CN106608834A - Method for cooperatively producing ethanolamine through liquid ammonia method and ammonium hydroxide method - Google Patents

Method for cooperatively producing ethanolamine through liquid ammonia method and ammonium hydroxide method Download PDF

Info

Publication number
CN106608834A
CN106608834A CN201510690201.3A CN201510690201A CN106608834A CN 106608834 A CN106608834 A CN 106608834A CN 201510690201 A CN201510690201 A CN 201510690201A CN 106608834 A CN106608834 A CN 106608834A
Authority
CN
China
Prior art keywords
tower
ammonia
ammonia process
caustic soda
liquid ammonia
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201510690201.3A
Other languages
Chinese (zh)
Other versions
CN106608834B (en
Inventor
刘银川
胡松
杨卫胜
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
Original Assignee
China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China Petroleum and Chemical Corp, Sinopec Shanghai Research Institute of Petrochemical Technology filed Critical China Petroleum and Chemical Corp
Priority to CN201510690201.3A priority Critical patent/CN106608834B/en
Publication of CN106608834A publication Critical patent/CN106608834A/en
Application granted granted Critical
Publication of CN106608834B publication Critical patent/CN106608834B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/584Recycling of catalysts

Abstract

The invention relates to a method for cooperatively producing ethanolamine through a liquid ammonia method and an ammonium hydroxide method. The method comprises the steps that a raw material containing liquid ammonia and oxirane is sent into a liquid ammonia method reactor; after a reaction product is deaminized, mixed amine I is obtained, and recycled amine is circulated to the liquid ammonia method reactor; a raw material containing ammonium hydroxide and oxirane is introduced into an ammonium hydroxide method reactor; after a reaction product is deaminized and dehydrated, mixed amine II is obtained, and recycled amine returns to the ammonium hydroxide method reactor, wherein water circulates as a catalyst; and after being mixed, the mixed amine I and the mixed amine II are separated through a separation system comprising three or more rectifying towers, so that products, namely monoethanolamine (MEA), diethanolamine (DEA) and triethanolamine (TEA) are obtained. By means of the method, the problems that recycled amine carries water, so that activity of a liquid ammonia method catalyst is lowered, and even the liquid ammonia method catalyst is inactivated are solved; and the method can be applied to industrial production and transformation and expanding production of the ethanolamine.

Description

The method of liquid ammonia process for caustic soda purification and Ammonia Process co-producing ethanol amine
Technical field
The present invention relates to a kind of method of liquid ammonia process for caustic soda purification and Ammonia Process co-producing ethanol amine.Can be used for commercial production and the expansion of ethanolamine In transforming.
Background technology
Ethanolamine is most important product in amido alcohol, is monoethanolamine (MEA), diethanolamine (DEA) and three ethanol The general designation of amine (TEA), is water white transparency thick liquid under room temperature, have the property of amine and alcohol concurrently, of many uses, mainly For aspects such as gas purifying agent, surfactant, pesticide, polyurethane and production ethyleneamineses, with boundless application Prospect.The process route that industrial production ethanolamine is mainly reacted with excess ammonia using oxirane (EO).In water or alcohol Under the catalysis of amine, 3 active hydrogens on amino molecule are replaced by ethyl successively, generate the mixture of MEA, DEA, TEA.
It is a traditional problem that EO ammonifications prepare ethanolamine, and domestic based on Ammonia Process research, catalysis liquid ammonia process for caustic soda purification is at home Research is less.EO ammonifications are a strong exothermal reactions, and in ammonia-water systems, used as catalyst, ammonia concn more high energy consumption is more for water It is low.Due to product separate on energy consumption it is higher, and products distribution have selectivity, so being faced with production very big Competitive pressure.The research of catalysis liquid ammonia process for caustic soda purification is developed mainly for the catalyst of phase autoclave or supercritical reaction.No matter which Technique is planted, less, energy consumption size is mainly reflected in product for the flow process and energy consumption difference of rectification under vacuum ethanolamine mixtures In deamination dehydration.By contrast, as liquid ammonia process for caustic soda purification is not aqueous, it is not necessary to increase the energy consumption produced by dehydration, and product form It is adjustable.Although catalysis liquid ammonia process for caustic soda purification have the advantages that it is very many, due to the critical temperature of liquefied ammonia it is relatively low, in the reaction such as Fruit is not regulated and controled will be very high, so the low-temperature reactivity of catalyst becomes the problem stood in the breach.
Ethanolamine is heat-sensitive substance, coking of easily decomposing at high temperature, and side reaction occurs, and produces band color impurities, sternly Ghost image rings product quality and purposes.Therefore select suitable operating pressure interval, it is ensured that relatively low bottom temperature, reduce full tower Pressure drop separates most important to product purification.
CN101885686A discloses a kind of method for producing ethanolamine.Oxirane and liquefied ammonia are adopted for raw material, with ZSM-5 For catalyst, ammonia is 0.5~15 with the molar ratio of oxirane, and reaction temperature is 50~100 DEG C, and system pressure is 4~12MPa, liquid phase air speed is in 0.5~4h-1Under conditions of, reaction generates ethanolamine.Solve reaction temperature in prior art Height, the high technical problem of system pressure.
CN101555208A discloses a kind of ammonia still process dewatering process of ethanolamine.Ethanolamine mixtures containing ammonia, water are sent Enter the ethanolamine mixed liquor of ammonia still, overhead condensation liquid ammonia recovery, tower reactor water containing major part and a small amount of ammonia through flash tank, gas Steam from flash drum overhead after change, ammonia tank is returned Jing after compressor, condenser are condensed into liquefied ammonia.Ethanolamine mixed liquor is entered Dehydrating tower dehydration is recycled, and enters tail ammonia absorber spray-absorption from overhead condenser remaining ammonia out.The method can Reclaim whole water and ammonia in ethanolamine production.
In method of the liquid ammonia process for caustic soda purification with Ammonia Process co-producing ethanol amine, the ammonia of ammonia still overhead extraction can carry a small amount of water secretly, affect Liquid ammonia process for caustic soda purification reacts, therefore cannot be directly as the raw material of liquid ammonia process for caustic soda purification technique.The product Jing deamination of Ammonia Process is dehydrated by the present invention The raw material of the ammonia that reclaims afterwards and water as Ammonia Process, raw material of the ammonia reclaimed after liquid ammonia process for caustic soda purification deamination as liquid ammonia process for caustic soda purification, targetedly Solve the problems referred to above.
The content of the invention
The technical problem to be solved is that water entrainment impact liquid ammonia process for caustic soda purification reaction in ammonia is reclaimed present in joint production process Problem, there is provided a kind of method of new liquid ammonia process for caustic soda purification and Ammonia Process co-producing ethanol amine.Ammonia Process is separated in rectification under vacuum with liquid ammonia process for caustic soda purification The flow process and energy consumption difference of ethanolamine mixtures less, can share a set of distillation system, convenient to adjust load.Liquid ammonia process for caustic soda purification reacts During do not need water, make recovery ammonia efficiency high, energy consumption is low.The ammonia that the product of Ammonia Process is reclaimed Jing after deamination dehydration With water as Ammonia Process raw material, raw material of the ammonia reclaimed after liquid ammonia process for caustic soda purification deamination as liquid ammonia process for caustic soda purification reduce water to liquid ammonia process for caustic soda purification Affect, can improve product quality, extend catalyst life, increase Business Economic Benefit.
To solve above-mentioned technical problem, technical scheme is as follows:A kind of side of liquid ammonia process for caustic soda purification and Ammonia Process co-producing ethanol amine Method, comprises the following steps:
(1) raw material including liquefied ammonia and oxirane is passed through liquid ammonia process for caustic soda purification reactor and is reacted, and product is obtained Jing after deamination To mixed amine I, ammonia return liquid ammonia process for caustic soda purification reactor cycles utilization;
(2) raw material including ammonia and oxirane is passed through Ammonia Process reactor and is reacted, and product deamination is dehydrated To mixed amine II, ammonia and water return Ammonia Process reactor cycles utilization;
(3) refine from side line through monoethanolamine tower, diethanolamine tower, triethanolamine tower after mixing amine I and mixed amine II mixing Product monoethanolamine (MEA), diethanolamine (DEA), triethanolamine (TEA) are obtained, tower top light component is back to previous respectively Individual tower circulation is refined, and triethanolamine tower bottoms is used as triethanolamine certified products.
In above-mentioned technical proposal, it is preferred that liquid ammonia process for caustic soda purification reactor adopts shell and tube reactor, Ammonia Process reactor to adopt long tube Formula reactor.
In above-mentioned technical proposal, it is preferred that the operating pressure of ammonia still is 1~5MPaA, and tower top temperature is 30~90 DEG C, is returned Flow ratio is 0.1~10.It is furthermore preferred that the operating pressure of ammonia still is 1.3~3MpaA.
In above-mentioned technical proposal, it is preferred that the operating pressure of ammonia still is 1~5MPaA, and tower top temperature is 30~90 DEG C, is returned Flow ratio is 0.1~10.It is furthermore preferred that the operating pressure of ammonia still is 1.3~3MpaA.
In above-mentioned technical proposal, it is preferred that the operating pressure of dehydrating tower is 0~200kPaA, and tower top temperature is 30~60 DEG C, Reflux ratio is 1~10.It is furthermore preferred that the operating pressure of dehydrating tower is 50~150kPaA.
In above-mentioned technical proposal, it is preferred that the operating pressure of monoethanolamine tower is 0~30kPaA, and tower top temperature is 35~60 DEG C, Reflux ratio is 10~100.It is furthermore preferred that the operating pressure of monoethanolamine tower is 0~10kPaA.
In above-mentioned technical proposal, it is preferred that diethanolamine tower operating pressure is 0~20kPaA, and tower top temperature is 50~150 DEG C, Reflux ratio is 10~100.It is furthermore preferred that diethanolamine tower operating pressure is 0~5kPaA.
In above-mentioned technical proposal, it is preferred that triethanolamine tower operating pressure is 0~10kPa, and tower top temperature is 120-150 DEG C, Reflux ratio is 10~100.It is furthermore preferred that triethanolamine tower operating pressure is 0~1kPaA.
In above-mentioned technical proposal, it is preferred that monoethanolamine tower, diethanolamine tower, triethanolamine column overhead light component are followed respectively Ring is refined to the circulation of previous tower, and overhead condenser is located internally or externally with respect to rectifying column.
In above-mentioned technical proposal, it is preferred that ammonia still, ammonia still, dehydrating tower, monoethanolamine tower, diethanolamine tower, three The tower reactor reboiler of ethanolamine tower is using the one kind in falling film evaporator, climbing film evaporator and luwa evaporator.
As the amine substances such as the product ethanolamine of liquid ammonia process for caustic soda purification and Ammonia Process, diethanolamine, triethanolamine belong to temperature-sensitive Property material, can decompose coking when temperature is higher than 180 DEG C, contaminated equipment causes product yield to reduce, and affects technique Economy.Therefore, product purification tower adopts negative-pressure operation, can select high efficiency packing and condenser is built-in reducing full tower pressure drop, Tower reactor is kept to have certain light component to reduce bottom temperature, when tower reactor also can reduce the stop of tower bottoms by way of undergauge Between.
Preferred technical scheme is:Tower bottom of rectifying tower reboiler is using in falling film evaporator, climbing film evaporator and luwa evaporator One kind;Monoethanolamine column overhead light component is back to dehydrating tower, and diethanolamine column overhead light component is back to monoethanolamine tower, Triethanolamine column overhead light component is back to diethanolamine tower;Rectifying column tower top condenser is preferably molded-in in rectifying column.
Using this kind of technical scheme, the technique that liquid ammonia process for caustic soda purification produces ethanolamine with Ammonia Process is combined, effectively reclaims ammonia and water, And the ammonia for the product of Ammonia Process being reclaimed Jing after deamination dehydration respectively, used as the raw material of Ammonia Process, water is circulated as catalyst Utilize, raw material of the ammonia reclaimed after liquid ammonia process for caustic soda purification deamination as liquid ammonia process for caustic soda purification, solve water entrainment in reclaiming ammonia and liquid ammonia process for caustic soda purification is reacted Affect, refining spearation is circulated using tower top light component, using membrane evaporator, improve product yield, it is ensured that product matter Amount, obtains preferable technique effect.
Description of the drawings
Fig. 1 is the process flow diagram of liquid ammonia process for caustic soda purification of the present invention and Ammonia Process co-producing ethanol amine.
In Fig. 1, R-101 is liquid ammonia process for caustic soda purification reactor, and R-102 Ammonia Process is reactor, and T101 is ammonia still, and T102 is ammonia Recovery tower, T103 are dehydrating tower, and T104 is monoethanolamine tower, and T105 is diethanolamine tower, and T106 is triethanolamine tower, E101 is monoethanolamine overhead condenser, and 1 is liquid ammonia process for caustic soda purification product, and 2 is that ammonia still T101 reclaims ammonia, and 3 is ammonia still process Tower T101 tower bottoms, 4 is Ammonia Process product, and 5 is that recovery ammonia tower T102 reclaims ammonia, and 6 is dehydrating tower T103 tower tops Recycle-water, 7 are mixed amine I, mix the mixture of amine II and diethanolamine column overhead light component, and 8 is E101 condensed fluid, and 9 are Product monoethanolamine, 10 are monoethanolamine tower T104 tower bottoms and triethanolamine tower T106 tower top light component mixed materials, 11 is diethanolamine tower T105 tower top light components, and 12 is diethanolamine, and 13 is diethanolamine T105 tower bottoms, and 14 is three Ethanolamine tower T106 tower top light components, 15 is triethanolamine, and 16 is triethanolamine certified products.
In Fig. 1, it is passed through liquid ammonia process for caustic soda purification reactor R101 and is reacted including the raw material of liquefied ammonia and oxirane, product Jing Mixed amine I is obtained after deamination, ammonia returns liquid ammonia process for caustic soda purification reactor R101 and recycles;It is passed through including the raw material of ammonia and oxirane Ammonia Process reactor R102 is reacted, and the dehydration of product deamination obtains mixed amine II, and ammonia and water return Ammonia Process reactor R102 is recycled;Through monoethanolamine tower T104, diethanolamine tower T105, three ethanol after mixed amine I and mixed amine II mixing Amine tower T106 is refined to obtain product monoethanolamine (MEA), diethanolamine (DEA), triethanolamine (TEA), tower top from side line Light component is back to previous tower circulation respectively and refines, triethanolamine tower T106 tower reactors extraction triethanolamine certified products.
Below by embodiment, the invention will be further elaborated, but these embodiments are not anyway to the present invention's Scope is construed as limiting.
Specific embodiment
【Embodiment 1】
It is passed through liquid ammonia process for caustic soda purification reactor R101 and is reacted including the raw material of liquefied ammonia and oxirane, product is Jing after deamination To mixed amine I, ammonia returns liquid ammonia process for caustic soda purification reactor R101 and recycles;Including the raw material of ammonia and oxirane, to be passed through Ammonia Process anti- Device R102 is answered to be reacted, the dehydration of product deamination obtains mixed amine II, ammonia and water return Ammonia Process reactor R102 circulations Utilize;Through monoethanolamine tower T104, diethanolamine tower T105, triethanolamine tower T106 after mixed amine I and mixed amine II mixing It is refined to obtain product monoethanolamine (MEA), diethanolamine (DEA), triethanolamine (TEA), tower top light component difference from side line It is back to previous tower circulation refined, triethanolamine tower T106 tower reactors extraction triethanolamine certified products.
Liquid ammonia process for caustic soda purification material molar ratio is ammonia:Oxirane=7.8
Ammonia Process material molar ratio is ammonia:Oxirane=8.5
Ammonia Process reactor operation temperature is 50 DEG C, and pressure is 1.6MPaA, is calculated in mass percent, product composition For ammonia 65.9%, water 6.6%, ethanolamine 13.2%, diethanolamine 8.8%, triethanolamine 5.5%.
Liquid ammonia process for caustic soda purification reactor operation temperature is 90 DEG C, and pressure is 8.4MPaA, is calculated in mass percent, product composition For ammonia 69.0%, ethanolamine 14.9%, diethanolamine 13.8%, triethanolamine 2.3%.
Operating pressure 1.3MPaA of ammonia still T101,34 DEG C of tower top temperature, reflux ratio 0.1 are calculated in mass percent, Tower reactor ammonia<2%.
Operating pressure 1.5MPaA of ammonia still T102,39 DEG C of tower top temperature, reflux ratio 2 are calculated in mass percent, tower Kettle ammonia<2%.
Operating pressure 100kPaA of dehydrating tower, 39 DEG C of tower top temperature, reflux ratio 1 are calculated in mass percent, tower reactor water<0.1%.
Operating pressure 20kPaA of monoethanolamine tower, 40 DEG C of tower top temperature, reflux ratio 50 are calculated in mass percent, side line Monoethanolamine>99.9%, moisture<0.1%, colourity<5.
Operating pressure 6kPaA of diethanolamine tower, 170 DEG C of tower top temperature, reflux ratio 30 are calculated in mass percent, side line Diethanolamine>99.0%, moisture<0.1%, colourity<15.
Operating pressure 0.8kPaA of triethanolamine tower, 142 DEG C of tower top temperature, reflux ratio 10 are calculated in mass percent, side Line triethanolamine>99.0%, moisture<0.2%, colourity<10;Tower reactor triethanolamine>85%, moisture<0.2%, colourity<30.
In the present embodiment, ammonia still T101, ammonia still T102, dehydrating tower, monoethanolamine tower, diethanolamine tower, three second The bottom temperature of hydramine tower is equal<180℃.
【Embodiment 2】
Embodiment is same as Example 1, except for the difference that the operating parameter of each tower.
Operating pressure 5MPaA of ammonia still T101,89 DEG C of tower top temperature, reflux ratio 1 are calculated in mass percent, tower reactor Ammonia<2%.
Operating pressure 5MPaA of ammonia still T102,89 DEG C of tower top temperature, reflux ratio 1 are calculated in mass percent, tower reactor Ammonia<2%.
Operating pressure 150kPaA of dehydrating tower, 40 DEG C of tower top temperature, reflux ratio 8 are calculated in mass percent, tower reactor water<0.1%.
Operating pressure 30kPaA of monoethanolamine tower, 40 DEG C of tower top temperature, reflux ratio 50 are calculated in mass percent, side line Monoethanolamine>99.9%, moisture<0.1%, colourity<5.
Operating pressure 1kPaA of diethanolamine tower, 68 DEG C of tower top temperature, reflux ratio 30 are calculated in mass percent, side line Diethanolamine>99.0%, moisture<0.1%, colourity<10.
Operating pressure 0.3kPaA of triethanolamine tower, 125 DEG C of tower top temperature, reflux ratio 50 are calculated in mass percent, side Line triethanolamine>99.0%, moisture<0.2%, colourity<10;Tower reactor triethanolamine>85%, moisture<0.2%, colourity<30.
In the present embodiment, ammonia still T101, ammonia still T102, dehydrating tower, monoethanolamine tower, diethanolamine tower, three second The bottom temperature of hydramine tower is equal<180℃.
【Embodiment 3】
Embodiment is same as Example 1, except for the difference that the operating parameter of each tower.
Operating pressure 1.8MPaA of ammonia still T101,46 DEG C of tower top temperature, reflux ratio 10 are calculated in mass percent, Tower reactor ammonia<2%.
Operating pressure 2MPaA of ammonia still T102,50 DEG C of tower top temperature, reflux ratio 8 are calculated in mass percent, tower reactor Ammonia<2%.
Operating pressure 170kPaA of dehydrating tower, 43 DEG C of tower top temperature, reflux ratio 0.5 are calculated in mass percent, tower reactor water <0.1%.
Operating pressure 3kPaA of monoethanolamine tower, 40 DEG C of tower top temperature, reflux ratio 30 are calculated in mass percent, side line Monoethanolamine>99.9%, moisture<0.1%, colourity<3.
Operating pressure 0.1kPaA of diethanolamine tower, 52 DEG C of tower top temperature, reflux ratio 40 are calculated in mass percent, side line Diethanolamine>99.0%, moisture<0.1%, colourity<5.
Operating pressure 0.1kPaA of triethanolamine tower, 128 DEG C of tower top temperature, reflux ratio 80 are calculated in mass percent, side Line triethanolamine>99.0%, moisture<0.2%, colourity<10;Tower reactor triethanolamine>85%, moisture<0.2%, colourity<30.
In the present embodiment, ammonia still T101, ammonia still T102, dehydrating tower, monoethanolamine tower, diethanolamine tower, three second The bottom temperature of hydramine tower is equal<180℃.
【Embodiment 4】
Embodiment is same as Example 1, and except for the difference that raw material is different from the operating parameter of each tower.
Liquid ammonia process for caustic soda purification material molar ratio is ammonia:Oxirane=26
Ammonia Process material molar ratio is ammonia:Oxirane=21
Ammonia Process reactor operation temperature is 50 DEG C, and pressure is 1.6MPaA, is calculated in mass percent, product composition For ammonia 83%, water 3%, ethanolamine 7%, diethanolamine 4%, triethanolamine 3%.
Liquid ammonia process for caustic soda purification reactor operation temperature is 90 DEG C, and pressure is 8.4MPaA, is calculated in mass percent, product composition For ammonia 88%, ethanolamine 11%, diethanolamine 0.23%, triethanolamine 0.06%.
Operating pressure 3MPaA of ammonia still T101,66 DEG C of tower top temperature, reflux ratio 3 are calculated in mass percent, tower reactor Ammonia<2%.
Operating pressure 1.3MPaA of ammonia still T102,34 DEG C of tower top temperature, reflux ratio 2 are calculated in mass percent, tower Kettle ammonia<2%.
Operating pressure 80kPaA of dehydrating tower, 36 DEG C of tower top temperature, reflux ratio 1 are calculated in mass percent, tower reactor water<0.1%.
Operating pressure 12kPaA of monoethanolamine tower, 40 DEG C of tower top temperature, reflux ratio 50 are calculated in mass percent, side line Monoethanolamine>99.9%, moisture<0.1%, colourity<5.
Operating pressure 5kPaA of diethanolamine tower, 108 DEG C of tower top temperature, reflux ratio 80 are calculated in mass percent, side line Diethanolamine>99.0%, moisture<0.1%, colourity<15.
Operating pressure 0.5kPaA of triethanolamine tower, 134 DEG C of tower top temperature, reflux ratio 90 are calculated in mass percent, side Line triethanolamine>99.0%, moisture<0.2%, colourity<10;Tower reactor triethanolamine>85%, moisture<0.2%, colourity<30.
In the present embodiment, ammonia still T101, ammonia still T102, dehydrating tower, monoethanolamine tower, diethanolamine tower, three second The bottom temperature of hydramine tower is equal<180℃.
【Comparative example 1】
Embodiment is identical with embodiment 1~4, except for the difference that:The operating pressure of monoethanolamine tower is improved to 50kPaA, tower Kettle temperature degree>180 DEG C, ethanolamine product yield reduces >=1%, and diethanolamine, triethanolamine product colourity increase by 5~40.

Claims (10)

1. a kind of method of liquid ammonia process for caustic soda purification and Ammonia Process co-producing ethanol amine, mainly includes the following steps that:
(1) raw material including liquefied ammonia and oxirane is passed through liquid ammonia process for caustic soda purification reactor and is reacted, and product is obtained Jing after deamination To mixed amine I, ammonia return liquid ammonia process for caustic soda purification reactor cycles utilization;
(2) raw material including ammonia and oxirane is passed through Ammonia Process reactor and is reacted, product deamination, dehydration Mixed amine II is obtained, ammonia returns Ammonia Process reactor cycles and utilizes, and water circulation is used as catalyst;
(3) refine from side line through monoethanolamine tower, diethanolamine tower, triethanolamine tower after mixing amine I and mixed amine II mixing Product monoethanolamine (MEA), diethanolamine (DEA), triethanolamine (TEA) are obtained, tower top light component is back to previous respectively Individual tower circulation is refined, and triethanolamine tower bottoms is used as triethanolamine certified products.
2. the method for liquid ammonia process for caustic soda purification and Ammonia Process co-producing ethanol amine according to claim 1, it is characterised in that the step (2) Middle product deamination operation includes ammonia still and recovery ammonia tower.
3. the method for liquid ammonia process for caustic soda purification and Ammonia Process co-producing ethanol amine according to claim 2, it is characterised in that the ammonia still Operating pressure is 1~5MPaA, and tower top temperature is 30~90 DEG C, and reflux ratio is 0.1~10.
4. the method for liquid ammonia process for caustic soda purification and Ammonia Process co-producing ethanol amine according to claim 2, it is characterised in that the recovery ammonia tower Operating pressure be 1~5MPaA, tower top temperature be 30~90 DEG C, reflux ratio be 0.1~10.
5. the method for liquid ammonia process for caustic soda purification and Ammonia Process co-producing ethanol amine according to claim 1, it is characterised in that the dehydrating tower Operating pressure is 0~200kPaA, and tower top temperature is 30~60 DEG C, and reflux ratio is 1~10, and bottom temperature is less than 180 DEG C.
6. the method for liquid ammonia process for caustic soda purification and Ammonia Process co-producing ethanol amine according to claim 1, it is characterised in that the monoethanolamine The operating pressure of tower is 0~30kPaA, and tower top temperature is 35~60 DEG C, and reflux ratio is 10~100, and bottom temperature is less than 180 DEG C.
7. the method for liquid ammonia process for caustic soda purification and Ammonia Process co-producing ethanol amine according to claim 1, it is characterised in that the diethanol Amine tower operating pressure is 0~20kPaA, and tower top temperature is 50~150 DEG C, and reflux ratio is 10~100, and bottom temperature is less than 180 ℃。
8. the method for liquid ammonia process for caustic soda purification and Ammonia Process co-producing ethanol amine according to claim 1, it is characterised in that the triethanolamine Tower operating pressure is 0~10kPaA, and tower top temperature is 120-150 DEG C, and reflux ratio is 10~100, and bottom temperature is less than 180 DEG C.
9. the method for liquid ammonia process for caustic soda purification and Ammonia Process co-producing ethanol amine according to claim 1, it is characterised in that the monoethanolamine Tower, diethanolamine tower, triethanolamine column overhead light component are recycled to previous tower circulation respectively and refine, and overhead condenser is built-in In or be placed on rectifying column.
10. the method for liquid ammonia process for caustic soda purification and Ammonia Process co-producing ethanol amine according to claim 1, it is characterised in that the ammonia still, Recovery ammonia tower, dehydrating tower, monoethanolamine tower, diethanolamine tower, the tower reactor reboiler of triethanolamine tower using falling film evaporator, One kind in climbing film evaporator and luwa evaporator.
CN201510690201.3A 2015-10-22 2015-10-22 The method of liquid ammonia process for caustic soda purification and Ammonia Process co-producing ethanol amine Active CN106608834B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510690201.3A CN106608834B (en) 2015-10-22 2015-10-22 The method of liquid ammonia process for caustic soda purification and Ammonia Process co-producing ethanol amine

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510690201.3A CN106608834B (en) 2015-10-22 2015-10-22 The method of liquid ammonia process for caustic soda purification and Ammonia Process co-producing ethanol amine

Publications (2)

Publication Number Publication Date
CN106608834A true CN106608834A (en) 2017-05-03
CN106608834B CN106608834B (en) 2018-10-23

Family

ID=58610348

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510690201.3A Active CN106608834B (en) 2015-10-22 2015-10-22 The method of liquid ammonia process for caustic soda purification and Ammonia Process co-producing ethanol amine

Country Status (1)

Country Link
CN (1) CN106608834B (en)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1519225A (en) * 2003-02-03 2004-08-11 ��ʽ�����ձ���ý Process for prepn. of high pureness trialkanolamine
CN101555208A (en) * 2009-02-24 2009-10-14 湖北仙磷化工有限责任公司 Ammonia-evaporating dewatering technique in production of neovaricaine
CN101613289A (en) * 2009-05-12 2009-12-30 嘉兴金燕化工有限公司 The abbreviated system that thanomin is produced
CN101723840A (en) * 2008-10-20 2010-06-09 苏舍化学技术有限公司 Method and plant for the production of ethanol amines
CN101735077A (en) * 2009-12-11 2010-06-16 广西壮族自治区化工研究院 Production method and production equipment for synthesizing ethanolamine by ethylene oxide
CN103772211A (en) * 2012-10-25 2014-05-07 中国石油化工股份有限公司 Method for producing ethanol amine by using liquid ammonia method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1519225A (en) * 2003-02-03 2004-08-11 ��ʽ�����ձ���ý Process for prepn. of high pureness trialkanolamine
CN101723840A (en) * 2008-10-20 2010-06-09 苏舍化学技术有限公司 Method and plant for the production of ethanol amines
CN101555208A (en) * 2009-02-24 2009-10-14 湖北仙磷化工有限责任公司 Ammonia-evaporating dewatering technique in production of neovaricaine
CN101613289A (en) * 2009-05-12 2009-12-30 嘉兴金燕化工有限公司 The abbreviated system that thanomin is produced
CN101735077A (en) * 2009-12-11 2010-06-16 广西壮族自治区化工研究院 Production method and production equipment for synthesizing ethanolamine by ethylene oxide
CN103772211A (en) * 2012-10-25 2014-05-07 中国石油化工股份有限公司 Method for producing ethanol amine by using liquid ammonia method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
孙英杰: ""乙醇胺生产技术和应用"", 《精细与专用化学品》 *

Also Published As

Publication number Publication date
CN106608834B (en) 2018-10-23

Similar Documents

Publication Publication Date Title
CN104761429B (en) A kind of method for producing dimethyl carbonate and ethylene glycol
CN107739301B (en) Polymethoxy dimethyl ether synthesis system and process
CN105001087A (en) Method and apparatus for producing formic esters by comprehensively utilizing metronidazole hydroxylation synthesis wastewater
CN104529763A (en) Process and device for synthesizing ethyl formate with reactive distillation dividing wall column
CN101830812A (en) Process for continuously producing N-monomethylethanolamine
CN102276485A (en) Method for producing dimethylaminoethylacrylate
CN106831315A (en) A kind of continuous production method of chloroethanes
CN106608832B (en) The process of liquid ammonia process for caustic soda purification and Ammonia Process co-producing ethanol amine
CN106542975B (en) The method of continuous production high-purity triethylene glycol
WO2021003974A1 (en) Method for preparing propylene carbonate on the basis of carbon dioxide raw material
CN104387236A (en) Trigeneration continuous production method for propiolic alcohol, 1,4-butinodiol and urotropine
CN103113257A (en) Continuous reactive distillation equipment for synthesising methoxylamine hydrochloride and process thereof
CN103524478B (en) Device and method for shortening ketalation time in ibuprofen synthesis process
CN106608865B (en) Power-economizing method for ethylene carbonate Lipase absobed
CN109748791B (en) Energy-saving method for producing dimethyl adipate
CN105085282B (en) Preparation method for alkyl alcohol amine
CN101898930A (en) Device for producing cyclohexane by adding hydrogen in benzene and synthesis process
CN112387077B (en) Tail gas absorption device and method for distillation tower for producing ethyleneimine
CN106608834A (en) Method for cooperatively producing ethanolamine through liquid ammonia method and ammonium hydroxide method
CN106349207A (en) Process for preparing cyclic organic carbonic ester indirectly from CO2 and polyhydric alcohol
CN101993381A (en) Synthetic method of 3-amino-1, 2-propanediol
CN106957284B (en) A kind of separating-purifying process for refining of tertiary carbonic acid glycidyl ester crude product
CN102502697A (en) Method for recovering ammonia in morpholine solution
CN107973728A (en) System and technique a kind of while that prepare methyl carbamate, dimethyl carbonate
CN210261603U (en) N-methyldiethanolamine production device

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant