CN114768276B - Dimethylamine purification system and method - Google Patents
Dimethylamine purification system and method Download PDFInfo
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- CN114768276B CN114768276B CN202210559803.5A CN202210559803A CN114768276B CN 114768276 B CN114768276 B CN 114768276B CN 202210559803 A CN202210559803 A CN 202210559803A CN 114768276 B CN114768276 B CN 114768276B
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- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 title claims abstract description 196
- 238000000746 purification Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000000926 separation method Methods 0.000 claims abstract description 103
- 239000007788 liquid Substances 0.000 claims abstract description 80
- 238000001179 sorption measurement Methods 0.000 claims abstract description 50
- 239000002994 raw material Substances 0.000 claims abstract description 43
- 238000002309 gasification Methods 0.000 claims abstract description 37
- 230000005484 gravity Effects 0.000 claims abstract description 37
- 239000012535 impurity Substances 0.000 claims abstract description 37
- 238000003860 storage Methods 0.000 claims abstract description 31
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000001301 oxygen Substances 0.000 claims abstract description 11
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 11
- 239000007789 gas Substances 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 31
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 239000003463 adsorbent Substances 0.000 claims description 7
- 229910001385 heavy metal Inorganic materials 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 239000002826 coolant Substances 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 239000002808 molecular sieve Substances 0.000 claims description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 3
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 abstract description 16
- 238000009833 condensation Methods 0.000 abstract description 12
- 230000005494 condensation Effects 0.000 abstract description 12
- 239000012071 phase Substances 0.000 description 11
- 239000012530 fluid Substances 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- -1 moisture Chemical compound 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 230000008016 vaporization Effects 0.000 description 3
- 238000005345 coagulation Methods 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- RHUYHJGZWVXEHW-UHFFFAOYSA-N 1,1-Dimethyhydrazine Chemical compound CN(C)N RHUYHJGZWVXEHW-UHFFFAOYSA-N 0.000 description 1
- LNVWRBNPXCUYJI-UHFFFAOYSA-N 3,5-dimethyl-1h-pyrazol-4-amine Chemical compound CC1=NNC(C)=C1N LNVWRBNPXCUYJI-UHFFFAOYSA-N 0.000 description 1
- 241000251468 Actinopterygii Species 0.000 description 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
- 238000013040 rubber vulcanization Methods 0.000 description 1
- 235000015170 shellfish Nutrition 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/0082—Regulation; Control
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D45/00—Separating dispersed particles from gases or vapours by gravity, inertia, or centrifugal forces
- B01D45/02—Separating dispersed particles from gases or vapours by gravity, inertia, or centrifugal forces by utilising gravity
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0057—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
- B01D5/006—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes with evaporation or distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0057—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
- B01D5/0069—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes with degasification or deaeration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0078—Condensation of vapours; Recovering volatile solvents by condensation characterised by auxiliary systems or arrangements
- B01D5/009—Collecting, removing and/or treatment of the condensate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/84—Purification
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention provides a dimethylamine purification system and a dimethylamine purification method, wherein the system comprises a raw material storage device, a gasification device, an adsorption device, a specific gravity separation device, a condensation device, a gas-liquid separation device and a product storage device, wherein the system firstly heats and gasifies liquid dimethylamine raw materials containing impurities through the gasification device, and then removes the impurities such as ammonia, water, methylamine, nitrogen, oxygen and the like in the raw materials through the adsorption device, the specific gravity separation device, the condensation device and the gas-liquid separation device, thereby obtaining high-purity dimethylamine.
Description
Technical Field
The invention relates to the technical field of dimethylamine production, in particular to a dimethylamine purification system and a dimethylamine purification method.
Background
Dimethylamine is a common organic chemical product, is colorless gas at normal temperature, has fish and shellfish smell at low concentration and ammonia smell at high concentration, and is mainly used as a raw material of rubber vulcanization accelerator, leather dehairing agent, medicine, pesticide, textile industry solvent, fuel, wafer deposited film gas, propellant, organic intermediates such as dimethylhydrazine, N-dimethylformamide and the like.
The current purification method of dimethylamine is generally to use methanol and ammonia as production raw materials and synthesize the product by a gas phase method, and because of the characteristics of the traditional dimethylamine manufacturing process, the dimethylamine product also contains a certain amount of impurities such as ammonia, moisture, methylamine and the like, so that the purity of the dimethylamine product sold in the market at present is lower. Particularly, as a raw material of biological reagents, impurities contained in dimethylamine directly affect the detection result of the reagents, and thus development of a system and a method for improving the purity of dimethylamine products have been desired.
Disclosure of Invention
The invention aims to solve the technical problem of how to remove impurities in dimethylamine and improve the purity of dimethylamine.
In order to solve the technical problems, the invention provides a dimethylamine purification system, which comprises
A raw material storage device for storing a liquid dimethylamine raw material containing impurities;
the gasification device is connected with the raw material storage device and is used for heating and gasifying the liquid dimethylamine raw material containing impurities;
the adsorption device is connected with the gasification device and is used for adsorbing part of impurities in the gas-phase dimethylamine conveyed by the gasification device;
the specific gravity separation device is connected with the adsorption device and is used for removing part of impurities in the gas-phase dimethylamine conveyed by the adsorption device;
a condensing device connected with the specific gravity separation device for condensing the gas-phase dimethylamine conveyed by the specific gravity separation device into liquid and condensing the moisture in the dimethylamine to remove the moisture;
the gas-liquid separation device is connected with the condensing device and is used for removing gas-phase impurities in dimethylamine conveyed by the condensing device;
and the product storage device is connected with the gas-liquid separation device and is used for recycling and storing the high-purity dimethylamine.
The invention designs a dimethylamine purifying system, which comprises a gasification device for heating and gasifying liquid dimethylamine raw materials containing impurities, and an adsorption device, a specific gravity separation device, a condensing device and a gas-liquid separation device for removing the impurities such as ammonia, water, methylamine, nitrogen, oxygen and the like contained in the raw materials, so that high-purity dimethylamine is obtained, and specific application requirements of dimethylamine are met.
Further, the gasification device comprises a heating shell and a gasification pipe arranged in the heating shell, a heating medium is arranged in the heating shell, and dimethylamine raw materials are conveyed through the gasification pipe. The gasification pipe has high heat transfer efficiency and can rapidly heat and gasify the liquid.
Further, the gasification device comprises a separation pipe, the outlet end of the gasification pipe is connected with the middle part of the separation pipe, the top of the separation pipe is provided with an air outlet, and the bottom of the separation pipe is connected with a liquid outlet. The separation tube can recycle part of unvaporized liquid raw material.
Further, the adsorption device comprises three layers of adsorption units, and each layer of adsorption unit is provided with one adsorbent of molecular sieve, activated carbon and potassium hydroxide. The adsorption device is internally provided with a plurality of adsorbents, has high adsorption efficiency, and can remove a plurality of impurities including ammonia and water.
Further, the specific gravity separation device comprises a separation tower and a reboiler arranged at the bottom of the separation tower, a tail gas outlet is arranged at the top of the separation tower, a gas outlet is arranged in the middle of the separation tower, a gas inlet is arranged at the lower part of the separation tower, an outlet of the adsorption device is connected with the gas inlet of the separation tower, and the gas outlet of the separation tower is connected with the inlet of the condensing device. The specific gravity separation device removes impurities such as heavy metals, nitrogen, oxygen, and the like by using the specific gravity difference.
Further, the condensing means comprises a condensing tube comprising a jacket for passing a cooling medium or a heating medium. The condensing device condenses the gas into liquid, and utilizes the difference between dimethylamine and the freezing point of water to condense and solidify the water.
Further, a plurality of baffles are arranged in the tube body of the condensation tube, and gaps are formed between the baffles and the inner wall of the tube body of the condensation tube to form a fluid channel. The baffle can prolong the passing time of fluid in the condensation tube, ensure the heat transfer efficiency and improve the water removal effect.
Further, the gas-liquid separation device comprises a vacuum pump, a vacuum chamber and a plurality of liquid conveying pipes, wherein the vacuum pump is communicated with the vacuum chamber, the liquid conveying pipes are arranged in the vacuum chamber, and the outer walls of the liquid conveying pipes are formed by breathable films. The gas-liquid separation device is matched with a vacuum pump by a ventilation membrane, so that gas-liquid separation can be efficiently realized, and impurities such as nitrogen, hydrogen, methylamine and the like are removed.
The invention also provides a dimethylamine purification method, which uses the dimethylamine purification system, and comprises the following steps:
s10, gasifying, namely heating and gasifying the liquid dimethylamine raw material containing impurities, and conveying the liquid dimethylamine raw material to a gasifying device for heating and gasifying;
s20, adsorbing, namely conveying the product obtained in the step S10 to an adsorption device, and adsorbing and removing ammonia and part of water;
s30, specific gravity separation, namely conveying the product obtained in the step S20 to a specific gravity separation device, and removing heavy metals, nitrogen and oxygen by utilizing specific gravity difference;
s40, condensing, namely conveying the product obtained in the step S30 to a condensing device for cooling, and condensing water to remove water;
s50, gas-liquid separation, namely conveying the product in the step S40 to a gas-liquid separation device for gas-liquid separation to remove gas-phase impurities;
s60, recycling the product, and conveying the product in the step S50 to a product storage device for storage.
Further, the heating gasification temperature in the step S10 is 30-40 ℃, the temperature in the adsorption device in the step S20 is 40-50 ℃, and the condensation temperature in the step S40 is-30 to-20 ℃.
The purification method of the invention does not need digestion and purification reagent, has low cost and high efficiency, is suitable for industrial production, and has good economic benefit when customers obtain dimethylamine with the purity of more than 99.99 percent.
Drawings
FIG. 1 is a process flow diagram of a dimethylamine purification system in an embodiment of the invention;
FIG. 2 is a schematic view of a gasification apparatus according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of an adsorption apparatus according to an embodiment of the present invention;
FIG. 4 is a schematic view showing the structure of a specific gravity separation device according to an embodiment of the present invention;
FIG. 5 is a schematic view of a condensing device according to an embodiment of the present invention;
FIG. 6 is a schematic diagram of a gas-liquid separation device according to an embodiment of the present invention;
FIG. 7 is a flow chart of a dimethylamine purification method in an embodiment of the present invention.
Reference numerals illustrate:
1-raw material storage device, 2-gasification device, 21-heating shell, 22-gasification pipe, 23-separation pipe, 3-adsorption device, 31-adsorption unit, 4-specific gravity separation device, 41-separation tower, 42-reboiler, 5-condensing device, 51-condensing pipe, 52-jacket, 53-baffle, 6-gas-liquid separation device, 61-vacuum pump, 62-vacuum chamber, 63-liquid delivery pipe, 7-product storage device.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that: like numerals and letters indicate like items in the following figures, and thus once an item is defined in one figure, no further definition or explanation thereof is necessary in the following figures.
The preferred embodiments of the present invention will be described below with reference to the accompanying drawings, it being understood that the preferred embodiments described herein are for illustration and explanation of the present invention only, and are not intended to limit the present invention.
Referring to fig. 1 to 6, an embodiment of the present invention discloses a dimethylamine purification system comprising a raw material storage device 1, a gasification device 2, an adsorption device 3, a specific gravity separation device 4, a coagulation device 5, a gas-liquid separation device 6, and a product storage device 7, which are connected in order by pipes. Wherein the raw material storage device 1 is used for storing liquid dimethylamine raw material containing impurities, and the impurities mainly comprise ammonia, moisture, methylamine, nitrogen, oxygen and heavy metals; the gasification device 2 is connected with the raw material storage device 1, the raw material storage device 1 conveys the liquid dimethylamine raw material containing impurities to the gasification device 2 by pressure, and the gasification device 2 is used for heating and gasifying the dimethylamine raw material; the adsorption device 3 is connected with the gasification device 2, the gasified dimethylamine raw material enters the adsorption device 3, and the adsorption device 3 is used for adsorbing part of impurities in the gas-phase dimethylamine; the specific gravity separation device 4 is connected with the adsorption device 3, the dimethylamine gas after adsorption enters the specific gravity separation device 4, separation is realized by utilizing the specific gravity difference of dimethylamine and impurities, and part of impurities are removed; the condensing device 5 is connected with the specific gravity separation device 4, and dimethylamine gas subjected to specific gravity separation enters the condensing device 5 to be condensed into liquid, and the moisture contained in the gas is condensed into ice so as to remove the moisture in the dimethylamine liquid; the gas-liquid separation device 6 is connected with the condensing device 5, and dimethylamine liquid enters the gas-liquid separation device 6 and then is subjected to gas-liquid separation to remove gas phase impurities, so that a dimethylamine product with high purity is obtained; the product storage device 7 is connected with the gas-liquid separation device 6, and dimethylamine products are conveyed into the product storage device 7 through a pipeline for recycling and storing.
Further, the raw material storage device 1 and the product storage device 7 are both high-pressure storage tanks, and cooling medium coils are arranged outside the raw material storage device 1 and the product storage device 7, so that dimethylamine in the raw material storage device 1 and the product storage device 7 is kept in a liquid state.
Referring to fig. 2, the vaporizing device 2 includes a heating housing 21, a vaporizing tube 22, and a separating tube 23, a heating medium is provided in the heating housing 21, and the vaporizing tube 22 and the separating tube 23 are provided in the heating housing 21. Dimethylamine raw material is conveyed through the gasification pipe 22, the gasification pipe 22 is spiral, the path through which the raw material flows can be prolonged, the contact area between the gasification pipe 22 and a heating medium is large, the heat transfer efficiency is improved, and the liquid raw material is vaporized and gasified in the gasification pipe 22 to become gas-phase dimethylamine. The outlet end of the gasification pipe 22 is connected with the middle part of the separation pipe 23, the top of the separation pipe 23 is provided with an air outlet, the bottom of the separation pipe 23 is provided with a liquid outlet, gas-liquid separation is carried out on the gas-phase dimethylamine in the separation pipe 23, liquid is discharged from the liquid outlet at the bottom and can be conveyed back to the raw material storage device 1, and the gas is output from the air outlet at the top and enters the adsorption device 3.
As shown in fig. 3, three layers of adsorption units 31 are arranged in the shell of the adsorption device 3, dimethylamine gas conveyed from the gasification device 2 sequentially passes through the three layers of adsorption units 31 from bottom to top, each layer of adsorption unit 31 is provided with an adsorbent, the adsorbents from top to bottom are molecular sieve, activated carbon and potassium hydroxide in sequence, a plurality of adsorbents are arranged in the adsorption device 3, the adsorption efficiency is high, and a plurality of impurities including ammonia and water can be removed in an adsorption mode. In other embodiments, the order of installation of the adsorbents may be replaced.
Further, electric tracing is arranged outside the shell of the adsorption device 3, so that the inside of the adsorption device 3 is kept at a higher temperature, and the reduction and liquefaction of dimethylamine gas temperature are avoided.
As shown in fig. 4, the specific gravity separation device 4 includes a separation column 41 and a reboiler 42 provided at the bottom of the separation column 41, the top of the separation column 41 is provided with a tail gas outlet, the middle is provided with a gas outlet, and the lower is provided with a gas inlet. The outlet of the adsorption device 3 is connected with the gas inlet of the separation tower 41, dimethylamine gas is conveyed from the adsorption device 3 to enter the separation tower 41 and then separated according to the specific gravity difference, liquid with high specific gravity and heavy metal fall into the reboiler 42, and the reboiler 42 heats and gasifies dimethylamine and enters the separation tower 41 again; the nitrogen and the oxygen with small specific gravity rise to the top of the separation tower 41 and are discharged from a top tail gas outlet; dimethylamine gas separated and removed of heavy metals and nitrogen and oxygen is discharged from the gas outlet of the separation tower 41 into the condensing device 5.
Referring to fig. 5, the condensing unit 5 includes a condensing tube 51, and the condensing tube 51 includes a jacket 52, and the jacket 52 is used to introduce a cooling medium or a heating medium. The dimethylamine gas fed from the specific gravity separation device 4 flows through the cooling pipe, and a cooling medium is introduced into the jacket 52 to condense the dimethylamine gas into a liquid, and at the same time, water is condensed into ice by utilizing the difference between the solidification points of dimethylamine and water, whereby the water is removed after the dimethylamine is discharged from the condensation pipe 51. When the condensing device 5 is overhauled, a heating medium is introduced into the jacket 52, and the ice remaining in the condensing tube 51 is liquefied into water and discharged. The pipe body of the condensation pipe 51 is internally provided with a plurality of baffles 53, gaps are formed between the baffles 53 and the inner wall of the pipe body of the condensation pipe 51 to form a fluid channel, the baffles 53 can limit the flowing direction of fluid in the condensation pipe 51, the passing time of the fluid in the condensation pipe 51 is prolonged, dimethylamine is guaranteed to be condensed into liquid, and the moisture removal effect is improved.
As shown in fig. 6, the gas-liquid separation device 6 includes a vacuum pump 61, a vacuum chamber 62, and a plurality of liquid delivery pipes 63, the vacuum pump 61 being in communication with the vacuum chamber 62 for evacuating the atmosphere within the vacuum chamber 62, the liquid delivery pipes 63 being provided within the vacuum chamber 62, the outer walls of the liquid delivery pipes 63 being constituted by gas-permeable films. The condensing device 5 outputs liquid-phase dimethylamine which enters the liquid conveying pipe 63 of the gas-liquid separation device 6, gas contained in the liquid-phase dimethylamine can pass through the breathable film, and liquid is remained in the liquid conveying pipe 63, so that gas-liquid separation is realized, and impurities such as nitrogen, hydrogen, methylamine and the like are efficiently removed.
The dimethylamine purification system has reasonable design and reliable operation, firstly, the gasification device 2 heats and gasifies the liquid dimethylamine raw material containing impurities, and then the adsorption device 3, the specific gravity separation device 4, the condensing device 5 and the gas-liquid separation device 6 remove the impurities such as ammonia, water, methylamine, nitrogen, oxygen and the like contained in the raw material, thereby obtaining the high-purity dimethylamine.
The embodiment of the invention also provides a dimethylamine purification method, which uses the dimethylamine purification system of the embodiment, and is shown in combination with fig. 7, the purification method comprises the following steps:
s10, gasifying, namely heating and conveying the liquid dimethylamine raw material containing impurities to a gasifying device 2 for heating and gasifying, wherein the heating and gasifying temperature is 30-40 ℃.
S20, adsorbing, namely conveying the product of the gasification step to an adsorption device 3, adsorbing and removing ammonia and part of water, and keeping the temperature in the adsorption device 3 at 40-50 ℃.
S30, specific gravity separation, namely conveying the product of the adsorption step to a specific gravity separation device 4, and removing heavy metals, nitrogen and oxygen by utilizing specific gravity difference.
S40, condensing, namely conveying the product of the specific gravity separation step to a condensing device 5 for cooling, condensing water to remove water, wherein the condensing temperature is-30 to-20 ℃.
S50, gas-liquid separation, namely conveying a product of the condensation step to a gas-liquid separation device 6 for gas-liquid separation, removing gas-phase impurities, wherein the vacuum degree of the gas-liquid separation device 6 is 2.5x10 -2 ～5×10 -2 torr。
S60, recovering the product, and conveying the product of the gas-liquid separation step to a product storage device 7 for storage.
The purification method does not need digestion and purification reagent, has low cost and high efficiency, is suitable for industrial production, and has good economic benefit when customers obtain dimethylamine with the purity of more than 99.99 percent.
Experimental example
The dimethylamine purification system of the above example was constructed and the dimethylamine purification method of the above example was used to analyze the components of dimethylamine raw material, adsorption device discharge, coagulation device discharge, and gas-liquid separation device discharge, and the results are shown in table 1 below.
TABLE 1 purification analysis results of dimethylamine
| Analysis item | Raw materials | Discharging of adsorption device | Discharging of condensing device | Discharging of gas-liquid separation device |
| Dimethylamine (%) | 99.0 | / | / | 99.99 |
| Nitrogen (ppmv) | 996 | 990 | 166 | 6 |
| Oxygen (ppmv) | 45 | 43 | 23 | 3 |
| Ammonia (ppmv) | 29 | 2 | 2 | 1 |
| Moisture (ppmv) | 87 | 18 | 3 | 3 |
| Methylamine (ppmv) | 42 | 42 | 40 | 4 |
According to experimental results, dimethylamine products with purity of more than 99.99% can be obtained by adopting the dimethylamine purification system.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solution of the present invention, and not limiting thereof; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (4)
1. A dimethylamine purification system, comprising
A raw material storage device (1) for storing a liquid dimethylamine raw material containing impurities;
the gasification device (2) is connected with the raw material storage device (1) and is used for heating and gasifying liquid dimethylamine raw materials containing impurities, the gasification device (2) comprises a heating shell (21) and a gasification pipe (22) arranged in the heating shell (21), a heating medium is arranged in the heating shell (21), the dimethylamine raw materials are conveyed through the gasification pipe (22), the gasification device (2) comprises a separation pipe (23), the outlet end of the gasification pipe (22) is connected with the middle part of the separation pipe (23), the top of the separation pipe (23) is provided with an air outlet, and the bottom of the separation pipe is provided with a liquid outlet;
the adsorption device (3) is connected with the gasification device (2) and is used for adsorbing part of impurities in the gas-phase dimethylamine conveyed by the gasification device (2);
the specific gravity separation device (4) is connected with the adsorption device (3) and is used for removing part of impurities in the gas-phase dimethylamine conveyed by the adsorption device (3), the specific gravity separation device (4) comprises a separation tower (41) and a reboiler (42) arranged at the bottom of the separation tower (41), a tail gas outlet is formed in the top of the separation tower (41), a gas outlet is formed in the middle of the separation tower (41), a gas inlet is formed in the lower portion of the separation tower (41), the outlet of the adsorption device (3) is connected with the gas inlet of the separation tower (41), and the gas outlet of the separation tower (41) is connected with the inlet of the condensing device (5);
a condensing device (5) connected with the specific gravity separation device (4) and used for condensing the gas-phase dimethylamine conveyed by the specific gravity separation device (4) into liquid and condensing the moisture in the dimethylamine to remove the moisture, wherein the condensing device (5) comprises a condensing pipe (51), the condensing pipe (51) comprises a jacket (52) used for introducing a cooling medium or a heating medium, a plurality of baffles (53) are arranged in the pipe body of the condensing pipe (51), and a gap is formed between the baffles (53) and the inner wall of the pipe body of the condensing pipe (51);
the gas-liquid separation device (6) is connected with the condensing device (5) and is used for removing gas-phase impurities in dimethylamine conveyed by the condensing device (5), the gas-liquid separation device (6) comprises a vacuum pump (61), a vacuum chamber (62) and a plurality of liquid conveying pipes (63), the vacuum pump (61) is communicated with the vacuum chamber (62), the liquid conveying pipes (63) are arranged in the vacuum chamber (62), and the outer wall of each liquid conveying pipe (63) is composed of a breathable film;
and the product storage device (7) is connected with the gas-liquid separation device (6) and is used for recycling and storing the high-purity dimethylamine.
2. Dimethylamine purification system according to claim 1, characterized in that the adsorption device (3) comprises three layers of adsorption units (31), each layer of adsorption units (31) being provided with one of the adsorbents molecular sieve, activated carbon and potassium hydroxide, respectively.
3. A dimethylamine purification method, characterized in that the dimethylamine purification system according to claim 1 or 2 is used, the purification method comprising the steps of:
s10, gasifying, namely heating and conveying the liquid dimethylamine raw material containing impurities to a gasifying device (2) for heating and gasifying;
s20, adsorbing, namely conveying the product obtained in the step S10 to an adsorption device (3) to adsorb and remove ammonia and part of water;
s30, specific gravity separation, namely conveying the product obtained in the step S20 to a specific gravity separation device (4), and removing heavy metals, nitrogen and oxygen by utilizing specific gravity difference;
s40, condensing, namely conveying the product obtained in the step S30 to a condensing device (5) for cooling, and condensing water to remove water;
s50, gas-liquid separation, namely conveying the product obtained in the step S40 to a gas-liquid separation device (6) for gas-liquid separation to remove gas-phase impurities;
s60, recycling the product, and conveying the product obtained in the step S50 to a product storage device (7) for storage.
4. The dimethylamine purification method according to claim 3, wherein the heating temperature in the step S10 is 30-40 ℃, the temperature in the adsorption device (3) in the step S20 is 40-50 ℃, and the condensing temperature in the step S40 is-30 to-20 ℃.
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| CN101062896A (en) * | 2006-04-25 | 2007-10-31 | 三菱丽阳株式会社 | Method for manufacturing trimethylamine |
| CN101554559A (en) * | 2008-04-10 | 2009-10-14 | 陈锚 | Adsorption method for purifying low-boiling-point organic compound |
| CN102942488A (en) * | 2012-11-02 | 2013-02-27 | 天津大学 | Regeneration technology of recovered methylamine solution and device thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101062896A (en) * | 2006-04-25 | 2007-10-31 | 三菱丽阳株式会社 | Method for manufacturing trimethylamine |
| CN101554559A (en) * | 2008-04-10 | 2009-10-14 | 陈锚 | Adsorption method for purifying low-boiling-point organic compound |
| CN102942488A (en) * | 2012-11-02 | 2013-02-27 | 天津大学 | Regeneration technology of recovered methylamine solution and device thereof |
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