CN101985452A - Regeneration technology of tributyl phosphate - Google Patents
Regeneration technology of tributyl phosphate Download PDFInfo
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- CN101985452A CN101985452A CN2010105469686A CN201010546968A CN101985452A CN 101985452 A CN101985452 A CN 101985452A CN 2010105469686 A CN2010105469686 A CN 2010105469686A CN 201010546968 A CN201010546968 A CN 201010546968A CN 101985452 A CN101985452 A CN 101985452A
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- tributyl phosphate
- regeneration
- organic phase
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a regeneration technology of tributyl phosphate. Tributyl phosphate required to be regenerated is pumped in from the bottom of a regeneration tower, 1-3mol/L sodium hydroxide solution is pumped in from the bottom of the regeneration tower in phase ratio, under the action of vibration of a sieve plate in tower, two phases are fully contacted, chemical reaction is taken place, organic phase gradually floats up to the top of tower from the bottom of tower and overflows into a washing process. In a regeneration washing tower, desalted water is pumped in from the top of tower, under the vibration of sieve plate, impurities carried by regenerated extractant are fully washed, and the washed extractant overflows into an extractant storage tank for extraction from the top of the regeneration washing tower.
Description
Technical field
The present invention relates to a kind of reclaiming process of extraction agent, especially a kind of reclaiming process after extraction agent tributyl phosphate extracting power reduces in the wet phosphoric acid purifying extraction process.
Background technology
In industrial extraction was produced, most of organic kind of extractants can be along with the increase that recycles number of times, and its extracting power can weaken gradually, causes extraction agent can not obtain fine utilization.Tributyl phosphate is phosphorous neutral extraction agent, the Sauerstoffatom on the function key P=O key, and its outer existing lone-pair electron also have unoccupied orbital, and lone-pair electron can form coordinate bond with the particle that unoccupied orbital is arranged, and can be used for extracting metals etc.; Unoccupied orbital can be accepted lone-pair electron, forms coordination compound, can extract the solute with lone-pair electron.In wet phosphoric acid purifying process, because of containing more different impurities in the phosphoric acid by wet process, extraction agent is in the extraction Vanadium Pentoxide in FLAKES, also with phosphoric acid in impurity (as sulfate radical etc.) interacting generates the very strong title complex of stability, only can not effectively its back extraction be come out with de-salted water, along with continuous accumulation, the extracting power of extraction agent can descend gradually, and influencing Industrial cleaning facility can't normally carry out.In addition, in extraction process Yin Wendu, stirring intensity etc. control improper, will cause extracting and emulsifying, also can influence the extracting power of extraction agent.So will guarantee the extracting power of extraction agent, it is very important to regenerate.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method of cyclic regeneration of tributyl phosphate.
The object of the present invention is achieved like this, and a kind of reclaiming process of tributyl phosphate may further comprise the steps:
A, the tributyl phosphate that extracting power is reduced add regenerator column, add the sodium hydroxide solution of 1-3mol/L again in regenerator column, the adjustment pH value is 8-10, the sieve plate in the vibrations regenerator column, guarantee that tributyl phosphate fully contacts standing demix with sodium hydroxide solution; Upper organic phase enters the regeneration washing tower from the cat head overflow, and lower layer of water is separated and enters underflow liquid receiving tank;
B, add de-salted water in regeneration in the washing tower, the sieve plate in the vibrations regeneration washing tower makes de-salted water fully contact with organic phase, leaves standstill, and tells water, and water enters underflow liquid receiving tank, and so repetitive scrubbing organic phase to solution pH value is a neutrality;
It is standby that the extraction agent storage tank is gone in the overflow from the regeneration washing tower of organic phase after c, the washing.
In wet phosphoric acid purifying process, impurity in tributyl phosphate and the phosphoric acid (as sulfate radical etc.) interacting generates the very strong title complex of stability, with title complex reaction in sodium hydroxide solution and the extraction agent, make that impurities is come out by back extraction with the form of salt in the extraction agent, pass through the further washing of de-salted water again, realize extractant regeneration.
In technique scheme, the sodium hydroxide solution of described 1-3mol/L and the volume ratio of tributyl phosphate are 20:1 ~ 25:1.
In order to make organic phase mix mutually with inorganic, described sieve plate vibration frequency 60 ~ 100rpm.
In order to reach better regenerative mixed effect, the tributyl phosphate that described extracting power reduces is squeezed into regenerator column from the bottom of regenerator column with pump, and the sodium hydroxide solution of 1-3mol/L is added by the top of regenerator column.
In order to reach better washing effect, the organic phase among the described step a flows into the regeneration washing tower from the bottom of regeneration washing tower, and de-salted water adds from the top of regeneration washing tower.
In order to wash totallyer, in step b, the each de-salted water that adds and the volume ratio of organic phase are 1:4-1:6.
From the inorganic phase waste liquid that regenerator column, regeneration wash tower bottoms are discharged except that mainly containing the sodium salt, also may contain certain alkali lye and organic extractant, for avoiding the wasting of resources, isolate upper organic phase after it is left standstill for some time, the tributyl phosphate that reduces with the next batch extracting power carries out manipulation of regeneration again.
The present invention adopts the chemical method that adds alkali continuously, and impurity and alkali in the extraction agent react, make its can be continuously from extraction agent back extraction come out, by further washing, realize extractant regeneration with de-salted water.This technology regeneration effect is remarkable, and is easy to operate, stable, meets the demand for development of recycling economy.
Description of drawings
Fig. 1 is a schema of the present invention.
Embodiment
Embodiment 1
The first step, to squeeze into the tributyl phosphate 20L that extracting power reduces with pump from the bottom of regenerator column, top from regenerator column pumps into the sodium hydroxide solution of the 1-3mol/L of 400L, adjusting pH value is 8, sieve plate in the vibrations regenerator column, vibration frequency is 60 ~ 100rpm, guarantees that tributyl phosphate fully contacts standing demix with sodium hydroxide solution; Upper organic phase enters the regeneration washing tower from the cat head overflow, and lower layer of water is separated to enter and leaves standstill underflow liquid receiving tank.
Second step, from the top of regeneration washing tower, add de-salted water 5L, sieve plate in the vibrations regeneration washing tower, vibration frequency is 60 ~ 100rpm, make de-salted water fully contact with organic phase, leave standstill and tell water, water enters underflow liquid receiving tank, and so repetitive scrubbing organic phase to solution pH value is neutral;
In the 3rd step, the extraction agent storage tank is gone in the overflow from the regeneration washing tower of the organic phase after the washing, and to be equipped with groove standby.
The 4th step, from the inorganic phase waste liquid that regenerator column, regeneration wash tower bottoms are discharged except that mainly containing the sodium salt, also may contain certain alkali lye and organic extractant, for avoiding the wasting of resources, isolate organic phase after it is left standstill for some time, the tributyl phosphate that reduces with the next batch extracting power carries out manipulation of regeneration again.
Embodiment 2
The first step, to squeeze into the tributyl phosphate 25L that extracting power reduces with pump from the bottom of regenerator column, top from regenerator column pumps into the sodium hydroxide solution of the 1-3mol/L of 625L, adjusting pH value is 8, sieve plate in the vibrations regenerator column, vibration frequency is 60 ~ 100rpm, guarantees that tributyl phosphate fully contacts standing demix with sodium hydroxide solution; Upper organic phase enters the regeneration washing tower from the cat head overflow, and lower layer of water is separated and enters underflow liquid receiving tank.
Second step added de-salted water 4L from the top of regeneration washing tower, the sieve plate in the vibrations regeneration washing tower, and vibration frequency is 60 ~ 100rpm, makes de-salted water fully contact with organic phase, leaves standstill and tells water, so repetitive scrubbing organic phase to solution pH value is neutral;
In the 3rd step, the extraction agent storage tank is gone in the overflow from the regeneration washing tower of the organic phase after the washing, and to be equipped with groove standby, and the water in the regeneration washing tower enters underflow liquid receiving tank.
The 4th step, from the inorganic phase waste liquid that regenerator column, regeneration wash tower bottoms are discharged except that mainly containing the sodium salt, also may contain certain alkali lye and organic extractant, for avoiding the wasting of resources, isolate organic phase after it is left standstill for some time, the tributyl phosphate that reduces with the next batch extracting power carries out manipulation of regeneration again.
Claims (7)
1. the reclaiming process of a tributyl phosphate may further comprise the steps:
A, the tributyl phosphate that extracting power is reduced add regenerator column, add the sodium hydroxide solution of 1-3mol/L again in regenerator column, the adjustment pH value is 8-10, the sieve plate in the vibrations regenerator column, guarantee that tributyl phosphate fully contacts standing demix with sodium hydroxide solution; Upper organic phase enters the regeneration washing tower from the cat head overflow, and lower layer of water is separated and enters underflow liquid receiving tank;
B, add de-salted water in regeneration in the washing tower, the sieve plate in the vibrations regeneration washing tower makes de-salted water fully contact with organic phase, leaves standstill, and tells water, and water enters underflow liquid receiving tank, and so repetitive scrubbing organic phase to solution PH is a neutrality;
It is standby that the extraction agent storage tank is gone in the overflow from the regeneration washing tower of organic phase after c, the washing.
2. according to the reclaiming process of the described tributyl phosphate of claim 1, it is characterized in that: the sodium hydroxide solution of described 1-3mol/L and the volume ratio of tributyl phosphate are 20:1 ~ 25:1.
3. according to the reclaiming process of the described tributyl phosphate of claim 1, it is characterized in that: described sieve plate vibration frequency is 60 ~ 100rpm.
4. according to the reclaiming process of the described tributyl phosphate of claim 1, it is characterized in that: the tributyl phosphate that described extracting power reduces is squeezed into regenerator column from the bottom of regenerator column with pump, and the sodium hydroxide solution of 1-3mol/L is added by the top of regenerator column.
5. according to the reclaiming process of the described tributyl phosphate of claim 1, it is characterized in that: the organic phase among the described step a flows into the regeneration washing tower from the bottom of regeneration washing tower, and de-salted water adds from the top of regeneration washing tower.
6. according to the reclaiming process of the described tributyl phosphate of claim 1, it is characterized in that: in step b, the each de-salted water that adds and the volume ratio of organic phase are 1:4-1:6.
7. according to the reclaiming process of the described tributyl phosphate of claim 1, it is characterized in that: the aqueous phase in the inflow underflow liquid receiving tank also contains and does not separate clean organic phase, with the water standing demix in the underflow liquid receiving tank, tell the tributyl phosphate that reduces with the next batch extracting power after the upper organic phase and carry out manipulation of regeneration.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010105469686A CN101985452B (en) | 2010-11-17 | 2010-11-17 | Regeneration technology of tributyl phosphate |
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| CN2010105469686A CN101985452B (en) | 2010-11-17 | 2010-11-17 | Regeneration technology of tributyl phosphate |
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| CN101985452A true CN101985452A (en) | 2011-03-16 |
| CN101985452B CN101985452B (en) | 2012-07-04 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106883262A (en) * | 2017-03-28 | 2017-06-23 | 南昌航空大学 | A kind of renovation process of aging TBP organic phases |
| CN107793446A (en) * | 2016-08-31 | 2018-03-13 | 天津市科密欧化学试剂有限公司 | A kind of purification process of SILVER REAGENT tributyl phosphate |
| CN108085492A (en) * | 2017-12-18 | 2018-05-29 | 中核二七二铀业有限责任公司 | A kind of method of zirconium hafnium extract and separate system emulsion recycling TBP |
| CN110092707A (en) * | 2018-01-30 | 2019-08-06 | 中昊晨光化工研究院有限公司 | The method of hydrogen fluoride is removed in a kind of tetrafluoroethene production process |
| CN115105857A (en) * | 2021-03-23 | 2022-09-27 | 郑州天一萃取科技有限公司 | Purifying treatment agent and purifying method for tributyl phosphate waste organic phase |
-
2010
- 2010-11-17 CN CN2010105469686A patent/CN101985452B/en active Active
Non-Patent Citations (3)
| Title |
|---|
| 《CA 2002:729949》 20020926 Zilberman, B. Ya， et al. Regeneration of Spent TBP-Diluent Solvent by Steam Distillation 第274-281页 1-7 第44卷, 第3期 * |
| 《CA 2004:883048》 20041025 Zil"berman, B. Ya, et al. Regeneration of the TBP waste extractant - the diluent of rectification with water steam 第158-162页 1-7 第3卷, * |
| 《化学工程》 20021231 江燕斌等 炼油碱渣废水处理萃取剂反萃再生实验研究 第58-61页 1-7 第30卷, 第5期 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107793446A (en) * | 2016-08-31 | 2018-03-13 | 天津市科密欧化学试剂有限公司 | A kind of purification process of SILVER REAGENT tributyl phosphate |
| CN106883262A (en) * | 2017-03-28 | 2017-06-23 | 南昌航空大学 | A kind of renovation process of aging TBP organic phases |
| CN108085492A (en) * | 2017-12-18 | 2018-05-29 | 中核二七二铀业有限责任公司 | A kind of method of zirconium hafnium extract and separate system emulsion recycling TBP |
| CN110092707A (en) * | 2018-01-30 | 2019-08-06 | 中昊晨光化工研究院有限公司 | The method of hydrogen fluoride is removed in a kind of tetrafluoroethene production process |
| CN115105857A (en) * | 2021-03-23 | 2022-09-27 | 郑州天一萃取科技有限公司 | Purifying treatment agent and purifying method for tributyl phosphate waste organic phase |
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| CN101985452B (en) | 2012-07-04 |
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