CN106608831A - Recycling method of ammonia in ethanol amine combined production - Google Patents
Recycling method of ammonia in ethanol amine combined production Download PDFInfo
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- CN106608831A CN106608831A CN201510689497.7A CN201510689497A CN106608831A CN 106608831 A CN106608831 A CN 106608831A CN 201510689497 A CN201510689497 A CN 201510689497A CN 106608831 A CN106608831 A CN 106608831A
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- ammonia
- monoethanolamine
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- stripping tower
- recovery method
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/10—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/024—Purification
Abstract
The invention provides a recycling method of ammonia high in ammonia recycling rate and low in equipment investment, and more specifically discloses a recycling method of ammonia in ethanol amine combined production. The recycling method comprises following steps: reaction products of liquid ammonia method and ammonia water method are mixed, and are delivered into an ammonia stripping tower, and an obtained gas phase is subjected to condensation, and is recycled back to a reactor; a residue of the ammonia stripping tower is delivered into an ammonia flash tank, a gas phase obtained from the top of the ammonia flash tank is subjected to condensation, and is delivered into an ammonia water method reaction unit as a reaction raw material, and a liquid phase obtained via the bottom of the ammonia flash tank is delivered into a dehydrating tower for dehydrating; and a residue of the dehydrating tower is delivered into an ethanol amine product refining unit. A gas phase outlet on the top of the ammonia stripping tower is provided with a high-efficiency gas-liquid separator so as to avoid gas phase water entrainment content exceeding standards, and reducing of the selectivity and service life of liquid ammonia method catalysts. The recycling method possesses following advantages: no low temperature cryogen is needed, no compressor is needed, equipment investment is saved, ammonia recovery rate is high, and the recycling method can be adopted in industrial production of ethanol amine, and is especially suitable for capacity expansion reformation of ammonia water method.
Description
Technical field
The present invention relates to monoethanolamine production field, it particularly relates to a kind of Ammonia Process and liquid ammonia process for caustic soda purification co-producing ethanol amine technique
In ammonia recovery method.
Background technology
Monoethanolamine is monoethanolamine (MEA), diethanol amine (DEA), the general name of triethanolamine (TEA), is ammonia point
Hydrogen atom in son is by ethoxy (- CH2CH2OH the product after) replacing successively.It derives as oxirane is important
One of thing, is product most with practical value in amino alcohol, and yield accounts for the 90%-95% of amino alcohol total output.Ethanolamine molecules
In have nitrogen-atoms and hydroxyl, therefore have the chemical property of amine and alcohol concurrently.At present, the most important purposes of ethanolamine product is production table
Face activating agent, be additionally operable in addition medicine and agricultural chemicals, TEXTILE CHEMICALS, gas purifying agent, accelerator for cement slurry, petroleum additive,
Bating agent, lubricating oil corrosion inhibitor, soot prevention compound etc..Wherein diethanol amine will be that monoethanolamine market is maximum
Consumption kind, is mainly used in glyphosate herbicidal production；Increasing is occurred by the stimulation of the treating of wood market demand in MEA；
And the triethanolamine market demand will be stimulated by personal care product and fabric softening growth in strong demand.
Under the support of the economic strong growth of the nations of China and India, 3 to five years futures Asia monoethanolamine demand is estimated will also be with average annual
6～7% speedup continues to increase.Same period US and European demand year speedup is only 2～3%.It is sub- in recent years according to ICIS data
The monoethanolamine consumption demand of continent area is presented rapid growth trend, reaches 560,000 tons within 2011, accounts for three points of world market demand
One of.Particularly Chinese growth in strong demand is just promoting Asia constantly to expand production capacity.
At present, the external relevant enterprise for being engaged in monoethanolamine production mainly has Dow chemical, and BASF AG, Huntsman is public
Department, Nippon Shokubai companies etc..Monoethanolamine enterprise can be divided into by four classes according to the concentration of ammonia in the raw material for using：1)
SD companies of the U.S. adopt the ammoniacal liquor of low concentration for reaction raw materials, by the ammoniacal liquor of EO and 20～30wt% (including fresh material
With circulation material), and circulation MEA reacted in fixed bed reactors (with MEA adjust product
Structure), NH3/ EO=10:1,100 DEG C of reaction temperature, system pressure 0.5MPa, after reaction product through separation,
Rectifying respectively obtains highly purified MEA, DEA, TEA, and its relative amount is respectively 69wt%, 21wt%, 10wt%,
Excess of ammonia Jing vacuum distillations in reaction system are reclaimed, residual ammonia repetitive cycling in the form of ammoniacal liquor.Because the water in system contains
Amount is high, heats up in reaction high with power consumption in temperature-fall period, and product is soluble in water, and dehydration energy is high.Therefore, although low dense
The ammoniacal liquor synthesising method reacting condition of degree is gentle, but its energy consumption is too high, will gradually be eliminated.2) Dow Chemical Company is adopted
The ammoniacal liquor of middle and high concentration is reaction raw materials, and ammonia concn is 35～50wt%, and system pressure is 3.5MPa, and reaction temperature is
115～130 DEG C.First using the method for high vacuum flash distillation come the ammonia in recovery system, product is distributed by original Dow Chemical Company
The content of material ammonia comes modulation, and the said firm aborning using EO and the combined production device of monoethanolamine.3) BASF AG adopts
The ammoniacal liquor of high concentration is raw material, and ammonia concn is in more than 90wt%, system pressure 10MPa, NH3/ EO=15～25:1, stop
3～30min of time is stayed, using level Four thermal insulation tubular reactor, EO is in inferior to different nodes and enters reactor in batches, instead
Material reduces pressure in flash column after answering, and boils off most of ammonia, and ammonia condensing is returned into liquefied ammonia, and residual ammonia is steamed in 0.4MPa, is used
The water of dehydrating tower is absorbed into after weak aqua ammonia, then is configured to the participation reaction of 90% concentrated ammonia liquor with liquefied ammonia.Using high concentration ammonia
Become the trend of Ammonia Process technique, Ammonia Process can obtain reconciliation of inventory composition, but have that product accessory substance is more, separating difficulty is high,
The problems such as reaction heat cannot be reclaimed.4) Nippon Shokubai companies are with liquefied ammonia as raw material, and the zeolite being modified with La is as catalysis
Agent, the generation diethanol amine of high selectivity, and have been carried out industrial applications.Its process conditions is as follows：It is in reaction temperature
100～110 DEG C, pressure is 12～15MPa, and liquid phase air speed is 8～10h-1When, using fixed bed reactors, diethanol amine
One way weight selectivities 41% or so；By circulating MEA, the weight selectivities of its diethanol amine can reach 81%,
And oxirane can be realized converting completely.The process selectivity is high, and it is easy that product is separated, reaction heat can centralized recovery utilize,
Energy consumption is low, is the developing direction of monoethanolamine technology, but its catalyst on-stream cycle time short (only several days), it is to be badly in need of solving
Problem.
The advantage of low ammonia concn technique is that reaction condition is gentle, side reaction is few, has the disadvantage high energy consumption, high ammonia concn technique
It is then just contrary.No matter which kind of technique, less, energy consumption is big for the flow process and energy consumption difference of rectification under vacuum separating alcohol amine blends
Little difference is mainly reflected in the deamination dewatering process of reactant.Traditional Ammonia Process production monoethanolamine technique, product proportion is adjusted
Section is difficult, and by-product species are more, quantity big, and the water as catalyst to be separated, and energy consumption is big, and economy is unfavorable for market
Competition.
The liquid ammonia process for caustic soda purification production monoethanolamine for researching and developing both at home and abroad at present does not need water as catalyst, and adopts zeolite molecules
Sieve reacts as catalyst, oxirane and liquefied ammonia under liquid-phase condition, and reaction is three step consecutive reactions, generates a second
Hydramine (MEA), three kinds of products of diethanol amine (DEA) and triethanolamine (TEA), reaction equation is as follows：
Because the chemical property of oxirane is extremely active, self-polymeric reaction is prone to when concentration is higher and generates polyoxyethylene
Or the high boiling substance such as polyethers；Or with the material containing hydroxyl in molecule, such as water, alcohols etc., occur hydration etc. reaction life
Into high boiling substances such as polyalcohol, polyalcohol ethers, these height boiling materials are referred to as higher ethanol amine (HEA), into low attached value
Triethanolamine (TEA) seconds among.Above-mentioned side reaction for oxirane and ammonia occur main reaction --- ammonolysis are anti-
All it is harmful side reaction for answering, the high boiling point by-products produced HEA of generation not only reduces the yield of major product, wastes
EO raw materials, and severely impacted the quality of ethanolamine product, it is therefore desirable to control in separation process bottom temperature not
More than 180 DEG C, while controlling in liquid ammonia process for caustic soda purification technique water content in liquefied ammonia.Individually monoethanolamine is produced using liquid ammonia process for caustic soda purification, liquefied ammonia is returned
During receipts, need to adopt the liquefied ammonia either cryogenic coolant such as freon or compressor, increase equipment investment and public work is taken
With.If liquid ammonia process for caustic soda purification and Ammonia Process combined, two kinds of product are sent into into a set of piece-rate system simultaneously, can be saved
Save equipment investment and utility cost, improve product quality.
Existing process mainly carries out monoethanolamine production using tubular reactor, and has made many improvement and innovation to reaction process.
Tubular type is adopted in the patents such as CN101148412A, CN101148413A, CN101613289A, CN101613290A
Reactor, pipe is outer to remove heat using hot water.Wherein CN101148412A clicks through EO techniques more using, reduces the circulation of ammonia
Amount, can greatly save the energy consumption of product ammonia still process (and removing the water brought into ammonia), so that ammonia still process dehydration can be saved
More than the 80～90% of energy consumption；Reaction tube one is managed on earth in CN101148413A, is not segmented, is not inserted into heat exchanger, and its is anti-
Should manage with water leg, the water in chuck is reverse with material in pipe and flow, continuously remove reaction heat, make the material in pipe can be with
Maintain than relatively low reaction temperature (≤100 DEG C), pressure is 6～7MPa.
In order to reduce the side reaction of EO, process safety is improved, can take reduces the water content of liquefied ammonia, reduce reaction zone ring
The concentration of oxidative ethane, it is strict to control the measures such as reactor temperature rise to improve ethanolamine product yield, reduce the growing amount of accessory substance.
Liquid ammonia process for caustic soda purification production monoethanolamine technique adopts anhydrous liquid ammonia, it is possible to decrease the generation probability and content of polyethers and polyol ethers；Carry simultaneously
High ammonia alkane ratio is to 8：1～12：1 (mol ratio), to reduce the concentration of oxirane, reduces the probability of oxirane autohemagglutination；
By continuously withdrawing reaction heat using circulating hot water, control reactor temperature rise waits measure in rational scope, can improve product
Yield, suppression accessory substance are generated, and product quality is high, energy consumption is low, non-wastewater discharge, safety and environmental protection.
The capacity expansion revamping of monoethanolamine technique is produced for Ammonia Process, Ammonia Process and liquid ammonia process for caustic soda purification are combined, can suitably reduce ammonia
Water law production scale, using the original ammonia still process dehydration device of Ammonia Process and product purification device, reduces equipment investment.
The content of the invention
It is to save recovery ammonia and the investment of ethanolamine product separation equipment in liquid ammonia process for caustic soda purification and Ammonia Process joint production process that the present invention is, with
And Ammonia Process and liquid ammonia process for caustic soda purification product mixing focus on during, a small amount of liquid phase water of aminoacid stripping tower top clip band, circulate into
Enter liquid ammonia process for caustic soda purification reaction member, the problems such as cause catalyst activity to reduce, there is provided the ammonia in a kind of new monoethanolamine joint production process is returned
Receiving method, during the recovery ammonia that the method is used in monoethanolamine joint production process, low with equipment investment, catalyst activity height etc. is excellent
Point.
To solve above-mentioned technical problem, technical scheme is as follows：A kind of ammonia recovery method in monoethanolamine joint production process,
Characterized in that, the method is followed the steps below：
(1) aminoacid stripping tower will be delivered to after liquid ammonia process for caustic soda purification and the mixing of Ammonia Process product, gas phase is reclaimed after condensation and is recycled to
Reactor；
(2) aminoacid stripping tower kettle liquid delivers to ammonia flash tank, and Ammonia Process reaction member work is delivered to after ammonia flash drum overhead vapor condensation
For reaction raw materials, ammonia flash tank bottom liquid phase delivers to dehydrating tower dehydration；
(3) dehydrating tower kettle liquid delivers to ethanolamine product refined unit, and it is anti-that top liquid of the dehydration tower top containing a small amount of ammonia delivers to Ammonia Process
Unit is answered as catalyst.
Because liquid ammonia process for caustic soda purification product form depends primarily on NH in charging3With the ratio (NH of EO3/ EO mol ratios, ammonia alkane ratio),
The present invention considers that ammonia alkane ratio is 4 in liquid ammonia process for caustic soda purification technique from product slates ratio and energy-saving angle：1～16：1 (mol ratio),
Preferably 6：1～10：1, the concentration of oxirane can be reduced, the probability of oxirane autohemagglutination is reduced, obtain suitable one
Monoethanolamine, diethanol amine, triethanolamine product proportion.Adjustment can be reached by adjusting ammonia alkane ratio according to the market demand simultaneously
The purpose of product proportion.
In above-mentioned technical proposal, it is preferable that count ammonia content as 60～85% with mass fraction in liquid ammonia process for caustic soda purification product, also contain
Having also contain monoethanolamine, diethanol amine, triethanolamine and heavy constituent.
Result of calculation shows that the ammonia concn in Ammonia Process technique productions monoethanolamine has a significant impact to energy consumption, and ammonia concn is got over
Height, separating energy consumption is lower.
In above-mentioned technical proposal, it is preferable that ammonia content is in terms of mass fraction in Ammonia Process product in the present invention
50～75%, water content is 1～10%, also containing also containing monoethanolamine, diethanol amine, triethanolamine and heavy constituent.
Simultaneously because monoethanolamine is heat-sensitive substance, it is the key factor to be considered that operation temperature is limited during ammonia is reclaimed.
180 DEG C of aminoacid stripping tower bottom temperature, flash tank operation temperature and dehydrating tower bottom temperature ＜ are controlled in the present invention.
Due to not aqueous in liquid ammonia process for caustic soda purification, to avoid bottom temperature more than 180 DEG C, aminoacid stripping tower is reclaimed during ammonia, can be by portion
Ammonia is divided to be depressed into tower reactor, the recovery ammonia of this portion of residual is extremely difficult, processing method is by remaining ammonia flash distillation or other
Method is separated, then is reclaimed or straight using cryogenic media such as propylene, freon with cooling water condensation with after compressor compresses
Connect condensation to reclaim, but equipment investment and operating cost will be increased.
Liquid ammonia process for caustic soda purification and Ammonia Process coproduction can change this unfavorable situation, because containing water in product, suitably grasp
Under making pressure, bottom temperature can be more easily controlled less than 180 DEG C, remaining liquefied ammonia divides together in dehydration tower top and water
Separate out and, used as the catalyst of Ammonia Process technique, liquefied ammonia therein is used as raw material for water.
Aminoacid stripping tower top is provided with wire packing, by the most of removing of the liquid carried secretly in gas phase.
In above-mentioned technical proposal, it is preferable that catalyst is adhesiveless ZSM-5 zeolite molecular sieve in liquid ammonia process for caustic soda purification technique.
Because catalyst is adhesiveless ZSM-5 zeolite molecular sieve in liquid ammonia process for caustic soda purification technique, molecular sieve has strict demand to water,
Seek water content no more than 200ppm in liquefied ammonia.Therefore, high efficient gas and liquid separator is set in aminoacid stripping tower top gaseous phase outlet,
By the liquid carried secretly in gas phase further removing as little as 100ppm (mainly water).
In above-mentioned technical proposal, it is preferable that aminoacid stripping tower theoretical cam curve is 10～30, tower top operating pressure is 1.0～3.0
MPaG, tower top operation temperature is 30～80 DEG C.
In above-mentioned technical proposal, it is preferable that ammonia flash tank operating pressure is 0.3～1.0MPaG, operation temperature is 130～170
℃。
In above-mentioned technical proposal, it is preferable that dehydration column overhead operating pressure is -0.1～0.3MPaG, tower top operation temperature is
60～120 DEG C.
Therefore, technique of the invention can be saved significantly in equipment investment and production process energy resource consumption, operating cost,
Production cost is reduced, technical process environmental protection achieves preferable technique effect.
Description of the drawings
Fig. 1 is present invention process schematic flow sheet.
In Fig. 1, C101 is aminoacid stripping tower, and S101 is high efficient gas and liquid separator, and V101 is ammonia flash tank, and C102 is de-
Water tower, E101 is aminoacid stripping tower condenser, and E102 is secondary condenser.1 is liquid ammonia process for caustic soda purification product, and 2 is that Ammonia Process is anti-
Answer product, 3 is aminoacid stripping tower top gas, 4 is ammonia, 5 is liquefied ammonia, 6 is reclaim liquid phase, 7 is aminoacid stripping tower kettle liquid, 8
For fixed gas, 9 is secondary recovery liquid, and 10 is flash tank bottom liquid, and 11 are dehydration liquid of top of the tower, and 12 is dehydrating tower kettle liquid.
In Fig. 1, aminoacid stripping tower C101, ammonia stripping are delivered to after liquid ammonia process for caustic soda purification product 1 and the mixing of Ammonia Process product 2
After the drop 6 that high efficient gas and liquid separator S101 separates entrainment, drop 6 is back to aminoacid stripping tower C101 to tower overhead gas 3,
The liquefied ammonia 5 after aminoacid stripping tower condenser E101 condensations of ammonia 4 is recycled to liquid ammonia process for caustic soda purification and Ammonia Process reaction member as reaction
Raw material, aminoacid stripping tower kettle liquid 7 delivers to ammonia flash tank V101, and after vacuum flashing, gas phase is secondary condenser portion through E102
After dividing condensation, the liquefied ammonia 9 containing a small amount of water delivers to Ammonia Process unit as reaction raw materials, and fixed gas 8 delivers to ammonia absorber absorption
Afterwards as Ammonia Process unit catalyst, flash tank bottom liquid 10 delivers to dehydrating tower C102, and liquid of top of the tower 11 mainly contains water, micro-
The ammonia of amount delivers to Ammonia Process unit as catalyst, and dehydrating tower kettle liquid 12 is mixed ethanol amine product, including monoethanolamine,
Diethanol amine, triethanolamine and heavy constituent.
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】
As shown in figure 1, liquid ammonia process for caustic soda purification product 1 and Ammonia Process product 2 deliver to aminoacid stripping tower C101, ammonia after mixing
After the drop 6 that high efficient gas and liquid separator S101 separates entrainment, drop 6 is back to aminoacid stripping tower to stripping tower overhead gas 3
C101, liquefied ammonia 5 is recycled to liquid ammonia process for caustic soda purification to ammonia 4 and Ammonia Process reaction member is made after aminoacid stripping tower condenser E101 condensations
For reaction raw materials, aminoacid stripping tower kettle liquid 7 delivers to ammonia flash tank V101, and after vacuum flashing, gas phase is two grades cold through E102
After condenser partial condensation, the liquefied ammonia 9 containing a small amount of water delivers to Ammonia Process unit as reaction raw materials, and fixed gas 8 delivers to ammonia absorption
Tower delivers to dehydrating tower C102 after absorbing as Ammonia Process unit catalyst, flash tank bottom liquid 10, and liquid of top of the tower 11 is mainly contained
Water, micro ammonia delivers to Ammonia Process unit as catalyst, and dehydrating tower kettle liquid 12 is mixed ethanol amine product, including one
Monoethanolamine, diethanol amine, triethanolamine and heavy constituent.
Liquid ammonia process for caustic soda purification product 1, in terms of mass fraction, ammonia content is 60%, also contains monoethanolamine, diethanol amine, three
Monoethanolamine and heavy constituent.
Ammonia Process product 2, in terms of mass fraction, ammonia content is 75%, and water content is 3%, also contains monoethanolamine,
Diethanol amine, triethanolamine and heavy constituent.
Aminoacid stripping tower theoretical cam curve is 10, and operating pressure is 1.4MPaG, and operation temperature is 35 DEG C.
Ammonia flash tank operating pressure is 0.3MPaG, and operation temperature is 155 DEG C.
Dehydrating tower operating pressure is -0.08MPaG, and operation temperature is 65 DEG C.
Mixed ethanol amine product 12, in terms of mass fraction, ammonia≤10ppm, water≤50ppm, monoethanolamine=45%, two
Monoethanolamine=40%, triethanolamine=15%.
In liquid ammonia recovery 5 water content be 20ppm, ammonia recovery >=99.9%.
In the present embodiment, 180 DEG C of the equal ＜ of aminoacid stripping tower bottom temperature, flash tank operation temperature and dehydrating tower bottom temperature.
【Embodiment 2】
Liquid ammonia process for caustic soda purification product 1, in terms of mass fraction, ammonia content is 75%, also contains monoethanolamine, diethanol amine, three
Monoethanolamine and heavy constituent.
Ammonia Process product 2, in terms of mass fraction, ammonia content is 62%, and water content is 6%, also contains monoethanolamine,
Diethanol amine, triethanolamine and heavy constituent.
Aminoacid stripping tower theoretical cam curve is 20, and operating pressure is 1.6MPaG, and operation temperature is 45 DEG C.
Ammonia flash tank operating pressure is 0.45MPaG, and operation temperature is 160 DEG C.
Dehydrating tower operating pressure is -0.05MPaG, and operation temperature is 68 DEG C.
Mixed ethanol amine product 12, in terms of mass fraction, ammonia≤10ppm, water≤50ppm, monoethanolamine=50%, two
Monoethanolamine=38%, triethanolamine=12%.
In liquid ammonia recovery 5 water content be 25ppm, ammonia recovery >=99.9%.
In the present embodiment, 180 DEG C of the equal ＜ of aminoacid stripping tower bottom temperature, flash tank operation temperature and dehydrating tower bottom temperature.
【Embodiment 3】
Liquid ammonia process for caustic soda purification product 1, in terms of mass fraction, ammonia content is 70%, also contains monoethanolamine, diethanol amine, three
Monoethanolamine and heavy constituent.
Ammonia Process product 2, in terms of mass fraction, ammonia content is 50%, and water content is 10%, also contains monoethanolamine,
Diethanol amine, triethanolamine and heavy constituent.
Aminoacid stripping tower theoretical cam curve is 30, and operating pressure is 1.85MPaG, and operation temperature is 48 DEG C.
Ammonia flash tank operating pressure is 0.65MPaG, and operation temperature is 170 DEG C.
Dehydrating tower operating pressure is 0.15MPaG, and operation temperature is 75 DEG C.
Mixed ethanol amine product 12, in terms of mass fraction, ammonia≤10ppm, water≤50ppm, monoethanolamine=55%, two
Monoethanolamine=35%, triethanolamine=10%.
In liquid ammonia recovery 5 water content be 25ppm, ammonia recovery >=99.9%.
In the present embodiment, 180 DEG C of the equal ＜ of aminoacid stripping tower bottom temperature, flash tank operation temperature and dehydrating tower bottom temperature.
【Comparative example 1】
Embodiment is identical with embodiment 1～3, and except for the difference that on aminoacid stripping tower top, gaseous phase outlet is not provided with high efficient gas and liquid separator,
The life-span of catalyst shortens at least 1/3rd than embodiment 1～3.
【Comparative example 2】
Coproduction mode is not adopted to liquid ammonia process for caustic soda purification and Ammonia Process technique in comparative example 2, a set of ammonia recovery unit, liquefied ammonia is respectively adopted
Method technique needs low-grade cryogen such as propylene, and freon is as liquefied ammonia cooling medium or needs to increase compressor, needs to increase
Plus an aminoacid stripping tower, a flash tank, increase equipment investment expense.
Claims (9)
1. in a kind of monoethanolamine joint production process ammonia recovery method, it is characterised in that the method is followed the steps below：
(1) aminoacid stripping tower will be delivered to after liquid ammonia process for caustic soda purification and the mixing of Ammonia Process product, gas phase is reclaimed after condensation and is recycled to
Reactor；
(2) aminoacid stripping tower kettle liquid delivers to ammonia flash tank, and Ammonia Process reaction member work is delivered to after ammonia flash drum overhead vapor condensation
For reaction raw materials, ammonia flash tank bottom liquid phase delivers to dehydrating tower dehydration；
(3) dehydrating tower kettle liquid delivers to ethanolamine product refined unit, and it is anti-that top liquid of the dehydration tower top containing a small amount of ammonia delivers to Ammonia Process
Unit is answered as catalyst.
2. according to claim 1 in monoethanolamine joint production process ammonia recovery method, it is characterised in that liquid ammonia process for caustic soda purification reaction produce
In terms of mass fraction, ammonia content is 60～85% to thing, also contains monoethanolamine, diethanol amine, triethanolamine and heavy constituent.
3. according to claim 1 in monoethanolamine joint production process ammonia recovery method, it is characterised in that Ammonia Process product
Ammonia content is counted as 50～75% with mass fraction, water content is 1～10%, also contains monoethanolamine, diethanol amine, triethanolamine
And heavy constituent.
4. according to claim 1 in monoethanolamine joint production process ammonia recovery method, it is characterised in that aminoacid stripping tower top sets
It is equipped with wire packing.
5. according to claim 1 in monoethanolamine joint production process ammonia recovery method, it is characterised in that in aminoacid stripping tower top gas
Mutually outlet arranges high efficient gas and liquid separator.
6. in the monoethanolamine joint production process according to claim 1 or 5 ammonia recovery method, it is characterised in that aminoacid stripping tower
Top gas Vapor Entrainment liquid water content after high efficient gas and liquid separator process is less than 100ppm.
7. according to claim 1 in monoethanolamine joint production process ammonia recovery method, it is characterised in that aminoacid stripping tower is theoretical
The number of plates is 10～30, and tower top operating pressure is 1.0～3.0MPaG, and tower top operation temperature is 30～80 DEG C.
8. according to claim 1 in monoethanolamine joint production process ammonia recovery method, it is characterised in that ammonia flash tank operate
Pressure is 0.3～1.0MPaG, and operation temperature is 130～170 DEG C.
9. according to claim 1 in monoethanolamine joint production process ammonia recovery method, it is characterised in that dehydration column overhead grasp
It is -0.1～0.3MPaG to make pressure, and tower top operation temperature is 60～120 DEG C.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6429844A (en) * | 1987-07-24 | 1989-01-31 | Fuji Photo Film Co Ltd | Method for processing silver halide color photographic sensitive material |
| CN101033194A (en) * | 2003-02-03 | 2007-09-12 | 株式会社日本触媒 | Process for producing high purity 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 |
| CN101560159A (en) * | 2009-05-12 | 2009-10-21 | 嘉兴金燕化工有限公司 | Method for reclaiming ammonia in production of cholamine |
| 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 |
| 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 |
| CN103951565A (en) * | 2014-06-03 | 2014-07-30 | 宁夏大学 | Synthesis method of novel trinuclear quaternary ammonium salt template agent as well as preparation method and application of molecular sieve solid acid |
-
2015
- 2015-10-22 CN CN201510689497.7A patent/CN106608831B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6429844A (en) * | 1987-07-24 | 1989-01-31 | Fuji Photo Film Co Ltd | Method for processing silver halide color photographic sensitive material |
| CN101033194A (en) * | 2003-02-03 | 2007-09-12 | 株式会社日本触媒 | Process for producing high purity 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 |
| CN101560159A (en) * | 2009-05-12 | 2009-10-21 | 嘉兴金燕化工有限公司 | Method for reclaiming ammonia in production of cholamine |
| 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 |
| 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 |
| CN103951565A (en) * | 2014-06-03 | 2014-07-30 | 宁夏大学 | Synthesis method of novel trinuclear quaternary ammonium salt template agent as well as preparation method and application of molecular sieve solid acid |
Non-Patent Citations (1)
| Title |
|---|
| 罗铭芳: "乙醇胺装置流程模拟与开发研究", 《天津大学硕士学位论文》 * |
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