene oxide |
| CN110981738B (en) * | 2019-12-30 | 2022-09-20 | 杭州新本立医药有限公司 | Synthesis method of 2-aminopropanol |
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