CN101130500B - Method for separating and refining high purity trimethylamine - Google Patents
Method for separating and refining high purity trimethylamine Download PDFInfo
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- CN101130500B CN101130500B CN2007101315598A CN200710131559A CN101130500B CN 101130500 B CN101130500 B CN 101130500B CN 2007101315598 A CN2007101315598 A CN 2007101315598A CN 200710131559 A CN200710131559 A CN 200710131559A CN 101130500 B CN101130500 B CN 101130500B
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- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 title claims abstract description 202
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000007670 refining Methods 0.000 title claims abstract description 11
- 238000000605 extraction Methods 0.000 claims abstract description 90
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 60
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims abstract description 50
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000007788 liquid Substances 0.000 claims abstract description 28
- 230000018044 dehydration Effects 0.000 claims abstract description 24
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 24
- 241000282326 Felis catus Species 0.000 claims description 22
- 238000010992 reflux Methods 0.000 claims description 15
- 238000000926 separation method Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 abstract description 47
- 238000005516 engineering process Methods 0.000 abstract description 11
- 238000005265 energy consumption Methods 0.000 abstract description 9
- 238000004821 distillation Methods 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 3
- ACWNMZGQJXFKDP-UHFFFAOYSA-N methanamine;n-methylmethanamine Chemical compound NC.CNC ACWNMZGQJXFKDP-UHFFFAOYSA-N 0.000 abstract 1
- 239000000047 product Substances 0.000 description 19
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 12
- 239000000463 material Substances 0.000 description 9
- 230000007613 environmental effect Effects 0.000 description 7
- 229910021529 ammonia Inorganic materials 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000013505 freshwater Substances 0.000 description 5
- 239000007791 liquid phase Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 description 4
- 235000019743 Choline chloride Nutrition 0.000 description 4
- 229960003178 choline chloride Drugs 0.000 description 4
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- 230000006837 decompression Effects 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000003809 water extraction Methods 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- UHZZMRAGKVHANO-UHFFFAOYSA-M chlormequat chloride Chemical compound [Cl-].C[N+](C)(C)CCCl UHZZMRAGKVHANO-UHFFFAOYSA-M 0.000 description 1
- 230000009615 deamination Effects 0.000 description 1
- 238000006481 deamination reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000122 growth hormone Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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Abstract
The invention relates to a separating and refining method of high-purity trimethylamine through abstraction with extraction tower and distillation with trimethylamine fractionating tower and dewatering with dehydration tower, which comprises the following parts: recycling circulating water as extractant by extraction tower, producing trimethylamine with more than 97% mass concentration to enter the trimethylamine fractionating tower to distill, recycling after abstracting tower kettle liquid into the dehydration column to reclaiming methylamine dimethylamine and carbinol, abstracting after the returning of feed liquid on top of the tower of trimethylamine fractionating tower and the tower kettle feed liquid, producing the high-purity trimethylamine ( the mass concentration is more than 99. 9%, the methylamine and the dimethylamine are less than200ppm) through side line of the trimethylamine fractionating tower. The new technology displays merits of being with high rating product and less abstraction water (only needed 1/2-2/3 of common usage), which has low energy consumption (totally saved about 15-30 steamer) and flexible operation and high reliability and so on.
Description
Technical field
The present invention relates to the refining isolating method of high purity trimethylamine.
Background technology
Trimethylamine 99 is a kind of important chemical material, can be used for making choline chloride 60, ion exchange resin, rubber ingredients, also be used to make explosive, chemical fibre solvent, tensio-active agent, sensitive materials, photographic developer, plant growth hormones, choline dichloride or the like, wherein exit portion is main is to be used for producing choline chloride 60.Generate in the process of choline chloride 60 in reaction, contained one in the Trimethylamine 99, dimethylamine can generate carcinogenic substance in side reaction, therefore must control its content.European Union in 2007 have issued the new standard of choline chloride 60 product, clear and definite regulation in the standard: in the Trimethylamine 99 one, the content of dimethylamine must be less than 200ppm.This just has higher requirement to domestic Trimethylamine 99 manufacturing enterprise.The Trimethylamine 99 product of present domestic methylamine manufacturing enterprise generally exceed standard (Trimethylamine 99 content 98.5～99.8%, wherein water-content about 0.3～0.5%, one, dimethylamine 500～5000ppm do not wait).
The reaction and the separation process of tradition methylamine are as follows: react generation Monomethylamine, dimethylamine, Trimethylamine 99 and water, and unreacted ammonia and methyl alcohol completely with methyl alcohol and ammonia.In follow-up rectifying separation unit, behind the deamination, loop back reactor after the azeotrope condensation that unreacted ammonia of cat head and part Trimethylamine 99 form, tower still material enters extraction tower.Though the boiling point of Monomethylamine and dimethylamine is lower than the boiling point of Trimethylamine 99, and is soluble in water, and Trimethylamine 99 is water insoluble substantially.Therefore after adding extraction agent water, the extraction tower cat head obtains the Trimethylamine 99 product, and the tower still obtains containing one, the waste water of dimethylamine removes dehydration tower Separation and Recovery separation and purification again.
China Petrochemical Industry has proposed a kind of methylamine separating and refining patent (CN99119955.3), solves mainly that Monomethylamine in the conventional art, dimethylamine and Trimethylamine 99 product can not obtain in same flow process simultaneously or to produce waste water many, and the fresh water consumption is big, the problem that energy consumption is high.Mainly be with the part of dehydration tower still part logistics circulation, and will separate the scheme that tower bottoms is recycled into the dehydration tower middle part, so reduce the fresh water consumption, cut down the consumption of energy as extraction agent.Domestic enterprise has adopted this kind method more at present.But contain in the recirculated water not reclaim completely one, dimethylamine, in extraction tower, can increase separating difficulty like this, and reduce the quality of Trimethylamine 99.Patent CN 01113480.1 suggests plans similar therewith.
Mitsubishi Rayon Co., Ltd discloses a kind of process for purification (CN 02118417.8) of Trimethylamine 99, it is characterized in that this method comprises operation 1 and 2, operation 1 is that at least a and ammonia of methylamine mixture and methyl alcohol is carrying out carrying out the operation that the water extraction distillation obtains thick Trimethylamine 99 with tower 1 (Trimethylamine 99 knockout tower) methylamine reaction mixture that the gas phase contact reacts obtains separates unreacted ammonia in the ammonia knockout tower after in the presence of the zeolite catalyst; Operation 2 is that the tower 2 (Trimethylamine 99 treating tower) with necessary amount carries out water extraction distillation and obtains highly purified Trimethylamine 99.This is exactly in fact with the twin-stage extraction tower Trimethylamine 99 of purifying, though the Trimethylamine 99 quality product has improved, extraction water consumption and energy consumption also increase considerably.
Patent CN 200510023665.5 proposes a kind of production of aminomethane of improvement, to solve the post-processing technology problem of existing technology Trimethylamine 99 surplus and extraction water and generation water.It is primarily aimed at environmental protection, fails to solve the urgent at present problem that the Trimethylamine 99 quality product is faced that improves.
No matter be traditional technology or the patent that is proposed in recent years, all do not have to solve simultaneously high-quality Trimethylamine 99 production, minimizing discharge of wastewater or recovery, this three aspects difficult problem of energy-conserving and environment-protective.From above each class methods and technology as can be seen, extraction tower is as the major equipment that directly obtains Trimethylamine 99, and its performance quality directly has influence on quality product and energy consumption size.Obtain high quality Trimethylamine 99 product, very high for the requirement of extraction tower: at first separation theorem plate number wants sufficient; Secondly the temperature of extraction water will be strict controlled in about 90 ℃, and temperature is high can to reduce separation performance, and temperature is low can to increase energy consumption; The extraction water consumption is very big once more, produces a large amount of waste water, though can recycle and reuse, energy consumption also promotes simultaneously significantly; The extraction water entry position is difficult to hold.These cause Trimethylamine 99 manufacturing enterprise all to face the unfavorable circumstances of extraction tower separating effect.
Summary of the invention:
The invention provides a kind of separating high-purity Trimethylamine 99 green energy conservation novel process, the ultrapure Trimethylamine 99 product (＞99.9% that the extraction water consumption is little, energy consumption is low to satisfy, flexible operation, good reliability and product meet European Union's export standard, one, the needs of diformazan＜200ppm)
Technical solution of the present invention is as follows:
The method of a kind of separation, refining high purity trimethylamine, it mainly is made up of extraction tower extraction, the rectifying of Trimethylamine 99 rectifying tower and dehydration tower three steps of dewatering,
Step 2. with the Trimethylamine 99 of step 1 cat head extraction in the rectifying of Trimethylamine 99 rectifying tower, Trimethylamine 99 rectifying tower cat head feed liquid is returned extraction tower with Trimethylamine 99 rectifying Tata still feed liquid and is extracted again, (mass concentration＞99.9%, one, diformazan＜200ppm) are by the side line extraction of Trimethylamine 99 rectifying tower for the high purity trimethylamine product;
Step 3. enters the extraction Tata still feed liquid of step 1 from the dehydration tower middle part, the dehydration cat head steams one, dimethylamine and methyl alcohol enter follow-up one, dimethylamine is refining separates, a tower still water part is as the extraction water recycle of extraction tower, and small portion carries out environment protection treating.
The extraction tower tower top pressure is 0.8～1.1MPa in the aforesaid method, 75～90 ℃ of tower top temperatures, 145～180 ℃ of tower still temperature, 45～70 of number of theoretical plates, cat head Trimethylamine 99 partial reflux, reflux ratio 0.5～5; The extraction water consumption is 0.5～2 with the ratio of inlet amount, 80～95 ℃ of extraction water temperature, extraction water go into the tower position on tower top 3～9 theoretical stage places.
Trimethylamine 99 rectifying tower tower top pressure 0.9～1.5MPa in the aforesaid method, 65～85 ℃ of tower top temperatures, 145～180 ℃ of tower still temperature, 36～70 of number of theoretical plates, trim the top of column is than 5～80; Be fed into the tower position on tower top 13～39 theoretical stage places, (mass concentration＞99.9%, one, diformazan＜200ppm) by the extraction of Trimethylamine 99 rectifying tower side line, the extraction position is between the total number of theoretical plate 70～99% of knockout tower for the high purity trimethylamine product.
Dehydration column overhead pressure 0.4～0.8MPa in the aforesaid method, 35～50 ℃ of tower top temperatures, 145～190 ℃ of tower still temperature, 35～70 of number of theoretical plates, trim the top of column is than 2～5; Be fed into the tower position between the total number of theoretical plate 20～46% of knockout tower.
More than each tower inner transmission matter element can select high capacity tray, efficient structured packing or suitable random packing separately for use, also can be according to the characteristics of each each section of tower gas-liquid flow, rerum natura, adopt the optimum combination mode of above various mass transfer components, selected mass transfer component must satisfy the number of theoretical plate requirement of each tower.
The inventive method has the following advantages:
1, product hierarchy height: high purity trimethylamine product (mass concentration＞99.9%, one, diformazan＜200ppm), the total yield height that can be met European Union's standard;
2, control flexibly, good reliability: the extraction tower separation requirement is reduced greatly, and former processing requirement cat head Trimethylamine 99 content is 98.5～99.5%, and the present invention only requires more than 97% and gets final product; During actually operating, when the extraction tower cat head went out the higher Trimethylamine 99 of content, the reflux ratio of Trimethylamine 99 tower can reduce with energy efficient; Otherwise when extraction tower separates when undesirable, the Trimethylamine 99 tower still can be compensated by strengthening the method that refluxes, and guarantees quality product.
3, environmental protection: extraction water all adopts the circulation recycle-water, and consumption is 1/2～2/3 of former technology only, meets the development trend of present national environmental protection, recycling economy;
4, energy-saving and cost-reducing: though the Trimethylamine 99 rectifying tower has increased a part of energy consumption, owing to the extraction water consumption reduces greatly, and the heat enthalpy value height of water, therefore the total energy consumption of a whole set of technology reduces by 15～30% than former technology;
5, output of the present invention/output investment ratio height is specially adapted to that industrial scale is big, specification of quality is high, the Trimethylamine 99 manufacturing enterprise of environmental protection and energy saving.
Description of drawings
Fig. 1 is a Trimethylamine 99 separation and purification process flow diagram of the present invention, and wherein: T1 is an extraction tower; T2 is the Trimethylamine 99 rectifying tower; T3 is a dehydration tower; B is a storage tank;
Embodiment
The invention will be further elaborated below by embodiment
Embodiment 1: the separation of Trimethylamine 99, refining
Certain chemical enterprise methylamine separates feed liquid and contains Monomethylamine 1830kg/h, dimethylamine 2820kg/h, Trimethylamine 99 5080kg/h, methyl alcohol 100kg/h, water 2800kg/h, 125 ℃ of temperature, pressure 2.04MPa.Adopt that Trimethylamine 99 of the present invention separates, process for purification, technical process as shown in Figure 1, promptly the feed liquid 1 of coming from storage tank B contain one, two, Trimethylamine 99, the first alcohol and water adds from extraction tower T1 middle part with liquid phase, recirculated water 8 adds from extraction tower top as extraction water.Extraction tower T1 cat head obtains Trimethylamine 99 condensation rear section and refluxes, and material 3 enters Trimethylamine 99 tower T2 and makes with extra care, and tower still material 2 enters dehydration tower T3 and handles.Trimethylamine 99 tower T2 cat head obtains mixing the azeotropic liquid 4 of methylamine, turns back to storage tank B, and near tower still part side line extraction high purity trimethylamine product 5, tower still material 6 enters extraction tower raw material storage tank B.Dehydration tower T3 cat head material 7 mainly contains one, dimethylamine and methyl alcohol, enters that follow-up workshop section is refining to be separated, and tower still material 8 is as the extraction water recycle, and tower still material 9 is concentrated as environmental protection water and administered.
Enter extraction tower after the decompression of stock liquid 1 liquid phase.This column overhead working pressure 0.94MPa, 80.2 ℃ of top temperature, tower still working pressure 0.98MPa, 165.8 ℃ of still temperature.Extraction cycle water consumption 18000kg/h wherein contains Monomethylamine 0.1% (mass fraction), dimethylamine 0.2%, methyl alcohol 0.1%, and all the other are water.Operating reflux ratio is 4,70 of total stage number (number of actual plates, down together), and it is 98% that the extraction tower cat head goes out Trimethylamine 99 content, Monomethylamine 0.3%, dimethylamine content 0.5%, all the other are water and methyl alcohol.This feed liquid enters the Trimethylamine 99 rectifying tower separate after, cat head obtains containing the azeotropic liquid 200kg/h of Trimethylamine 99, Trimethylamine 99 content 70%, tower still feed liquid 140kg/h, wherein front three content 82.9%, returns the extraction tower raw material tank in the lump; Trimethylamine 99 column overhead pressure 1.0MPa, 71.2 ℃ of top temperature, 113.8 ℃ of tower still temperature, operating reflux ratio 20,70 of numbers of actual plates.Trimethylamine 99 is in the extraction of 64 column plate side line liquid phases, produced quantity 4800kg/h, and Trimethylamine 99 content 99.97%, dimethylamine 58ppm, Monomethylamine does not detect, water-content 189ppm, methyl alcohol 33ppm.Extraction Tata still feed liquid enters from the dehydration tower middle and upper part, dehydration column overhead working pressure 0.62MPa, 50.9 ℃ of top temperature, tower still pressure 0.67MPa, 163.3 ℃ of still temperature, operating reflux ratio 3.5, total 60 high capacity trays of stage number.The water inventory 20690kg/h that reclaims, wherein 18000kg/h recycles as extraction water, and all the other are entered environment protection treating by being with moisture in the beginning raw material, concentrating.
In this flow process, the wastage in bulk or weight heat is 7.2 * 10
6Kilocalorie/hour, the circulation cold consumes 6.2 * 10
6Kilocalorie/hour, do not disappear
Comparative example 1:
Certain chemical enterprise methylamine separates feed liquid and contains Monomethylamine 1830kg/h, dimethylamine 2820kg/h, Trimethylamine 99 5080kg/h, methyl alcohol 100kg/h, water 2800kg/h, 125 ℃ of temperature, and pressure 2.04MPa adopts old technology to separate Trimethylamine 99.Enter extraction tower after the decompression of feed liquid liquid phase.This column overhead working pressure 0.94MPa, 80.2 ℃ of top temperature, tower still working pressure 0.98MPa, 165.8 ℃ of still temperature.Extraction cycle water consumption 24000kg/h wherein contains Monomethylamine 0.1% (mass fraction), dimethylamine 0.2%, methyl alcohol 0.1%, and all the other are water.Operating reflux ratio is 5,80 of total stage number, and it is 99.5% that the extraction tower cat head goes out Trimethylamine 99 content, Monomethylamine 200ppm, dimethylamine content 0.1%, all the other are water and methyl alcohol.Extraction Tata still feed liquid enters from the dehydration tower middle and upper part, dehydration column overhead working pressure 0.62MPa, 50.9 ℃ of top temperature, tower still pressure 0.67MPa, 163.3 ℃ of still temperature, operating reflux ratio 3.5, total 60 high capacity trays of stage number.The water inventory 26710kg/h that reclaims, wherein 24000kg/h recycles as extraction water, and all the other are entered environment protection treating by being with moisture in the beginning raw material, concentrating.
In this flow process, the wastage in bulk or weight heat is 8.7 * 10
6Kilocalorie/hour, the circulation cold consumes 7.1 * 10
6Kilocalorie/hour, do not consume fresh water (85～90 ℃), extraction cycle water consumption 24000kg/h, environmental protection water quantity discharged 2710kg/h.The product hierarchy of Trimethylamine 99 does not reach the standard of outlet European Union.
Comparative example 2:
Certain chemical enterprise methylamine separates feed liquid and contains Monomethylamine 1830kg/h, dimethylamine 2820kg/h, Trimethylamine 99 5080kg/h, methyl alcohol 100kg/h, water 2800kg/h, 125 ℃ of temperature, and pressure 2.04MPa adopts old technology to separate Trimethylamine 99.Enter extraction tower after the decompression of feed liquid liquid phase.This column overhead working pressure 0.94MPa, 80.2 ℃ of top temperature, tower still working pressure 0.98MPa, 165.8 ℃ of still temperature.Extraction cycle water consumption 18000kg/h wherein contains Monomethylamine 0.1% (mass fraction), dimethylamine 0.2%, methyl alcohol 0.1%, and all the other are water.Operating reflux ratio is 4,70 of total stage number, and it is 98% that the extraction tower cat head goes out Trimethylamine 99 content, Monomethylamine 0.3%, dimethylamine content 0.5%, all the other are water and methyl alcohol.This feed liquid enters the secondary extraction tower separate after, cat head obtains 99.9% Trimethylamine 99 product, dimethylamine content 183ppm, water-content 560ppm, tower still feed liquid enters dehydration tower with the previous stage extraction tower and handles.Secondary extraction tower tower top pressure 0.9MPa, 79.8 ℃ of top temperature, 165.8 ℃ of tower still temperature, operating reflux ratio 5, extraction water adopts fresh water 11400kg/h, 70 of numbers of actual plates.Extraction Tata still feed liquid enters from the dehydration tower middle and upper part, dehydration column overhead working pressure 0.62MPa, 50.9 ℃ of top temperature, tower still pressure 0.67MPa, 163.3 ℃ of still temperature, operating reflux ratio 3.5, total 60 high capacity trays of stage number.The water inventory 32200kg/h that reclaims, wherein 18000kg/h recycles as extraction water, and all the other enter environment protection treating by being with moisture in the beginning raw material.
In this flow process, the wastage in bulk or weight heat is 10.3 * 10
6Kilocalorie/hour, the circulation cold consumes 9.1 * 10
6Kilocalorie/hour, consume fresh water (85～90 ℃) 11400kg/h, extraction cycle water consumption 18000kg/h, environmental protection water quantity discharged 14200kg/h.The product hierarchy of Trimethylamine 99 can reach the standard of outlet European Union.
Claims (3)
1. the method for a separation, refining high purity trimethylamine is characterized in that it mainly is made up of extraction tower (T1) extraction, (T2) rectifying of Trimethylamine 99 rectifying tower and dehydration tower (T3) dehydration three steps:
Step 1. contains one, two, Trimethylamine 99, and the feed liquid of first alcohol and water enters from extraction tower (T1) middle part, and extraction water adds from extraction tower (T1) top, and cat head extraction mass concentration enters Trimethylamine 99 rectifying tower (T2) rectifying greater than 97% Trimethylamine 99;
Step 2. with the Trimethylamine 99 of step 1 extraction tower (T1) cat head extraction in Trimethylamine 99 rectifying tower (T2) rectifying, Trimethylamine 99 rectifying tower (T2) cat head feed liquid is returned extraction tower (T1) with Trimethylamine 99 rectifying tower (T2) tower still feed liquid and is extracted again, the high purity trimethylamine product is by the side line extraction of Trimethylamine 99 rectifying tower (T2), described Trimethylamine 99 rectifying tower (T2) tower top pressure 0.9～1.5MPa, 65～85 ℃ of tower top temperatures, 145～180 ℃ of tower still temperature, 36～70 of number of theoretical plates, trim the top of column is than 5～80; Be fed into the tower position on tower top 13～39 theoretical stage places, the high purity trimethylamine product is by the extraction of Trimethylamine 99 rectifying tower (T2) side line, the extraction position is between the total number of theoretical plate 70～99% of knockout tower;
Step 3. enters extraction tower (T1) the tower still feed liquid of step 1 from dehydration tower (T3) middle part, dehydration tower (T3) cat head steams one, dimethylamine and methyl alcohol enter follow-up one, dimethylamine is refining separates, a tower still water part is as the extraction water recycle of extraction tower (T1), and small portion carries out environment protection treating.
2. according to the described method of claim 1, it is characterized in that: in the described step 1, extraction tower (T1) tower top pressure is 0.8～1.1MPa, 75～90 ℃ of tower top temperatures, 145～180 ℃ of tower still temperature, 45～70 of number of theoretical plates, cat head Trimethylamine 99 partial reflux, reflux ratio 0.5～5; The extraction water consumption is 0.5～2 with the ratio of inlet amount, 80～95 ℃ of extraction water temperature, extraction water go into the tower position on tower top 3～9 theoretical stage places.
3. according to the described method of claim 1, it is characterized in that: in the described step 3, dehydration tower (T3) tower top pressure 0.4～0.8MPa, 35～50 ℃ of tower top temperatures, 145～190 ℃ of tower still temperature, 35～70 of number of theoretical plates, trim the top of column is than 2～5; Be fed into the tower position between the total number of theoretical plate 20～46% of knockout tower.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2007101315598A CN101130500B (en) | 2007-09-14 | 2007-09-14 | Method for separating and refining high purity trimethylamine |
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| CN2007101315598A CN101130500B (en) | 2007-09-14 | 2007-09-14 | Method for separating and refining high purity trimethylamine |
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| CN115803313A (en) * | 2020-08-05 | 2023-03-14 | 中央硝子株式会社 | Method for purifying trialkylamine, method for producing trialkylamine, and composition |
| CN113842852B (en) * | 2021-10-29 | 2023-05-23 | 聊城鲁西甲胺化工有限公司 | Process and system for annual production of 20 ten thousand tons of methylamine |
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