CN110950905A - Method for recovering P507 from waste P507 extraction organic phase - Google Patents
Method for recovering P507 from waste P507 extraction organic phase Download PDFInfo
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- CN110950905A CN110950905A CN201911270145.2A CN201911270145A CN110950905A CN 110950905 A CN110950905 A CN 110950905A CN 201911270145 A CN201911270145 A CN 201911270145A CN 110950905 A CN110950905 A CN 110950905A
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- organic phase
- waste
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- extraction organic
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- 239000012074 organic phase Substances 0.000 title claims abstract description 58
- 238000000605 extraction Methods 0.000 title claims abstract description 46
- 239000002699 waste material Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 20
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002253 acid Substances 0.000 claims abstract description 9
- 238000001556 precipitation Methods 0.000 claims abstract description 9
- 230000008929 regeneration Effects 0.000 claims abstract description 9
- 238000011069 regeneration method Methods 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 239000012716 precipitator Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 34
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 239000002244 precipitate Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 12
- 239000008346 aqueous phase Substances 0.000 claims description 10
- 239000012071 phase Substances 0.000 claims description 10
- 238000005191 phase separation Methods 0.000 claims description 10
- 230000003068 static effect Effects 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000003350 kerosene Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 5
- 238000005554 pickling Methods 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims 1
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 239000004808 2-ethylhexylester Substances 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/38—Phosphonic acids [RP(=O)(OH)2]; Thiophosphonic acids ; [RP(=X1)(X2H)2(X1, X2 are each independently O, S or Se)]
- C07F9/40—Esters thereof
- C07F9/4003—Esters thereof the acid moiety containing a substituent or a structure which is considered as characteristic
- C07F9/4006—Esters of acyclic acids which can have further substituents on alkyl
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/38—Phosphonic acids [RP(=O)(OH)2]; Thiophosphonic acids ; [RP(=X1)(X2H)2(X1, X2 are each independently O, S or Se)]
- C07F9/40—Esters thereof
- C07F9/4071—Esters thereof the ester moiety containing a substituent or a structure which is considered as characteristic
- C07F9/4075—Esters with hydroxyalkyl compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention relates to a method for recovering P507 from a waste P507 extraction organic phase, which takes the waste P507 extraction organic phase as a raw material and strontium oxide as a precipitator and specifically comprises 3 steps of acid washing, precipitation and regeneration. The extractant P507 is recovered from the organic phase extracted by the waste P507, and the yield of the P507 reaches 90 to 92 percent. The method has the advantages of high P507 yield, short process flow, less reagent consumption, simple equipment, low energy consumption, low recovery cost and the like.
Description
Technical Field
The invention discloses a method for recovering P507 from a waste P507 extraction organic phase, and particularly relates to a method for recovering an extractant P507 from the waste P507 organic phase by taking strontium oxide as a precipitator. The specific technical field of the invention is the recovery of P507.
Background
P507 is one of acidic phosphorus extractants, and is known as 2-ethylhexyl phosphine mono 2-ethylhexyl ester. P507 is dissolved in kerosene or sulfonated kerosene to form an extraction organic phase, and additives such as TBP and the like are sometimes added into the extraction organic phase of P507 to improve the extraction performance.
P507 is commonly used for separating and purifying rare earth elements, and with the increasing number of extraction cycles and other reasons, more P507 extraction organic phase has to be discarded. At present, because no method for recovering the extractant P507 from the waste P507 extraction organic phase exists, the waste P507 extraction organic phase is usually directly discharged or used as fuel oil. The direct discharge of the waste P507 extraction organic phase not only wastes resources (the extractant P507 and the organic solvent), but also directly pollutes the environment and destroys the ecology. Because P507 contains phosphorus in the molecule, the waste P507 from combustion is used for extracting the organic phase, so that the extractant P507 is wasted, and acid rain pollution is generated. Therefore, it is one of the urgent matters to establish a method for economically, simply and rapidly recovering the extractant P507 from the organic phase extracted from the waste P507.
The invention aims at the problem that no method for recovering P507 from the waste P507 extraction organic phase exists at present, and establishes a method for economically, simply and quickly recovering an extracting agent P507 from the waste P507 extraction organic phase.
Disclosure of Invention
The invention provides a method for economically, simply and quickly recovering an extracting agent P507 from a waste P507 extraction organic phase, aiming at the situation that no method for recovering the P507 from the waste P507 extraction organic phase exists at present.
The invention relates to a method for recovering P507 from a waste P507 extraction organic phase, which takes the waste P507 extraction organic phase as a raw material and strontium oxide as a precipitator and consists of 3 steps of acid washing, precipitation and regeneration. The 3 steps are as follows:
step 1: acid pickling
Adding the waste P507 organic phase into a reaction kettle, adding hydrochloric acid with the concentration of 3.0-4.0 mol/L according to the molar ratio of P507 to HCl of 1: 1.2-1: 1.4 at room temperature, and stirring for 5-10 min at room temperature. After static phase separation, the upper layer is an acid-washing P507 extraction organic phase, and the lower layer is a water phase. The lower aqueous phase is discharged to obtain the acid-washed P507 extraction organic phase. The acid-washed P507 extracted organic phase remained in the reaction kettle for use in step 2.
Step 2: precipitation of
In the reaction pot containing the acid-washed P507 extraction organic phase in the step 1, strontium oxide is added according to the mol ratio of P507 to CaO of 1: 0.7-1: 0.9, and the mixture is stirred at room temperature for 10-20 min. Dry filtration to obtain a white precipitate for use in step 3.
And step 3: regeneration
And (3) transferring the white precipitate obtained in the step (2) to a reaction pot, adding hydrochloric acid with the concentration of 3.0-4.0 mol/L at room temperature according to the molar ratio of P507 to HCl of 1: 1.2-1: 1.4, and stirring until the white precipitate is completely dissolved. After static phase separation, the upper layer is an extractant P507, and the lower layer is a water phase. The lower aqueous phase was discharged to obtain extractant P507.
The waste P507 extraction organic phase is a kerosene solution or sulfonated kerosene solution of P507, wherein the concentration of the P507 is 1.0-1.5 mol/L.
The invention has the beneficial effects that: 1) the yield of P507 is high: the extractant P507 is recovered from the organic phase extracted by the waste P507, and the yield of the P507 reaches 90 to 92 percent. 2) The process flow is short: the whole process only comprises 3 steps of acid washing, precipitation and regeneration. 3) The reagent consumption is less: only a small amount of hydrochloric acid and strontium oxide is consumed. 4) The equipment is simple: only the common equipment such as a reaction pot, a filter and the like is needed. 5) The energy consumption is low: the extraction agent P507 is recovered from the waste P507 extraction organic phase at room temperature, and only energy for stirring and material transfer is consumed. 6) The recovery cost is low: the reagents, namely hydrochloric acid and strontium oxide, consumed by treating the waste P507 to extract the organic phase are low in price.
Detailed Description
A process of the present invention for recovering P507 from an organic phase of waste P507 extraction will now be further described with reference to specific examples.
Example 1
The waste P507 extraction organic phase is a kerosene solution of P507, wherein the concentration of P507 is 1.0 mol/L.
Step 1: acid pickling
Adding the waste P507 organic phase into a reaction kettle, adding 3.0mol/L hydrochloric acid according to the molar ratio of P507 to HCl of 1: 1.2 at room temperature, and stirring for 5min at room temperature. After static phase separation, the upper layer is an acid-washing P507 extraction organic phase, and the lower layer is a water phase. The lower aqueous phase is discharged to obtain the acid-washed P507 extraction organic phase. The acid-washed P507 extracted organic phase remained in the reaction kettle for use in step 2.
Step 2: precipitation of
In the reaction pot containing the acid-washed P507 extraction organic phase in the step 1, strontium oxide is added according to the mol ratio of P507 to CaO of 1: 0.9, and the mixture is stirred for 20min at room temperature. Dry filtration to obtain a white precipitate for use in step 3.
And step 3: regeneration
Transferring the white precipitate obtained in the step 2 to a reaction pot, adding hydrochloric acid with the concentration of 3.0mol/L at room temperature according to the molar ratio of P507 to HCl of 1: 1.2, and stirring until the white precipitate is completely dissolved. After static phase separation, the upper layer is an extractant P507, and the lower layer is a water phase. The lower aqueous phase was discharged to obtain extractant P507.
The yield of P507 was 90%.
Example 2
The waste P507 extraction organic phase is P507 sulfonated kerosene solution, wherein the concentration of P507 is 1.2 mol/L.
Step 1: acid pickling
Adding the waste P507 organic phase into a reaction kettle, adding 3.5mol/L hydrochloric acid according to the molar ratio of P507 to HCl of 1: 1.3 at room temperature, and stirring for 8min at room temperature. After static phase separation, the upper layer is an acid-washing P507 extraction organic phase, and the lower layer is a water phase. The lower aqueous phase is discharged to obtain the acid-washed P507 extraction organic phase. The acid-washed P507 extracted organic phase remained in the reaction kettle for use in step 2.
Step 2: precipitation of
In the reaction pot containing the acid-washed P507 extraction organic phase in the step 1, strontium oxide is added according to the mol ratio of P507 to CaO of 1: 0.8, and the mixture is stirred for 15min at room temperature. Dry filtration to obtain a white precipitate for use in step 3.
And step 3: regeneration
Transferring the white precipitate obtained in the step 2 to a reaction pot, adding hydrochloric acid with the concentration of 3.5mol/L at room temperature according to the molar ratio of P507 to HCl of 1: 1.3, and stirring until the white precipitate is completely dissolved. After static phase separation, the upper layer is an extractant P507, and the lower layer is a water phase. The lower aqueous phase was discharged to obtain extractant P507.
The yield of P507 was 91%.
Example 3
The waste P507 extraction organic phase is a kerosene solution of P507, wherein the concentration of P507 is 1.5 mol/L.
Step 1: acid pickling
Adding the waste P507 organic phase into a reaction kettle, adding hydrochloric acid with the concentration of 4.0mol/L according to the molar ratio of P507 to HCl of 1: 1.4 at room temperature, and stirring for 10min at room temperature. After static phase separation, the upper layer is an acid-washing P507 extraction organic phase, and the lower layer is a water phase. The lower aqueous phase is discharged to obtain the acid-washed P507 extraction organic phase. The acid-washed P507 extracted organic phase remained in the reaction kettle for use in step 2.
Step 2: precipitation of
In the reaction pot containing the acid-washed P507 extraction organic phase in the step 1, strontium oxide is added according to the molar ratio of P507 to CaO of 1: 0.7, and the mixture is stirred for 10min at room temperature. Dry filtration to obtain a white precipitate for use in step 3.
And step 3: regeneration
Transferring the white precipitate obtained in the step 2 to a reaction pot, adding hydrochloric acid with the concentration of 4.0mol/L at room temperature according to the molar ratio of P507 to HCl of 1: 1.4, and stirring until the white precipitate is completely dissolved. After static phase separation, the upper layer is an extractant P507, and the lower layer is a water phase. The lower aqueous phase was discharged to obtain extractant P507.
The yield of P507 was 92%.
Claims (2)
1. A method for recovering P507 from waste P507 extraction organic phase is characterized in that: the method takes a waste P507 extraction organic phase as a raw material and strontium oxide as a precipitator, and comprises 3 steps of acid washing, precipitation and regeneration;
the 3 steps are as follows:
step 1: acid pickling
Adding the waste P507 extraction organic phase into a reaction kettle, adding hydrochloric acid with the concentration of 3.0-4.0 mol/L according to the molar ratio of P507 to HCl of 1: 1.2-1: 1.4 at room temperature, and stirring for 5-10 min at room temperature; after static phase separation, the upper layer is an acid-washing P507 extraction organic phase, and the lower layer is a water phase; discharging the lower aqueous phase to obtain an acid-washed P507 extraction organic phase; the acid-washed P507 extracted organic phase is kept in a reaction kettle for the step 2;
step 2: precipitation of
In the reaction pot containing the acid-washed P507 extraction organic phase in the step 1, adding strontium oxide according to the molar ratio of P507 to CaO of 1: 0.7-1: 0.9, and stirring at room temperature for 10-20 min; dry filtering to obtain white precipitate for step 3;
and step 3: regeneration
Transferring the white precipitate obtained in the step 2 into a reaction pot, adding hydrochloric acid with the concentration of 3.0-4.0 mol/L into the reaction pot according to the molar ratio of P507 to HCl of 1: 1.2-1: 1.4 at room temperature, and stirring until the white precipitate is completely dissolved; after static phase separation, the upper layer is an extractant P507, and the lower layer is a water phase; the lower aqueous phase was discharged to obtain extractant P507.
2. A method of recovering P507 from an organic phase of waste P507 extraction as claimed in claim 1 wherein: the waste P507 extraction organic phase is a kerosene solution or sulfonated kerosene solution of P507, wherein the concentration of the P507 is 1.0-1.5 mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911270145.2A CN110950905A (en) | 2019-12-11 | 2019-12-11 | Method for recovering P507 from waste P507 extraction organic phase |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911270145.2A CN110950905A (en) | 2019-12-11 | 2019-12-11 | Method for recovering P507 from waste P507 extraction organic phase |
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| CN110950905A true CN110950905A (en) | 2020-04-03 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101160334A (en) * | 2005-06-22 | 2008-04-09 | 日本聚氨酯工业株式会社 | Catalyst for isocyanurate bond formation reaction and process for producing isocyanurate-bond-containing modified polyisocyanate mixture with the same |
| CN101948483A (en) * | 2010-08-20 | 2011-01-19 | 王德兴 | Method for preparing calcium soap by utilizing quick lime and method for processing produced emulsified compound |
| CN104131163A (en) * | 2014-08-05 | 2014-11-05 | 南昌航空大学 | Regeneration method of P507 organic-phase emulsified mixture for extracting and separating rare earth |
| CN105132683A (en) * | 2015-09-15 | 2015-12-09 | 南昌航空大学 | Regeneration method of aged P507 organic phase |
| CN107384217A (en) * | 2016-03-31 | 2017-11-24 | 荒川化学工业株式会社 | The manufacture method and rosin ester of rosin ester |
-
2019
- 2019-12-11 CN CN201911270145.2A patent/CN110950905A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101160334A (en) * | 2005-06-22 | 2008-04-09 | 日本聚氨酯工业株式会社 | Catalyst for isocyanurate bond formation reaction and process for producing isocyanurate-bond-containing modified polyisocyanate mixture with the same |
| CN101948483A (en) * | 2010-08-20 | 2011-01-19 | 王德兴 | Method for preparing calcium soap by utilizing quick lime and method for processing produced emulsified compound |
| CN104131163A (en) * | 2014-08-05 | 2014-11-05 | 南昌航空大学 | Regeneration method of P507 organic-phase emulsified mixture for extracting and separating rare earth |
| CN105132683A (en) * | 2015-09-15 | 2015-12-09 | 南昌航空大学 | Regeneration method of aged P507 organic phase |
| CN107384217A (en) * | 2016-03-31 | 2017-11-24 | 荒川化学工业株式会社 | The manufacture method and rosin ester of rosin ester |
Non-Patent Citations (3)
| Title |
|---|
| P507的纯化: "P507的纯化", 《有色金属》 * |
| 钟学明: "老化P507萃取剂再生研究", 《江西科学》 * |
| 黄可龙等: "钴盐结晶沉淀法纯化2-乙基己基膦单2-乙基己基酯", 《中南矿冶学院学报》 * |
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