CN101085738A - Method and device for preparing low water content trimethylamine - Google Patents
Method and device for preparing low water content trimethylamine Download PDFInfo
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- CN101085738A CN101085738A CN 200710069855 CN200710069855A CN101085738A CN 101085738 A CN101085738 A CN 101085738A CN 200710069855 CN200710069855 CN 200710069855 CN 200710069855 A CN200710069855 A CN 200710069855A CN 101085738 A CN101085738 A CN 101085738A
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- valve
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- trimethylamine
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- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 title claims abstract description 94
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000010521 absorption reaction Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 230000008929 regeneration Effects 0.000 claims abstract description 5
- 238000011069 regeneration method Methods 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 230000008676 import Effects 0.000 claims description 12
- 239000012530 fluid Substances 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000002594 sorbent Substances 0.000 claims description 7
- 238000001179 sorption measurement Methods 0.000 claims description 4
- 239000012776 electronic material Substances 0.000 abstract description 3
- 239000006096 absorbing agent Substances 0.000 abstract 3
- 238000005265 energy consumption Methods 0.000 abstract 1
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 230000007420 reactivation Effects 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
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 description 1
- 235000019743 Choline chloride Nutrition 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- UHZZMRAGKVHANO-UHFFFAOYSA-M chlormequat chloride Chemical compound [Cl-].C[N+](C)(C)CCCl UHZZMRAGKVHANO-UHFFFAOYSA-M 0.000 description 1
- 229960003178 choline chloride Drugs 0.000 description 1
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 description 1
- 235000019628 coolness Nutrition 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000000835 fiber 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
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000003956 methylamines Chemical group 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention discloses a method for preparing low water content trimethylamine and employed device. It employs two vertical tubular absorbers, and said tubu is filled with 3A molecular screen, which absorbs water in trimethylamine when trimethylamine passes through it. The working circulation comprises three working sections: absorption, absorber regeneration under vacuum condition through heating and absorber cooling, said two absorbes worke alternately. The time for each working circulation is certain, so the operation can be automatic. The invention reduces water content from 2% to 0.5%, the product can be used for electronic material. The process is convenient and energy consumption is low.
Description
Technical field
The present invention relates to a kind of method and device thereof of producing low water content trimethylamine.
Background technology
Trimethylamine 99 is used to make choline chloride 60, ion exchange resin, rubber ingredients, also is used to make explosive, chemical fibre solvent, tensio-active agent, sensitive materials, photographic developer, plant growth hormones, choline dichloride.In addition, also be used for the production of medicine, dyestuff.Moisture 2% mass percent of Trimethylamine 99 product on the market can not be suitable as electronic material (requiring water content to be lower than 0.5% mass percent).Owing to Monomethylamine, dimethylamine etc. are arranged in the Trimethylamine 99, these methylamines and water form complicated azeotropic system, so can not remove water in the Trimethylamine 99 by the conventional distillation method.
Summary of the invention
The object of the present invention is to provide a kind of method and device thereof of producing low water content trimethylamine.
The technical solution used in the present invention is:
1, a kind of method of producing the Trimethylamine 99 of low water content:
Carry out work with two vertical shell and tube adsorbers of placing, filling 3A molecular sieve in the tubulation pipe, in the time of in the aqueous Trimethylamine 99 process adsorber tubulation pipe, moisture content in the Trimethylamine 99 is removed by the 3A molecular sieve adsorption, the working cycle of each adsorber comprises absorption, sorbent material 3 workplace sections such as thermal regeneration, sorbent material cooling under vacuum environment, two adsorber alternations.
2, a kind of device of producing the Trimethylamine 99 of low water content:
The outlet of Trimethylamine 99 original fluid container is behind feedstock pump and connect first valve and the 12 valve, first valve is divided into two-way, one the tunnel connects the Trimethylamine 99 original fluid container through second valve, the lower cover of first adsorber is inserted on another road, the 12 valve is divided into two-way, one the tunnel connects the Trimethylamine 99 original fluid container through the 13 valve, and the lower cover of second adsorber is inserted on another road; Cold oil jar outlet is divided into two-way through cold oil pump, and one the tunnel connects the import of the first adsorber shell side lower end through the 4th valve, and another Lu Jingdi 14 valves connect the import of the second adsorber shell side lower end; Two ends after the 6th valve and the 16 valve serial connection connect the import of the first adsorber shell side lower end and the import of the second adsorber shell side lower end respectively; The outlet of oil heating kettle connects the 6th valve and the 16 valve serial connection point through hot oil pump; The outlet of the first adsorber shell side lower end is divided into two-way, and one the tunnel is hot oil outlet through the 5th valve, and another Lu Jingdi three valves are the cold oil outlet; The outlet of the second adsorber shell side lower end is divided into two-way, and one the tunnel is hot oil outlet through the 17 valve, and another Lu Jingdi 15 valves are the cold oil outlet; The outlet of the first adsorber upper cover is divided into two-way, one the tunnel connects Trimethylamine 99 finished product jar through the 11 valve, another Lu Jingdi ten valves connect vacuum system, compressed nitrogen inserts from the first adsorber upper cover through the 9th valve, the shell side upper end outlet of first adsorber is divided into two-way, one the tunnel is hot oil outlet through the 8th valve, and another Lu Jingdi seven valves are the cold oil outlet; The outlet of the second adsorber upper cover is divided into two-way, one the tunnel connects Trimethylamine 99 finished product jar through the 22 valve, another road the 21 valve connects vacuum system, compressed nitrogen inserts from the second adsorber upper cover through the 20 valve, the shell side upper end outlet of second adsorber is divided into two-way, one the tunnel is hot oil outlet through the 19 valve, and another Lu Jingdi eight valves are the cold oil outlet.
The beneficial effect that the present invention has is: the present invention carries out work with two vertical shell and tube adsorbers of placing, filling 3A molecular sieve in the tubulation pipe.In the time of in the aqueous Trimethylamine 99 process adsorber tubulation pipe, moisture content in the Trimethylamine 99 is removed by the 3A molecular sieve adsorption, the working cycle of each adsorber comprises absorption, sorbent material 3 workplace sections such as thermal regeneration, sorbent material cooling under vacuum environment, two adsorber alternations.Because each workplace section time is certain in the working cycle, therefore can utilize automatic control means to operate automatically, do not need manual operation in the working process.Present method is reduced to the water content in the Trimethylamine 99 below 0.5% mass percent by 2% mass percent by convenient, low power technology, and products obtained therefrom can be suitable for electronic material.
Description of drawings
Accompanying drawing is a structural principle synoptic diagram of the present invention.
Among the figure: 1～22, valve, 23, cold oil pump, 24, the cold oil jar, 25, hot oil pump, 26, oily heating kettle, 27, adsorber, 28, adsorber, 29, Trimethylamine 99 finished product jar 30, Trimethylamine 99 original fluid container, 31, feedstock pump.
Embodiment
As shown in drawings, the outlet of Trimethylamine 99 original fluid container 30 is behind feedstock pump 31 and connect first valve 1 and the 12 valve 12, first valve 1 is divided into two-way, one the tunnel connects Trimethylamine 99 original fluid container 30 through second valve 2, the lower cover of first adsorber 27 is inserted on another road, the 12 valve 12 is divided into two-way, and one the tunnel connects Trimethylamine 99 original fluid container 30 through the 13 valve 13, and the lower cover of second adsorber 28 is inserted on another road; Cold oil jar 24 outlet is divided into two-way through cold oil pump 23, and one the tunnel connects the import of first adsorber, 27 shell side lower ends through the 4th valve 4, and another Lu Jingdi 14 valves 14 connect the import of second adsorber, 28 shell side lower ends; Two ends after the 6th valve 6 and the 16 valve 16 serial connections connect the import of first adsorber, 27 shell side lower ends and the import of second adsorber, 28 shell side lower ends respectively; 26 outlets of oil heating kettle connect the 6th valve 6 and the 16 valve 16 serial connection points through hot oil pump 25; The outlet of first adsorber, 27 shell side lower ends is divided into two-way, and one the tunnel is hot oil outlet through the 5th valve 5, and another Lu Jingdi three valves 3 are the cold oil outlet; The outlet of second adsorber, 28 shell side lower ends is divided into two-way, and one the tunnel is hot oil outlet through the 17 valve 17, and another Lu Jingdi 15 valves 15 are the cold oil outlet; The outlet of first adsorber, 27 upper covers is divided into two-way, one the tunnel connects Trimethylamine 99 finished product jar 29 through the 11 valve 11, another Lu Jingdi ten valves 10 connect vacuum system, compressed nitrogen inserts from first adsorber, 27 upper covers through the 9th valve 9, the shell side upper end outlet of first adsorber 27 is divided into two-way, one the tunnel is hot oil outlet through the 8th valve 8, and another Lu Jingdi seven valves 7 are the cold oil outlet; The outlet of second adsorber, 28 upper covers is divided into two-way, one the tunnel connects Trimethylamine 99 finished product jar 29 through the 22 valve 22, another road the 21 valve 21 connects vacuum system, compressed nitrogen inserts from second adsorber, 28 upper covers through the 20 valve 20, the shell side upper end outlet of second adsorber 28 is divided into two-way, one the tunnel is hot oil outlet through the 19 valve 19, and another Lu Jingdi eight valves 8 are the cold oil outlet.
Described adsorber is the shell and tube adsorber, filling 3A molecular sieve in the tubulation pipe.
Principle of work of the present invention is as follows:
(1) at normal temperatures, feedstock pump 31 will be delivered in first adsorber 27 by first valve 1 from the Trimethylamine 99 of Trimethylamine 99 head tank 30, adsorbs to dewater, and enters Trimethylamine 99 finished product jar by the 11 valve 11 then;
(2) when first adsorber 27 outlet Trimethylamine 99 water content surpass set quota, close first valve 1 and the 11 valve 11, open the 12 valve 12 and the 22 valve 22 simultaneously, make the Trimethylamine 99 raw material adsorb and dewater by inhaling second adsorber 28;
(3) first adsorber 27 is carried out the adsorbent reactivation operation, the concrete operations step is:
(a) compressed nitrogen from compressor pushes back the Trimethylamine 99 in first adsorber 27 to Trimethylamine 99 head tank 30 by second valve 2 by the 9th valve 9;
(b) close second valve 2 and the 9th valve 9, open the tenth valve 10, with first adsorber 27 with go to vacuum system UNICOM;
(c) hot oil pump 25 is sent into 200～250 ℃ the deep fat from oily heating kettle 26 between the pipe of first adsorber 27 by the 6th valve 6, and the sorbent material in managing is carried out thermal regeneration, and deep fat flows out from the 8th valve 8 hot oil outlets and turns back to oily heating kettle 26;
(d) adsorbent reactivation finishes, and closes the 6th valve 6;
(e) deep fat flow back into oily heating kettle 26 by the 5th valve 5 hot oil outlets between first adsorber, 27 pipes, behind the deep fat, closes the 8th valve 8 and the 5th valve 5 in draining between first adsorber, 27 pipes;
(f) shut-off valve 10, and first adsorber 27 and vacuum system are disconnected;
(g) cold oil of cold oil jar 24 delivers into by the 4th valve 4 between first adsorber, 27 pipes through cold oil pump 23, discharges cold oil jar 24 from the cold oil mouth of the 7th valve 7;
(h) 27 coolings of first adsorber finish, and close the 4th valve 4, and the cold oil between first adsorber, 27 pipes is drained into cold oil jar 24 by the 3rd valve 3, close the 7th valve 7 and the 3rd valve 3 after draining, and so far first adsorber 27 can enter the next round adsorption operations.
(4) after 28 absorption of second adsorber finished, its regenerative process was with first adsorber 27.
Claims (3)
1, a kind of method of producing low water content trimethylamine is characterized in that: carry out work with two vertical shell and tube adsorbers of placing, filling 3A molecular sieve in the tubulation pipe.In the time of in the aqueous Trimethylamine 99 process adsorber tubulation pipe, moisture content in the Trimethylamine 99 is removed by the 3A molecular sieve adsorption, the working cycle of each adsorber comprises absorption, sorbent material 3 workplace sections such as thermal regeneration, sorbent material cooling under vacuum environment, two adsorber alternations.
2, a kind of device of producing low water content trimethylamine, it is characterized in that: the outlet of Trimethylamine 99 original fluid container (30) is behind feedstock pump (31) and connect first valve (1) and the 12 valve (12), first valve (1) is divided into two-way, one the tunnel connects Trimethylamine 99 original fluid container (30) through second valve (2), the lower cover of first adsorber (27) is inserted on another road, the 12 valve (12) is divided into two-way, and one the tunnel connects Trimethylamine 99 original fluid container (30) through the 13 valve (13), and the lower cover of second adsorber (28) is inserted on another road; Cold oil jar (24) outlet is divided into two-way through cold oil pump (23), and one the tunnel connects the import of first adsorber (27) shell side lower end through the 4th valve (4), and another Lu Jingdi 14 valves (14) connect the import of second adsorber (28) shell side lower end; Two ends after the 6th valve (6) and the 16 valve (16) serial connection connect the import of first adsorber (27) shell side lower end and the import of second adsorber (28) shell side lower end respectively; Oil heating kettle (26) outlet connects the 6th valve (6) and the 16 valve (16) serial connection point through hot oil pump (25); The outlet of first adsorber (27) shell side lower end is divided into two-way, and one the tunnel is hot oil outlet through the 5th valve (5), and another Lu Jingdi three valves (3) are the cold oil outlet; The outlet of second adsorber (28) shell side lower end is divided into two-way, and one the tunnel is hot oil outlet through the 17 valve (17), and another Lu Jingdi 15 valves (15) are the cold oil outlet; The outlet of first adsorber (27) upper cover is divided into two-way, one the tunnel connects Trimethylamine 99 finished product jar (29) through the 11 valve (11), another Lu Jingdi ten valves (10) connect vacuum system, compressed nitrogen inserts from first adsorber (27) upper cover through the 9th valve (9), the shell side upper end outlet of first adsorber (27) is divided into two-way, one the tunnel is hot oil outlet through the 8th valve (8), and another Lu Jingdi seven valves (7) are the cold oil outlet; The outlet of second adsorber (28) upper cover is divided into two-way, one the tunnel connects Trimethylamine 99 finished product jar (29) through the 22 valve (22), another road the 21 valve (21) connects vacuum system, compressed nitrogen inserts from second adsorber (28) upper cover through the 20 valve (20), the shell side upper end outlet of second adsorber (28) is divided into two-way, one the tunnel is hot oil outlet through the 19 valve (19), and another Lu Jingdi eight valves (8) are the cold oil outlet.
3, a kind of device of producing low water content trimethylamine according to claim 2, it is characterized in that: described adsorber is the shell and tube adsorber, filling 3A molecular sieve in the tubulation pipe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710069855 CN101085738A (en) | 2007-07-05 | 2007-07-05 | Method and device for preparing low water content trimethylamine |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710069855 CN101085738A (en) | 2007-07-05 | 2007-07-05 | Method and device for preparing low water content trimethylamine |
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| Publication Number | Publication Date |
|---|---|
| CN101085738A true CN101085738A (en) | 2007-12-12 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200710069855 Pending CN101085738A (en) | 2007-07-05 | 2007-07-05 | Method and device for preparing low water content trimethylamine |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111068361A (en) * | 2018-10-22 | 2020-04-28 | 中国石油化工股份有限公司 | Caprolactam ion exchange device and regeneration method thereof |
| CN111948086A (en) * | 2019-05-17 | 2020-11-17 | 张洁风 | Method for directly and rapidly determining water content of industrial anhydrous methylamine product with unknown absorbed dose |
| CN114874068A (en) * | 2022-05-05 | 2022-08-09 | 南京工业大学 | Method for continuously producing high-purity o-chlorotoluene by adsorption separation method |
-
2007
- 2007-07-05 CN CN 200710069855 patent/CN101085738A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111068361A (en) * | 2018-10-22 | 2020-04-28 | 中国石油化工股份有限公司 | Caprolactam ion exchange device and regeneration method thereof |
| CN111068361B (en) * | 2018-10-22 | 2022-02-11 | 中国石油化工股份有限公司 | Caprolactam ion exchange device and regeneration method thereof |
| CN111948086A (en) * | 2019-05-17 | 2020-11-17 | 张洁风 | Method for directly and rapidly determining water content of industrial anhydrous methylamine product with unknown absorbed dose |
| CN111948086B (en) * | 2019-05-17 | 2022-05-06 | 张洁风 | Method for directly and rapidly determining water content of industrial anhydrous methylamine product with unknown absorbed dose |
| CN114874068A (en) * | 2022-05-05 | 2022-08-09 | 南京工业大学 | Method for continuously producing high-purity o-chlorotoluene by adsorption separation method |
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