CN1221775A - Dewatering tech. for microwater in organic solvent - Google Patents
Dewatering tech. for microwater in organic solvent Download PDFInfo
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- CN1221775A CN1221775A CN 97126199 CN97126199A CN1221775A CN 1221775 A CN1221775 A CN 1221775A CN 97126199 CN97126199 CN 97126199 CN 97126199 A CN97126199 A CN 97126199A CN 1221775 A CN1221775 A CN 1221775A
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Abstract
A process for removing micro water from organic solvent includes passing the organic solvent through the adsorbent layer in fixed-bed filled tower, discharging the collected liquid from tower when the adsorben is closed to saturation, vacuum desorption, scavenging with dried air until the concentration of combustible gas in output air of tower is under explosion limit, regenerating the adsorbent at ordinary pressure with dried hot air and cooling the temp in tower to ordinary temp with dried cold air. Its advantages are simple process, high water removing rate and long service life of molecular sieve.
Description
The present invention relates to the dewatering of solvent, the absorbing process that removes of minor amount of water in a kind of organic solvent is provided especially.
Document related to the present invention is not reported at present.The patent documentation overwhelming majority of publishing is the dewatering of specific a certain solution.Remove the absorbing process ＂ Chinese patent of water and methyl alcohol in the alcohol, publication number CN 1036944A as the ＂ of inventions such as Sun Weiruo.This invention is at water in the alcohol and methyl alcohol, its core is to use earlier the corn adsorption tower, the back removes moisture content and methyl alcohol in the alcohol with the zeolite molecular sieve adsorption tower, can make the alcohol of 90% (V) remove moisture content, methyl alcohol and some other impurity obtain the alcohol of 95.5% (V) or 99.6% (V), below its methanol content 200ppm.This method need consume a large amount of nitrogen or carbon monoxide gas when adsorbent reactivation, its dehydration degree of depth is dark inadequately, can not get the straight alcohol of water content ppm level, inconvenient operation, and because of the corn tower easily blocks, the facility investment amount is bigger.In addition, U.S.'s union carbide corporation John Draenor is thanked to Germania etc. and has been invented the drying means ＂ that ＂ adopts the Chabazite-type sorbent material, Chinese patent, CN 86208824A, this method is at the acidic fluid that contains moisture content and at least a acidic cpd, is applicable to the drying of gas.Sorbent material is the Chabazite-type zeolite.This method is better to following sour gas effect: halohydrocarbon, alcohol, ether, organic acid, ketone etc.Well-known in the prior art, when organic solvent adopted the sorbent material dehydration, solvent should fully contact with sorbent material.Its principle is that the water molecules diameter is less, molecular sieve is a porous mass, when molecular sieve bore diameter during greater than the water molecules diameter and less than the molecular dimension of organic solvent, the organic solvent molecule can be stayed beyond the adsorbent surface in theory, water molecules then is adsorbed to inner surface, sorbent material duct, can reach the purpose of dehydration like this.When sorbent material suction when saturated, reproducing adsorbent recycles.Such dewatering can not make water and sorbent material generation chemical reaction generate hydrate, belongs to the physical adsorption dewatering.Except that molecular sieve, silica gel, gac also can be used as sorbent material.Another kind of is the chemisorption dewatering, as being sorbent material with calcium sulfate, calcium chloride, peroxophosphoric acid magnesium etc., by water and their water generation reaction compounds.In general, the physical adsorption dehydration is made the sorbent material best results with molecular sieve.But the intensity of molecular sieve and age limit it in industrial application.
The object of the present invention is to provide the removing process of minor amount of water in a kind of organic solvent, it can be implemented in the minor amount of water that industrial use molecular sieve adsorption removes organic solvent, its technical process is simple, easy to operate, can make the dehydration of organic solvent degree of depth low, and molecular sieve can use repeatedly, has prolonged molecular sieve work-ing life.
The invention provides the removing process of minor amount of water in a kind of organic solvent, it is characterized in that operating process is as follows:
(1) water smoking
Make organic solvent with the void tower linear speed of 0.5～20cm/min by the sorbent material in the fixed bed packing tower, the aspect ratio 5～30 of tower, organic solvent fully contacts with sorbent material, 1～24 hour duration of contact, the initial water content of organic solvent should be less than 1%;
(2) purge stages of residual solvent in the tower
When sorbent material suction when saturated, storing liquid in tower is put only, vacuum desorption 1～5 hour purged 2～10 hours with dry air then, inflammable gas concentration is beyond limits of explosion in tower is worked off one's feeling vent one's spleen, air moisture content requirement dew point is lower than-20 ℃;
(3) the adsorbent reactivation stage
Be used for warm air sorbent material is regenerated under normal pressure, 200～500 ℃ of temperature, to 2～24 hours, air moisture content required dew point to be lower than-20 ℃, regeneration tolerance 0.8～3.0NM
3/ hrKg molecular sieve:
(4) sorbent material temperature-fall period
With cold dry air temperature in the tower is reduced to normal temperature, air moisture content requires dew point to be lower than-20 ℃.
Above-mentioned steps repeats.
In addition, organic solvent of the present invention comprises aromatic hydrocarbons, alkanes, alcohols, amides, alkyl halide class etc.Sorbent material comprises A type, X type, Y type, mordenite type, ZSM type, MCM series molecular sieve.
Above-mentioned dehydration tower aspect ratio is preferably 10～15, and organic solvent and sorbent material are preferably in 3～12 hours duration of contact.
Above-mentioned air regenesis tolerance is preferably in 1.8～3.0NM
3/ hrKg molecular sieve.
Require dew point to be preferably lower than-40 ℃ at described air moisture content.
The present invention adopts physical adsorption, the desorption method that periodical operation is carried out in a tower, and technical process is simple, and is easy to operate, the dehydration degree of depth is low, can make the dehydration of organic solvent degree of depth to 500ppm, the best can be to 5ppm, and minor amount of water removes in the suitable multiple organic solvent.
Below by embodiment in detail the present invention is described in detail.
Accompanying drawing 1 dewatering process equipment flowsheet.
Embodiment 1
Equipment used is seen accompanying drawing 1, mainly constitute by air compressor (1), air-heating furnace (2), head tank (3), dehydration tower (4), product jar (5) five parts, dehydration tower (4) bottom joins with head tank (3) by valve C (6), passes through valve B (9) emptying downwards simultaneously; Its top joins with product jar (5) by valve D (7), passes through valve A (8) simultaneously and links to each other with air compressor (1) with air-heating furnace (2).Air-heating furnace (2) is a jetting type heat pipe electrical heater, and 200～500 ℃ of outlet air temperatures are to satisfy the adsorbent reactivation processing condition.
The alcohol of 1% (V) water content is fed 4A molecular sieve (Dalian Chemistry and Physics Institute product) dehydration tower, the granularity of adsorbent of molecular sieve be in 15 to φ 30 orders; Dehydration tower internal diameter φ 110mm, high 3.0m, aspect ratio 27, be 5 hours the duration of contact of alcohol and sorbent material, treatment capacity is 100Kg/ days alcohol; Tower internal adsorption agent loading amount 20Kg, alcohol liquid air speed 0.2h
-1The water content of tower outlet alcohol is initially 105ppm, and water content rises to about 200ppm after 2 days, and sorbent material penetrates loading capacity and can reach 10% (wt) water.To surpass 200ppm right when the water content of alcohol, and molecular sieve needs regeneration.At first took out 2 hours with vacuum pump, used the air purge dehydration tower again 2 hours, use 200～500 ℃ then, dew point is-40 ℃, air regenesis 4 hours, and adsorbent of molecular sieve is reusable.Regeneration tolerance is 2.4NM
3/ hour Kg molecular sieve.
Equipment is identical with embodiment 1,3A molecular sieve (Dalian Chemistry and Physics Institute product) dehydration tower is equipped with in the industrial organic solvent 1.1-ethylene dichloride feeding of water content 0.3% (wt), the sorbent material granularity is φ 2～3mm: 300mm in the dehydration tower internal diameter, high 3.5m, treatment capacity is 2 tons/day, tower internal adsorption agent loading amount is 175Kg, and ethylene dichloride liquid air speed is 0.5h
-1Tower outlet ethylene dichloride water content is initially 40ppm, rises to 500ppm after 3 days, and sorbent material penetrates loading capacity 10% (wt) to water.When the ethylene dichloride water content surpasses 500ppm, stop going up dehydration operation, sorbent material needs regeneration.At first took out 3 hours with vacuum pump, used the air purge dehydration tower again 2 hours, then the air that feeds is slowly heated up, kept when being raised to 350 ℃ 4 hours, regeneration finishes.The regeneration air amount is 3.0M
3/ hour Kg molecular sieve.
Claims (7)
1. the removing process of minor amount of water in the organic solvent is characterized in that operating process is as follows: (1) water smoking
Make organic solvent with the void tower linear speed of 0.5～20cm/min by the sorbent material in the fixed bed packing tower, the aspect ratio 5～30 of tower, organic solvent fully contacts with sorbent material, contacts 1～24 hour, the initial water content of organic solvent should be less than 1%;
(2) purge stages of residual solvent in the tower
When sorbent material suction when saturated, storing liquid in tower is put only, vacuum desorption 1～5 hour was used for air purge 2～10 hours then, inflammable gas concentration is beyond limits of explosion in tower is worked off one's feeling vent one's spleen, air moisture content requirement dew point is lower than-20 ℃;
(3) the adsorbent reactivation stage
Be used for warm air sorbent material regenerated under normal pressure, 200～500 ℃ of temperature, the time with 2～24 hours, air moisture content requires dew point to be lower than-20 ℃, regeneration tolerance 0.8～3.0NM
3/ hrKg molecular sieve;
(4) sorbent material temperature-fall period
With cold dry air temperature in the tower is reduced to normal temperature, air moisture content requires-20 ℃ of the low sons of dew point.
Above-mentioned steps repeats.
2. according to the removing process of minor amount of water in the described organic solvent of claim 1, it is characterized in that: organic solvent comprises aromatic hydrocarbons, alkanes, alcohols, amides, alkyl halide class etc.; Sorbent material comprises A type, X type, Y type, mordenite type, ZSM type, MCM series molecular sieve.
3. according to the removing process of minor amount of water in claim 1, the 2 described organic solvents, it is characterized in that: tower aspect ratio 10～15, organic solvent and 3～12 hours duration of contact of sorbent material.
4. according to the removing process of minor amount of water in claim 1, the 2 described organic solvents, it is characterized in that: air regenesis tolerance 0.8～3.0NM
3/ hrKg molecular sieve.
5. according to the removing process of minor amount of water in claim 1, the 2 described organic solvents, it is characterized in that: air moisture content requires dew point to be lower than-40 ℃.
6. an equipment that is exclusively used in minor amount of water removing process in the described organic solvent of claim 1 mainly is made of air compressor (1), air-heating furnace (2), head tank (3), dehydration tower (4), product jar (5) five parts, it is characterized in that:
Dehydration tower (4) bottom joins with head tank (3) by valve C (6), passes through valve B (9) emptying downwards simultaneously; Its top joins with product jar (5) by valve D (7), passes through valve A (8) simultaneously and links to each other with air compressor (1) with air-heating furnace (2).
7. remove equipment according to minor amount of water in the described organic solvent of claim 6, it is characterized in that: air-heating furnace (2) is a jetting type heat pipe electrical heater, and 200～500 ℃ of outlet air temperatures are to satisfy the adsorbent reactivation processing condition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97126199 CN1117139C (en) | 1997-12-31 | 1997-12-31 | Dewatering tech. for microwater in organic solvent |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97126199 CN1117139C (en) | 1997-12-31 | 1997-12-31 | Dewatering tech. for microwater in organic solvent |
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| CN1221775A true CN1221775A (en) | 1999-07-07 |
| CN1117139C CN1117139C (en) | 2003-08-06 |
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| CN 97126199 Expired - Fee Related CN1117139C (en) | 1997-12-31 | 1997-12-31 | Dewatering tech. for microwater in organic solvent |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101707919B (en) * | 2007-06-15 | 2012-02-01 | 英国石油化学品有限公司 | A method for the online analysis of a vapour phase process stream |
| CN103170160A (en) * | 2013-04-09 | 2013-06-26 | 六九硅业有限公司 | Water removal method by utilizing mixed solvent of methylbenzene and 1,2-dimethoxyethane |
| CN103933934A (en) * | 2014-05-07 | 2014-07-23 | 南京工业大学 | Adsorbent for removing trace moisture in gas and preparation method thereof |
| CN104771933A (en) * | 2015-04-02 | 2015-07-15 | 周建伟 | Lubricating oil vacuum microwave water removing device |
| CN104877705A (en) * | 2015-06-01 | 2015-09-02 | 四川天采科技有限责任公司 | Method for normal-temperature adsorption dewatering of liquid phase of gasoline |
| CN105080181A (en) * | 2014-05-20 | 2015-11-25 | 中石化广州工程有限公司 | Molecular sieve dehydration method for C-4 fraction |
| CN105732378A (en) * | 2014-12-08 | 2016-07-06 | 厦门伟捷化工工程有限公司 | Organic water-containing mixture dehydration purification method |
| CN105087048B (en) * | 2014-05-20 | 2017-06-20 | 中石化广州工程有限公司 | A kind of method of heavy naphtha molecular sieve dehydration |
| CN112479797A (en) * | 2020-11-30 | 2021-03-12 | 安徽泽升科技有限公司 | Preparation method of ultra-dry organic solvent |
| CN112707838A (en) * | 2019-10-25 | 2021-04-27 | 中国石油化工股份有限公司 | Method for recovering N, N-dimethylacetamide |
-
1997
- 1997-12-31 CN CN 97126199 patent/CN1117139C/en not_active Expired - Fee Related
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101707919B (en) * | 2007-06-15 | 2012-02-01 | 英国石油化学品有限公司 | A method for the online analysis of a vapour phase process stream |
| CN103170160A (en) * | 2013-04-09 | 2013-06-26 | 六九硅业有限公司 | Water removal method by utilizing mixed solvent of methylbenzene and 1,2-dimethoxyethane |
| CN103933934A (en) * | 2014-05-07 | 2014-07-23 | 南京工业大学 | Adsorbent for removing trace moisture in gas and preparation method thereof |
| CN105087048B (en) * | 2014-05-20 | 2017-06-20 | 中石化广州工程有限公司 | A kind of method of heavy naphtha molecular sieve dehydration |
| CN105080181B (en) * | 2014-05-20 | 2017-08-22 | 中石化广州工程有限公司 | A kind of method of C-4-fraction molecular sieve dehydration |
| CN105080181A (en) * | 2014-05-20 | 2015-11-25 | 中石化广州工程有限公司 | Molecular sieve dehydration method for C-4 fraction |
| CN105732378B (en) * | 2014-12-08 | 2018-09-07 | 厦门伟捷化工工程有限公司 | A kind of method that organic-aqueous mixture carries out dehydration purification |
| CN105732378A (en) * | 2014-12-08 | 2016-07-06 | 厦门伟捷化工工程有限公司 | Organic water-containing mixture dehydration purification method |
| CN104771933A (en) * | 2015-04-02 | 2015-07-15 | 周建伟 | Lubricating oil vacuum microwave water removing device |
| CN104877705A (en) * | 2015-06-01 | 2015-09-02 | 四川天采科技有限责任公司 | Method for normal-temperature adsorption dewatering of liquid phase of gasoline |
| CN112707838A (en) * | 2019-10-25 | 2021-04-27 | 中国石油化工股份有限公司 | Method for recovering N, N-dimethylacetamide |
| CN112707838B (en) * | 2019-10-25 | 2022-12-09 | 中国石油化工股份有限公司 | Method for recovering N, N-dimethylacetamide |
| CN112479797A (en) * | 2020-11-30 | 2021-03-12 | 安徽泽升科技有限公司 | Preparation method of ultra-dry organic solvent |
| CN112479797B (en) * | 2020-11-30 | 2023-03-07 | 安徽泽升科技有限公司 | Preparation method of ultra-dry organic solvent |
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| Publication number | Publication date |
|---|---|
| CN1117139C (en) | 2003-08-06 |
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