CN1951935A - Reclamation method of sulfolane containing inorganic salt - Google Patents
Reclamation method of sulfolane containing inorganic salt Download PDFInfo
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- CN1951935A CN1951935A CN 200610134285 CN200610134285A CN1951935A CN 1951935 A CN1951935 A CN 1951935A CN 200610134285 CN200610134285 CN 200610134285 CN 200610134285 A CN200610134285 A CN 200610134285A CN 1951935 A CN1951935 A CN 1951935A
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- inorganic salt
- tetramethylene sulfone
- recovery method
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Abstract
The invention discloses a recycling disposing method of chemical solvent with inorganic cyclobutosulfone, which is characterized by the following: adding filter aid in the inorganic cyclobutosulfone to dissolve with filter under normal temperature; evolving large amount inorganic from cyclobutosulfone; filtering at -10-20 deg.c; decompressing filtrate; distilling the filter aid; removing inorganics from cyclobutosulfone; azeotroping water; recycling cyclobutosulfone.
Description
Technical field:
The present invention relates to the recovery method of a kind of recovery and treatment method of chemical solvents, particularly tetramethylene sulfone.
Background technology:
Be a kind of solid of colorless and odorless under the highly purified tetramethylene sulfone normal temperature, it is the non-proton multiple-effect polar solvent that a kind of dissolving power is strong, selectivity is good, to heat, acid, alkaline stability is high, is difficult for reacting with acid, alkali, diolefine, sulphur, alcohol etc., also is difficult for decomposition and polymerization below 240 degree.In traditional petroleum industry, tetramethylene sulfone is usually used in extracting aromatic hydrocarbons from the petroleum reforming fraction, also can be used as the scavenging agent of Sweet natural gas, synthetic gas and other sour gas, removes hydrogen sulfide and carbonic acid gas.It can be used as the solvent of macromolecular compound such as polyacrylonitrile, acrylonitrile copolymer, fluorinated ethylene propylene etc.Recently, owing to find that tetramethylene sulfone has good dissolved salt, tetramethylene sulfone also is used as some organic reaction solvent that generates a large amount of inorganic salt.But because the good dissolved salt of tetramethylene sulfone, make that the light constituent product is separated after, the tetramethylene sulfone that has dissolved salt is difficult for recycling, thereby causes production cost too high, unsuitable industrialization.
Existing tetramethylene sulfone recovery and treatment method, generally be at the design of the acidic substance that deterioration produced of tetramethylene sulfone in the aromatics extraction process, as publication number is CN1230545A, the Chinese patent application that open day is on October 6th, 1999 discloses a kind of method with macroreticular weakly base ion exchange resin treatment inferior sulfolane, this method is passed through an anion-exchange resin column with inferior sulfolane, acidic impurities wherein stays in resin layer, thereby improves the quality of tetramethylene sulfone.Remove a small amount of acidic impurities that produces in the aromatics extraction process but this method mainly is applicable to, and be not suitable for removing a large amount of inorganic salt.
Publication number is CN1634917, and the Chinese patent application that open day is on July 6th, 2005 discloses a kind of method with corrosive impurity in the solid alkali absorption tetramethylene sulfone.This method can be used for the absorption of corrosive impurity and small amount of solid inorganic salt, but is not suitable for removing a large amount of inorganic salt equally, should not realize industrialization.
For removing a large amount of inorganic salt that dissolved produces because of reaction in the tetramethylene sulfone, thereby reach the recycling of tetramethylene sulfone, not seeing has special report.
Summary of the invention:
The objective of the invention is to address the above problem, a kind of recovery method that contains the tetramethylene sulfone of inorganic salt is provided, be suitable for removing a large amount of inorganic salt, technology is simple to operation, reclaims the quality height, the efficient height.
The technical scheme that the present invention is adopted for achieving the above object is as follows: a kind of recovery method that contains the tetramethylene sulfone of inorganic salt, in the tetramethylene sulfone that contains inorganic salt, add flocculating aids, flocculating aids is can dissolve each other with tetramethylene sulfone under the normal temperature, but do not dissolve inorganic salt wherein, make a large amount of inorganic salt that are dissolved in the tetramethylene sulfone separate out, filter down temperature-10 ℃～20 ℃, filtrate decompression steams flocculating aids, thereby the inorganic salt in the removal tetramethylene sulfone, and remove the moisture that may contain by the flocculating aids azeotropic, obtain recycling tetramethylene sulfone thereby reclaim.
Various inorganic salt in that inorganic salt in the described tetramethylene sulfone that contains inorganic salt produce for reaction or the adding system, as the hydrochloride of various amine, vitriol etc.: common have dimethylamine hydrochloride, Diisopropylamine vitriol or an ammonia chloride etc.
The inorganic salt that contain mass percent 1-50% in the described tetramethylene sulfone that contains inorganic salt.
Described flocculating aids is toluene, chlorobenzene, normal hexane or normal heptane etc.
Described flocculating aids is 0.5-2 with the tetramethylene sulfone weight ratio that contains inorganic salt: 1.
Described flocculating aids is a toluene, and filtrate is at pressure-0.095Mpa, steams toluene under 40～90 ℃ of the system temperatures.
Preferred 0 ℃ of described filtration temperature.
Described flocculating aids that steams and the simple layering of water, simply be recycled and reused for the recovery of tetramethylene sulfone after dewatering.
The invention has the beneficial effects as follows: recovery method efficient height, easy to operate, the lower and easy industrialization of processing cost; Used flocculating aids, for general industry level solvent, as toluene, chlorobenzene, normal hexane, normal heptane or the like, the selection common feature of these flocculating aidss is: can dissolve each other with tetramethylene sulfone under this flocculating aids normal temperature, but the inorganic salt that do not dissolve wherein to be contained; Flocculating aids that steams in the system and the simple layering of water, simply can be recycled and reused for the recovery of tetramethylene sulfone after dewatering; The add-on of flocculating aids should be not very little, otherwise add-on very little, all inorganic salt can not be leached, and quality is reclaimed in influence; Method of the present invention not only can effectively be removed dissolved inorganic salt in the tetramethylene sulfone, and can effectively reduce the moisture in the tetramethylene sulfone, makes the content of tetramethylene sulfone and moisture situation return to the level of the tetramethylene sulfone of new purchase, thereby reaches the effect of recycling.
Embodiment:
Below by specific embodiment the present invention is further detailed, but the present invention is not limited to embodiment.
Embodiment one:
In 100 grams contain the tetramethylene sulfone of 50 gram dimethylamine hydrochlorides, add 60 gram toluene, be refrigerated to 0 ℃, filter, gained filtrate is at-0.095MPa, and 40 ℃～90 ℃ following underpressure distillation steam toluene, get content 98%, moisture＜0.1%, saltiness is less than the tetramethylene sulfone of 1 gram.
Embodiment two:
Add 120 gram toluene under the room temperature in 100 grams contain the tetramethylene sulfone of 40 gram dimethylamine hydrochlorides, filter, gained filtrate is at-0.095MPa, and 40 ℃～90 ℃ following underpressure distillation steam toluene, content 97%, moisture＜0.1%, saltiness is less than the tetramethylene sulfone of 1 gram.
Embodiment three:
In 100 grams contain the tetramethylene sulfone of 40 gram Diisopropylamine vitriol, add 60 gram normal hexanes under the room temperature, be refrigerated to 0 ℃, filter, gained filtrate decompression distillation ,-0.095MPa steams normal hexane under 40 ℃～90 ℃, get content 98%, moisture＜0.1%, saltiness is less than the tetramethylene sulfone of 1 gram.
Embodiment four:
In 10 kilograms of tetramethylene sulfone that contain 4 kilograms of dimethylamine hydrochlorides, add 10 kilograms of toluene under 10 ℃, centrifuging, the distillation of gained filtrate decompression ,-0.095MPa steams toluene under 40 ℃～90 ℃, content 97%, the tetramethylene sulfone of moisture＜0.1%.
Embodiment five:
Add 80 gram normal heptanes under the room temperature in 100 grams contain the tetramethylene sulfone of 30 gram dimethylamine hydrochlorides, filter, gained filtrate is at-0.095MPa, 40 ℃～90 ℃ following underpressure distillation steam normal heptane, get content 97%, moisture＜0.1%, saltiness is less than the tetramethylene sulfone of 1 gram.
Claims (9)
1, a kind of recovery method that contains the tetramethylene sulfone of inorganic salt, it is characterized in that: in the tetramethylene sulfone that contains inorganic salt, add flocculating aids, flocculating aids is can dissolve each other with tetramethylene sulfone under the normal temperature, but do not dissolve inorganic salt wherein, make a large amount of inorganic salt that are dissolved in the tetramethylene sulfone separate out, filter down temperature-10 ℃～20 ℃, filtrate decompression steams flocculating aids, thereby the inorganic salt in the removal tetramethylene sulfone, and remove the moisture that may contain by the flocculating aids azeotropic, obtain recycling tetramethylene sulfone thereby reclaim.
2, a kind of recovery method that contains the tetramethylene sulfone of inorganic salt according to claim 1 is characterized in that: contain the hydrochloride of the various amine in that inorganic salt in the tetramethylene sulfone of inorganic salt produce for reaction or the adding system or the vitriol of various amine.
3, a kind of recovery method that contains the tetramethylene sulfone of inorganic salt according to claim 2 is characterized in that: the inorganic salt that contain in the tetramethylene sulfone of inorganic salt are dimethylamine hydrochloride, Diisopropylamine vitriol or ammonia chloride.
4, a kind of recovery method that contains the tetramethylene sulfone of inorganic salt according to claim 1 is characterized in that: contain the inorganic salt that contain mass percent 1-50% in the tetramethylene sulfone of inorganic salt.
5, a kind of recovery method that contains the tetramethylene sulfone of inorganic salt according to claim 1, it is characterized in that: flocculating aids is toluene, chlorobenzene, normal hexane or normal heptane.
6, a kind of recovery method that contains the tetramethylene sulfone of inorganic salt according to claim 1 is characterized in that: flocculating aids is 0.5-2 with the tetramethylene sulfone weight ratio that contains inorganic salt: 1.
7, a kind of recovery method that contains the tetramethylene sulfone of inorganic salt according to claim 1, it is characterized in that: flocculating aids is a toluene, filtrate is at pressure-0.095Mpa, steams toluene under 40～90 ℃ of the system temperatures.
8, a kind of recovery method that contains the tetramethylene sulfone of inorganic salt according to claim 1, it is characterized in that: filtration temperature is 0 ℃.
9, according to the arbitrary described a kind of recovery method that contains the tetramethylene sulfone of inorganic salt of claim 1-8, it is characterized in that: the simple layering of flocculating aids that steams and water, simply be recycled and reused for the recovery of tetramethylene sulfone after dewatering.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101342853A CN100425606C (en) | 2006-11-13 | 2006-11-13 | Reclamation method of sulfolane containing inorganic salt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101342853A CN100425606C (en) | 2006-11-13 | 2006-11-13 | Reclamation method of sulfolane containing inorganic salt |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1951935A true CN1951935A (en) | 2007-04-25 |
| CN100425606C CN100425606C (en) | 2008-10-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2006101342853A Active CN100425606C (en) | 2006-11-13 | 2006-11-13 | Reclamation method of sulfolane containing inorganic salt |
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Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1076726C (en) * | 1998-03-26 | 2001-12-26 | 中国石油化工集团公司 | Regeneration process of inferior sulfolane |
| CN1125063C (en) * | 2000-09-25 | 2003-10-22 | 中国石油化工股份有限公司 | Refining process of coarse sulfolane product |
| CN1279037C (en) * | 2004-10-12 | 2006-10-11 | 南京工业大学 | Method for removing corrosive impurity from inferior sulfolane |
| CN1644581A (en) * | 2004-11-25 | 2005-07-27 | 中国石化集团天津石油化工公司 | Method for removing chlorine and corrosion negative ions from poor sulfolane |
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Assignee: Dalian Lianhua Medical Technology Co., Ltd. Assignor: Allychem Co., Ltd., Dalian, China Contract fulfillment period: 2009.12.22 to 2014.12.21 contract change Contract record no.: 2009210000300 Denomination of invention: Reclamation method of sulfolane containing inorganic salt Granted publication date: 20081015 License type: Exclusive license Record date: 20091223 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.12.22 TO 2014.12.21; CHANGE OF CONTRACT Name of requester: DALIAN ALLYCHEM MEDICAL TECHNOLOGY CO., LTD. Effective date: 20091223 |