CN103952551A - Method for preparing copper extraction agent LPA - Google Patents
Method for preparing copper extraction agent LPA Download PDFInfo
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- CN103952551A CN103952551A CN201410195817.9A CN201410195817A CN103952551A CN 103952551 A CN103952551 A CN 103952551A CN 201410195817 A CN201410195817 A CN 201410195817A CN 103952551 A CN103952551 A CN 103952551A
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- lpa
- extraction agent
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
The invention discloses a method for preparing a copper extraction agent LPA. The method comprises the following steps: mixing 2-hydroxy-5-nonyl benzaldoxime, 2-hydroxy-5-nonyl acetophenone oxime, 4-dodecyl-2-phenoly benzaldehyde and 2,2,4-trimethyl-1,3-pentanediol diisobutyrate at a mole ratio of (3-5):(1-3):1:0.5, so as to obtain a main material of the extraction agent, and mixing the main material of the extraction agent with kerosene at a volume ratio of 1:(3-9), so as to obtain the copper extraction agent LPA. The copper extraction agent LPA is applicable to extraction on copper of a material liquid of which the pH value is 2-8, and the efficiency is relatively high (as high as 98%).
Description
Technical field
The present invention relates to the preparation method of a kind of high-efficiency copper extraction agent LPA.
Background technology
Copper, as a kind of strategy metal, is widely used in the multiple industries such as electronic information, household electrical appliances and machinofacture.In industry, a large amount of contained waste liquids generate, and the recovery of therefore carrying out copper by extraction is the hot topic of current chemical industry research.Hydroxyl ketone (aldehyde) oxime is the more copper extractant of industrial application in recent years (as the lix984 of BASF); This extraction agent is with 2-hydroxyl-5-nonylacetophenone oxime and 4-dodecyl-Benzaldehyde,2-hydroxy, to take volume ratio 1:1 (being that mol ratio is as 1.07:1) to mix; Have advantages of that rate of extraction is fast, copper recovery is high, but its oxidation-resistance is poor, and is only applicable to the extraction of copper in low pH value (being that pH value is <3) solution.Therefore its application has certain limitation, and the performance of improving hydroxyl ketone (aldehyde) kind of extractants has more important using value.
Summary of the invention
The technical problem to be solved in the present invention is to provide strong, the applicable material liquid pH value scope of a kind of oxidation-resistance extensively and the high copper extractant of efficiency.
In order to solve the problems of the technologies described above, the invention provides the preparation method of a kind of copper extractant LPA: by 2-hydroxyl-5-nonyl benzene formoxime, 2-hydroxyl-5-nonylacetophenone oxime, suc as formula the 4-dodecyl-Benzaldehyde,2-hydroxy shown in I with suc as formula 2 shown in II, 2,4-trimethylammonium-1,3-pentanediol diisobutyrate according to the mixed in molar ratio of 3～5:1～3:1:0.5 after, obtain extraction agent major ingredient;
After extraction agent major ingredient is mixed according to the volume ratio of 1:3～9 (being preferably 1:3.5～4) with kerosene, obtain copper extractant LPA.
Improvement as the preparation method of copper extractant LPA of the present invention: described kerosene is sulfonated kerosene.
Further improvement as the preparation method of copper extractant LPA of the present invention: 2-hydroxyl-5-nonyl benzene formoxime, 2-hydroxyl-5-nonylacetophenone oxime, 4-dodecyl-Benzaldehyde,2-hydroxy and 2,2,4-trimethylammonium-1, the mol ratio of 3-pentanediol diisobutyrate: 4～4.9:2～2.9:1:0.5.
Copper extractant provided by the invention because of blend component (, 4-dodecyl-Benzaldehyde,2-hydroxy and 2,2,4-trimethylammonium-1, adding 3-pentanediol diisobutyrate) has stronger oxidation-resistance, can be applicable to pH value and be the extraction of copper in 2～8 feed liquid, and efficiency higher (up to 98%).
Embodiment
Room temperature refers to 10～30 ℃.
The preparation method of embodiment 1, a kind of copper extractant LPA,
Under room temperature, by 105g (0.4mol) 2-hydroxyl-5-nonyl benzene formoxime, 55g (0.2mol) 2-hydroxyl-5-nonylacetophenone oxime, 29g (0.1mol) 4-dodecyl-Benzaldehyde,2-hydroxy and 14.3g (0.05mol) 2,2,4-trimethylammonium-1,3-pentanediol diisobutyrate evenly mixes, and obtains extraction agent major ingredient (about 220ml); Add again 850mL kerosene (sulfonated kerosene), after mixing, obtain copper extractant LPA.
Embodiment 1 gained extraction agent LPA is tested:
Choosing copper (ion) concentration is the feed liquid that 5.0g/L, pH value are 2, is in a ratio of O/A=1:1 (volume ratio), 25 ℃ of the warm spots such as extraction, 25 ℃ of the warm spots such as back extraction, extraction time 30s, back extraction time 15s.Recording copper net transfer rate is 97%.Under the same terms, only change the pH of feed liquid, obtain percentage extraction under different pH, specifically as shown in table 1.
Remarks explanation: above-mentioned test, adopt copper sulfate, using dilute sulphuric acid as damping fluid and solvent.
For illustrate the present invention's four components in copper extraction synergy, compare with three component extracting agent of same concentrations, concrete data are in Table 1.
Remarks explanation:
Lack the 3rd component (aldehyde), be: cancel the use of the 4-dodecyl-Benzaldehyde,2-hydroxy in embodiment 1, all the other are with embodiment 1.
Lack the 4th component (ester), be: cancel 2,2 in embodiment 1,4-trimethylammonium-1, the use of 3-pentanediol diisobutyrate, all the other are with embodiment 1.
Table 1
PH by the applicable feed liquid of the visible extraction agent of the present invention of contrast of upper table 1 is wider, and extraction efficiency is higher.
In addition, it is stronger for extraction agent oxidation-resistance of the present invention is described, spy arranges following contrast degradation experiment: get the prepared extraction agent 100mL of embodiment 1, the hydrogen peroxide 20mL that adds wherein mass concentration 15%, at 25 ℃, stir 1 hour, the degradation rate that records major constituent aldoxime and ketoxime is 5%, and containing the extraction agent of the 3rd component degradation rate under the same conditions, is not 20%.
The preparation method of embodiment 2, a kind of copper extractant LPA,
Under room temperature, by 130g (0.49mol) 2-hydroxyl-5-nonyl benzene formoxime, 80g (0.29mol) 2-hydroxyl-5-nonylacetophenone oxime, 29g (0.1mol) 4-dodecyl-Benzaldehyde,2-hydroxy and 14.3g (0.05mol) 2,2,4-trimethylammonium-1,3-pentanediol diisobutyrate evenly mixes, and obtains extraction agent major ingredient (290ml); Add again 1000mL kerosene (sulfonated kerosene), after mixing, obtain copper extractant LPA.
Select test condition in the same manner as in Example 1, obtain result as table 2;
Table 2
| pH | Copper net transfer rate, % |
| 2 | 96 |
| 3 | 96 |
| 4 | 95 |
| 5 | 95 |
| 6 | 91 |
| 7 | 91 |
| 8 | 90 |
The copper extractant LPA of above-described embodiment 2 gained is carried out to the detection of oxidation-resistance in the manner described above, and acquired results is: with degradation rate under condition, be 6%.
Comparative example 1-1, the 4-dodecyl-Benzaldehyde,2-hydroxy in embodiment 1 is made into " 4-butyl-2-hydroxy phenyl aldehyde ", molar weight is constant; All the other contents are with embodiment 1.
Comparative example 1-2, make the 4-dodecyl-Benzaldehyde,2-hydroxy in embodiment 1 into " 4-propyl group-Benzaldehyde,2-hydroxy ", molar weight is constant; All the other contents are with embodiment 1.
Embodiment 1-3, by 29g (0.1mol), make the consumption of the 4-dodecyl-Benzaldehyde,2-hydroxy in embodiment 1 into " 54.23g (0.187mol) "; All the other contents are with embodiment 1.
Comparative example 2-1, " 2,2,4-trimethylammonium-1,3-pentanediol diisobutyrate " in embodiment 1 made into " diethyl succinate ", all the other contents are with embodiment 1.
Comparative example 2-2, " 2,2,4-trimethylammonium-1,3-pentanediol diisobutyrate " in embodiment 1 made into " ethylene sebacate ", all the other contents are with embodiment 1.
Comparative example 2-3, by embodiment 12,2,4-trimethylammonium-1, the consumption of 3-pentanediol diisobutyrate makes 7.15g (0.25mol) into by 14.3g (0.05mol); All the other contents are with embodiment 1.
Comparative example 2-4, by embodiment 12,2,4-trimethylammonium-1, the consumption of 3-pentanediol diisobutyrate makes 28.6g (0.1mol) into by 14.3g (0.05mol); All the other contents are with embodiment 1.
Comparative example 3, by 55g (0.2mol), make the 2-hydroxyl-5-nonylacetophenone oxime in embodiment 1 into 110g (0.4mol), that is, make 2-hydroxyl-5-nonyl benzene formoxime: the mol ratio 1:1 of 2-hydroxyl-5-nonylacetophenone oxime; All the other are with embodiment 1.
By above-mentioned all comparative examples according to described in embodiment 1, carry out copper net transfer rate under different pH and and the experiment of carrying out oxidation-resistance, acquired results is as following table 3:
Table 3
Finally, it is also to be noted that, what more than enumerate is only several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, can also have many distortion.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention, all should think protection scope of the present invention.
Claims (3)
1. the preparation method of copper extractant LPA, is characterized by:
By 2-hydroxyl-5-nonyl benzene formoxime, 2-hydroxyl-5-nonylacetophenone oxime, suc as formula the 4-dodecyl-Benzaldehyde,2-hydroxy shown in I with suc as formula 2 shown in II, 2,4-trimethylammonium-1,3-pentanediol diisobutyrate according to the mixed in molar ratio of 3～5:1～3:1:0.5 after, obtain extraction agent major ingredient;
After extraction agent major ingredient is mixed according to the volume ratio of 1:3～9 with kerosene, obtain copper extractant LPA.
2. the preparation method of copper extractant LPA according to claim 1, is characterized by: described kerosene is sulfonated kerosene.
3. the preparation method of copper extractant LPA according to claim 1 and 2, is characterized by:
2-hydroxyl-5-nonyl benzene formoxime, 2-hydroxyl-5-nonylacetophenone oxime, 4-dodecyl-Benzaldehyde,2-hydroxy and 2,2,4-trimethylammonium-1, the mol ratio of 3-pentanediol diisobutyrate: 4～4.9:2～2.9:1:0.5.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1175982A (en) * | 1995-02-16 | 1998-03-11 | 亨凯尔公司 | Modifiers for aldoxime extractant of metal values |
| CN101386912A (en) * | 2008-10-24 | 2009-03-18 | 南京市华凯化工有限公司 | Copper extractive agent |
| CN101914680A (en) * | 2010-08-20 | 2010-12-15 | 重庆浩康医药化工有限公司 | Copper extractant |
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2014
- 2014-05-11 CN CN201410195817.9A patent/CN103952551B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1175982A (en) * | 1995-02-16 | 1998-03-11 | 亨凯尔公司 | Modifiers for aldoxime extractant of metal values |
| CN101386912A (en) * | 2008-10-24 | 2009-03-18 | 南京市华凯化工有限公司 | Copper extractive agent |
| CN101914680A (en) * | 2010-08-20 | 2010-12-15 | 重庆浩康医药化工有限公司 | Copper extractant |
Non-Patent Citations (1)
| Title |
|---|
| 姚绪杰等: "脱氢枞胺水杨醛类席夫碱(Schiff Bases)对铜离子萃取性能的研究", 《江西农业大学学报》 * |
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Effective date of registration: 20181105 Address after: 629100 Jinqiao New District, Pengxi, Suining, Sichuan Patentee after: Zhijiang (Sichuan) high and New Material Application Technology Research Institute Co., Ltd. Address before: 629128 Jinqiao Industrial Port, Pengxi County, Suining, Sichuan Patentee before: SICHUAN ZHIJIANG ADVANCED MATERIALS CO., LTD. |