CN102702258A - Water removal method for quaternary phosphonium salt aqueous solution - Google Patents
Water removal method for quaternary phosphonium salt aqueous solution Download PDFInfo
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- CN102702258A CN102702258A CN2012102054844A CN201210205484A CN102702258A CN 102702258 A CN102702258 A CN 102702258A CN 2012102054844 A CN2012102054844 A CN 2012102054844A CN 201210205484 A CN201210205484 A CN 201210205484A CN 102702258 A CN102702258 A CN 102702258A
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- organic solvent
- quaternary alkylphosphonium
- aqueous solution
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- alkylphosphonium salt
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Abstract
The invention provides a water removal method for a quaternary phosphonium salt aqueous solution, relates to the field of water removal for a quaternary phosphonium salt, and particularly provides a method of achieving a water removal purpose by transferring the phosphonium salt into an organic solvent first and then removing the organic solvent by aiming at the defects of a direct water distillation method of the quaternary phosphonium salt aqueous solution. Compared with the prior art, the water removal method has the advantages of saving equipment and energy and realizing complete water removal, and is therefore more suitable for industrial production.
Description
Technical field
The present invention relates to the quaternary alkylphosphonium salt field that dewaters, is to remove the method that obtains anhydrous quaternary alkylphosphonium salt about the water in the quaternary alkylphosphonium salt aqueous solution furtherly.
Background technology
Quaternary alkylphosphonium salt is a kind of sterilant, can be used as industrial water conditioning agent.It is again one type of important ionic liquid simultaneously, has the ion liquid general character, can be used as green solvent or catalyzer.It is that a kind of technology commonly used is gone up in industry with the alkyl chloride salify again that Grignard prepares trialkyl phosphine, and this technology Zhong quaternary alkylphosphonium salt is (CN200310100174) that the form with the aqueous solution exists at last.Often need use anhydrous quaternary alkylphosphonium salt in the practical application of Zai quaternary alkylphosphonium salt; How to obtain the most frequently used method of anhydrous quaternary alkylphosphonium salt except that anhydrating is exactly pressure reducing and steaming water; But this method needs to increase the input of vacuum apparatus on the one hand in industry; Compare distillation organic solvent zero(ppm) water on the other hand and need more energy consumption, make whole cost rise, the method for directly steaming water simultaneously also is difficult to thorough evaporating water and obtains anhydrous quaternary alkylphosphonium salt.
Summary of the invention
The object of the invention is exactly that deficiency to above quaternary alkylphosphonium salt water-eliminating method provides a kind of quaternary alkylphosphonium salt is transferred to the method for removing organic solvent in the organic solvent again and then reaching the purpose that dewaters earlier.
The process step of the water-eliminating method of the quaternary alkylphosphonium salt aqueous solution provided by the invention is that: adds a certain amount of inorganic salt in the quaternary alkylphosphonium salt aqueous solution, adds certain amount of organic solvent again, fully stirs; Leave standstill, layering; This moment, quaternary alkylphosphonium salt was just almost all transferred to organic layer, discarded water layer, added siccative in the organic layer; The mother liquor normal pressure boiled off organic solvent and promptly gets anhydrous quaternary alkylphosphonium salt with after-filtration in 2 hours.
Said quaternary alkylphosphonium salt can be following structure:
Wherein R can be C1～C4 alkyl, R
1Can be C1～C16 alkyl, X
-Can be Cl
-, Br
-, SO
4 2-, HSO
4 -, PF
6 -Deng negatively charged ion, and said quaternary alkylphosphonium salt is not limited to above several types.
Said inorganic salt can be sodium-chlor, Repone K, magnesium chloride, Sodium Bromide, sodium sulfate, SODIUMNITRATE etc., or the mixture of above two or more salt, and said inorganic salt are not limited to above several types.
Said organic solvent can be benzene,toluene,xylene, ETHYLE ACETATE, ether, methylene dichloride etc., or the mixture of above two or more organic solvent, and said organic solvent all is not limited to above several types.
Provided by the present invention quaternary alkylphosphonium salt is transferred to earlier to remove organic solvent in the organic solvent again and then reach remove the method anhydrate and compare with the method that directly boils off water, have saving equipment, save energy, the advantage completely that dewaters, thereby be more suitable in suitability for industrialized production.
Embodiment
Following embodiment can make those skilled in the art more fully understand the present invention, but does not limit the present invention in any way.
Embodiment 1
With adding 8 gram sodium-chlor in 200 grams, the 50% chlorination tributyl Shi Si Wan Ji Phosphonium aqueous solution, add 200mL ETHYLE ACETATE again, fully stir; Leave standstill, layering, discard water layer, add anhydrous magnesium sulfate drying in the organic layer; 2 hours after-filtration, mother liquor normal pressure boil off ETHYLE ACETATE and get the anhydrous quaternary alkylphosphonium salt of 98 grams.
Embodiment 2
With adding 7 gram Sodium Bromides in 200 grams, the 50% chlorination tributyl Shi Er Wan Ji Phosphonium aqueous solution, add 200mL toluene again, fully stir; Leave standstill, layering, discard water layer, add anhydrous magnesium sulfate drying in the organic layer; 2 hours after-filtration, mother liquor normal pressure boil off toluene and get the anhydrous quaternary alkylphosphonium salt of 95 grams.
Embodiment 3
With adding 6 gram sodium sulfate in 200 grams, the 50% chlorination tributyl Shi Si Wan Ji Phosphonium aqueous solution, add the 200mL methylene dichloride again, fully stir; Leave standstill, layering, discard water layer, add anhydrous magnesium sulfate drying in the organic layer; 2 hours after-filtration, mother liquor normal pressure steaming vibrating dichloromethane get the anhydrous quaternary alkylphosphonium salt of 99 grams.
Embodiment 4
With adding 10 gram SODIUMNITRATE in 200 grams, the 50% bromination tributyl Shi Er Wan Ji Phosphonium aqueous solution, add the 200mL ether again, fully stir; Leave standstill, layering, discard water layer, add anhydrous magnesium sulfate drying in the organic layer; 2 hours after-filtration, mother liquor normal pressure boil off ether and get the anhydrous quaternary alkylphosphonium salt of 98 grams.
Embodiment 5
With adding 8 gram sodium-chlor in 200 grams, the 50% chlorination tributyl Shi Si Wan Ji Phosphonium aqueous solution, add 200mL YLENE again, fully stir; Leave standstill, layering, discard water layer, add anhydrous magnesium sulfate drying in the organic layer; 2 hours after-filtration, mother liquor normal pressure boil off YLENE and get the anhydrous quaternary alkylphosphonium salt of 98 grams.
Claims (4)
1. the water-eliminating method of a quaternary alkylphosphonium salt aqueous solution is characterized in that adding certain amount of organic solvent again with adding a certain amount of inorganic salt in the quaternary alkylphosphonium salt aqueous solution; Fully stir; Leave standstill, layering, discard water layer, add siccative in the organic layer; The mother liquor normal pressure boiled off organic solvent and promptly gets anhydrous quaternary alkylphosphonium salt with after-filtration in 2 hours.
2. according to the method for claim 1, it is characterized in that said quaternary alkylphosphonium salt can be following structure:
Wherein R can be C1～C4 alkyl, R
1Can be C1～C16 alkyl, X
-Can be Cl
-, Br
-, SO4
2-, HSO
4 -, PF
6 -Deng negatively charged ion, and said quaternary alkylphosphonium salt is not limited to above several types.
3. according to the method for claim 1, it is characterized in that said inorganic salt can be sodium-chlor, Repone K, magnesium chloride, Sodium Bromide, sodium sulfate, SODIUMNITRATE etc., or the mixture of above two or more inorganic salt, and said salt is not limited to above several types.
4. according to the method for claim 1; It is characterized in that said organic solvent can be benzene,toluene,xylene, ETHYLE ACETATE, ether, methylene dichloride etc.; Or the mixture of above two or more organic solvent, and said organic solvent all is not limited to above several types.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102054844A CN102702258A (en) | 2012-06-21 | 2012-06-21 | Water removal method for quaternary phosphonium salt aqueous solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102054844A CN102702258A (en) | 2012-06-21 | 2012-06-21 | Water removal method for quaternary phosphonium salt aqueous solution |
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| CN102702258A true CN102702258A (en) | 2012-10-03 |
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| CN2012102054844A Pending CN102702258A (en) | 2012-06-21 | 2012-06-21 | Water removal method for quaternary phosphonium salt aqueous solution |
Country Status (1)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103805307A (en) * | 2012-11-09 | 2014-05-21 | 中化化工科学技术研究总院 | Preparation method for capacitor insulating oil |
| CN105017320A (en) * | 2015-07-02 | 2015-11-04 | 武汉理工大学 | Method for preparing difluoroethyl phosphonium salt/1,2-vinyl double phosphonium salt under solvent-free condition |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6169209B1 (en) * | 1997-11-21 | 2001-01-02 | Ube Industries, Ltd. | Preparation of organic phosphonium chloride |
| CN1607203A (en) * | 2003-10-15 | 2005-04-20 | 北京联众大地科技有限公司 | Method for synthesizing phosphonium salt by three organo-phosphines and alkyl halide hydrocarbon |
| CN101092399A (en) * | 2007-04-11 | 2007-12-26 | 东华大学 | Method for preparing ionic liquid with anion being as ion in halogen family |
| CN102268039A (en) * | 2010-06-01 | 2011-12-07 | 南开大学 | Preparation method of phosphonium salt |
-
2012
- 2012-06-21 CN CN2012102054844A patent/CN102702258A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6169209B1 (en) * | 1997-11-21 | 2001-01-02 | Ube Industries, Ltd. | Preparation of organic phosphonium chloride |
| CN1607203A (en) * | 2003-10-15 | 2005-04-20 | 北京联众大地科技有限公司 | Method for synthesizing phosphonium salt by three organo-phosphines and alkyl halide hydrocarbon |
| CN101092399A (en) * | 2007-04-11 | 2007-12-26 | 东华大学 | Method for preparing ionic liquid with anion being as ion in halogen family |
| CN102268039A (en) * | 2010-06-01 | 2011-12-07 | 南开大学 | Preparation method of phosphonium salt |
Non-Patent Citations (2)
| Title |
|---|
| 姚成等: "杀菌剂DYPC和TTPC的合成与应用研究", 《工业水处理》 * |
| 王瑛等: "烷基三丁基氯化鏻的合成与性能研究", 《应用化工》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103805307A (en) * | 2012-11-09 | 2014-05-21 | 中化化工科学技术研究总院 | Preparation method for capacitor insulating oil |
| CN103805307B (en) * | 2012-11-09 | 2015-07-15 | 中化化工科学技术研究总院 | Preparation method for capacitor insulating oil |
| CN105017320A (en) * | 2015-07-02 | 2015-11-04 | 武汉理工大学 | Method for preparing difluoroethyl phosphonium salt/1,2-vinyl double phosphonium salt under solvent-free condition |
| CN105017320B (en) * | 2015-07-02 | 2017-03-01 | 武汉理工大学 | The method preparing the double salt of two fluoro ethyl salt/1,2 vinyls under condition of no solvent |
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Application publication date: 20121003 |