CN107478767A - A kind of method for determining long-chain fat alcohol content in organic phospho acid solution - Google Patents
A kind of method for determining long-chain fat alcohol content in organic phospho acid solution Download PDFInfo
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Abstract
The present invention relates to a kind of method for determining long-chain fat alcohol content in organic phospho acid solution, it is related to field of hydrometallurgy.Solving existing chromatogram analysis method simply can not efficiently distinguish alcoholic extract hydroxyl group and phosphonate groups, it is impossible to monitor the technical problem of additive long-chain fat alcohol content.This method quantitatively adds standard long-chain fatty alcohol by extracting organic phase to organic phospho acid extractant, determine the extraction ability of organic phospho acid extractant under its different content, its extracting power and alcohol addition, the relation of organic phospho acid concentration is made, obtains standard curve and equation.Then, can be quantitative to obtain corresponding alcohol content by its extraction ability reference standard curvilinear equation for the alcohol in unknown system.This method can realize that the degree of accuracy is high to organic phase inner additive long-chain fatty alcohol stable content whether complete monitoring in Rare Earth Separation whole process, and method flexibility and reliability, realize simple and fast, online monitored over time and regulation and control truly.
Description
Technical field
The present invention relates to field of hydrometallurgy, and in particular to a kind of to determine long-chain fat alcohol content in organic phospho acid solution
Method.
Background technology
In recent years because heavy rare earth element holmium (Ho), yttrium (Y), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu) are situated between in laser
It is widely used in the key core material in the photoelectromagnetic such as matter, radiation source, scintillation crystal, magnetic material field, in high-tech and state
Irreplaceable effect is shown in anti-field.
World's heavy rare earth element is sparser, and main source concentrates on south China ionic ore deposit, and content is less than 5%.Tradition
Two (2- ethylhexyls) phosphonic acids-single 2-ethyl hexyl ester techniques to these have the heavy rare earth strategic resource of absolute competitive advantage without
Method realizes back extraction completely, restricts its separation and High Purity.Occurring some in succession is based on two (2- ethylhexyls) phosphonic acids-mono- at present
The new separating technology of 2- ethylhexyls.Chinese patent CN 1670228A disclose a kind of extraction system for adding modifying agent
The technique for separating heavy rare earth element.This method is effectively improved by adding a kind of long-chain fatty alcohol in organic extractant phase agent
Stripping efficiencies of two (2- ethylhexyls) phosphonic acids-single 2-ethyl hexyl esters to heavy rare earth in South Ore Deposit feed liquid, reduce back extraction acid
Degree, improve process green cleannes.
In above-mentioned process exploitation running, how the additive alcohol content in tracing and monitoring its extractant organic phase into
To examine the important step that can the technique be run steadily in the long term.At present, alcohol hydroxyl of the conventional chromatogram analysis method to additive
Base response sensitivity in by organic phase coexistent phosphonates influenceed serious, hydroxyl goes out peak position in alcoholic extract hydroxyl group and phosphonates
It is extremely close, held high when causing its content can not prepare to analyze, and being given up if other analyzable detection means such as nuclear-magnetism, mass spectrum etc.
It is expensive, and can not realize and the consecutive hours of a large amount of samples is monitored in fact.Still lack a kind of convenient simple means of testing at present to characterize
Content of this long-chain fatty alcohol additive in organic phase acidity phosphonates.
The content of the invention
The invention solves existing chromatogram analysis method simply can not efficiently distinguish alcoholic extract hydroxyl group and phosphonate groups, it is impossible to supervise
Survey the technical problem of additive long-chain fat alcohol content, there is provided one kind directly, simply, efficiently determines long in organic phospho acid solution
The method of chain fatty alcohol content, this method can be realized to be contained to organic phase inner additive long-chain fatty alcohol in Rare Earth Separation whole process
The complete monitoring whether stablized is measured, method flexibility and reliability, the degree of accuracy is high, realizes simple, quick, online whole process truly
Monitoring and regulation and control.
In order to solve the above-mentioned technical problem, technical scheme is specific as follows：
A kind of method for determining long-chain fat alcohol content in organic phospho acid solution, comprises the following steps：
Step 1, prepare series standard organic phospho acid solution to be measured and determine its extraction yield to rare earth feed liquid
The standard organic phospho acid solution to be measured includes organic phospho acid extractant, long-chain fatty alcohol and diluent, San Zheti
Fraction summation is 100%；
The organic phospho acid extractant concentration is 0.2-1.5mol/L, and the long-chain fat alcohol content is calculated by volume fraction
For the 0%-30% of standard organic phospho acid overall solution volume to be measured, 1 is in a ratio of：1；Calculating standard organic phospho acid solution to be measured
Extraction yield of the middle addition different content long-chain fatty alcohol to rare earth feed liquid；
The rare earth feed liquid is actual process feed liquid, acidity 0.4-1.0mol/L；
Step 2, the above-mentioned extraction yield data of fitting, draw extraction yield with organic phospho acid extractant in extraction organic phospho acid solution
With the rule of long-chain fatty alcohol additive level change, linear regression equation, standard control curve is made；
Step 3, for unknown organic phase to be measured in practical application, determine organic phospho acid extractant in organic phase to be measured first
Concentration, and then determine standard curve and equation corresponding to the concentration；Then after the extraction yield for measuring its corresponding rare earth feed liquid, lead to
Reference standard curve and equation are crossed, long-chain fat alcohol content in organic phospho acid solution can be calculated.
In the above-mentioned technical solutions, calculated in step 1 and different content long-chain fat is added in standard organic phospho acid solution to be measured
Fat alcohol concretely comprises the following steps to the extraction yield of rare earth feed liquid：
Standard containing different content long-chain fatty alcohol organic phospho acid solution to be measured is mixed with rare earth feed liquid, vibrated, quiet
After putting split-phase, a layer aqueous phase clear liquid is removed, with its raffinate aqueous phase middle rare earth concentration of disodium EDTA volumetric determination, so
Organic phase is obtained by minusing afterwards and has extracted rare earth concentration, is calculated in standard organic phospho acid solution to be measured and adds different content
Extraction yield of the long-chain fatty alcohol to rare earth feed liquid.
In the above-mentioned technical solutions, the organic phospho acid extractant is two (2- ethylhexyls) phosphonic acids, two (2- ethyl hexyls
Base) phosphonic acids-single 2-ethyl hexyl ester (P507) or 2,4,4- tri-methyl-amyl phosphonic acids.
In the above-mentioned technical solutions, the long-chain fatty alcohol is isooctanol.
In the above-mentioned technical solutions, the diluent is kerosene.
In the above-mentioned technical solutions, organic phospho acid extractant in determination of acid-basetitration organic phase to be measured is used in step 3
Concentration.
The beneficial effects of the invention are as follows：
The method of long-chain fat alcohol content passes through ethylenediamine tetra-acetic acid two in measure organic phospho acid solution provided by the invention
Sodium salt volumetric method, organic phase component in southern ionic ore deposit separating technology is analyzed, obtains wherein additive long-chain fat
The content of alcohol.Standard long-chain fatty alcohol is quantitatively added by extracting organic phase to organic phospho acid extractant, determines its different content
The extraction ability of lower organic phospho acid extractant, its extracting power and alcohol addition, the relation of organic phospho acid concentration is made, is marked
Directrix curve and equation.Then for the alcohol in unknown system, can quantitatively be obtained by its extraction ability reference standard curvilinear equation
Alcohol content must be corresponded to.It has the advantages that：
1st, measure alcohol content standard curve is drawn.Including different organic phospho acid extractant species, content and additive alcohol
Species, changes of contents is to the quantitative effect result of extraction yield.
2nd, each component concentration in the unknown sample of qualitative Accurate Determining., can be with by the comparison with above-mentioned standard curve and equation
Accurate quantitative analysis measures the content of additive long-chain fatty alcohol in organic phase.
3rd, can be realized using the present invention steady to organic phase inner additive long-chain fat alcohol content in Rare Earth Separation whole process
The complete monitoring whether determined, and method flexibility and reliability, the degree of accuracy is high, realizes simple and fast, online whole prison truly
Survey and regulate and control.
Brief description of the drawings
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
Fig. 1 is the extraction yield variation diagram of different isooctanol contents；
RE corresponding to the figure3+=0.102mol/L, H+=0.80mol/L, compared to 1：1；It is 1.35mol/L in P507 concentration
When, corresponding curvilinear equation is y1=-127.8564x1+94.9346, and wherein y1 represents extraction yield, and x1 represents isooctanol content；
When P507 concentration is 1.20mol/L, corresponding curvilinear equation is y2=-133.5942x2+93.0997, and wherein y2 represents extraction
Rate is taken, x2 represents isooctanol content.
Fig. 2 is the extraction yield variation diagram of different P507 contents；
Isooctanol (v/v)=10%, RE corresponding to the figure3+=0.102M, H+=0.80M, compared to 1：1, curvilinear equation is
Y3=149.5422x3+24.1188, wherein y3 represent extraction yield, and x3 represents P507 contents.
Embodiment
The present invention is described in detail below in conjunction with the accompanying drawings.
The method of long-chain fat alcohol content, specifically includes following steps in measure organic phospho acid solution provided by the invention：
Organic phase system in step 1, pre-simulated south ionic ore deposit separating technology, prepare series standard organic phosphine to be measured
Acid solution simultaneously determines its extraction yield to rare earth feed liquid；
The standard organic phospho acid solution to be measured includes organic phospho acid extractant, long-chain fatty alcohol and diluent, San Zheti
Fraction summation is 100%；
The organic phospho acid extractant concentration is 0.2-1.5mol/L, and the long-chain fat alcohol content is calculated by volume fraction
For the 0%-30% of standard organic phospho acid overall solution volume to be measured, 1 is in a ratio of：1；
Standard containing different content long-chain fatty alcohol organic phospho acid solution to be measured is mixed with rare earth feed liquid, vibrated, quiet
After putting split-phase, a layer aqueous phase clear liquid is removed, with its raffinate aqueous phase middle rare earth concentration of disodium EDTA volumetric determination, so
Organic phase is obtained by minusing afterwards and has extracted rare earth concentration, is calculated in standard organic phospho acid solution to be measured and adds different content
Extraction yield of the long-chain fatty alcohol to rare earth feed liquid.
It is preferred that the organic phospho acid extractant is two (2- ethylhexyls) phosphonic acids, two (2- ethylhexyls) phosphonic acids-mono- 2- second
Base hexyl ester (P507) or 2,4,4- tri-methyl-amyl phosphonic acids；The long-chain fatty alcohol is isooctanol；The diluent is kerosene.
Step 2, the above-mentioned extraction yield data of fitting, draw extraction yield with extractant and long-chain fat in extraction organic phospho acid solution
The rule of fat alcohol additive level change, linear regression equation, is made standard control curve.
Step 3, for unknown organic phase to be measured in practical application, using organic in determination of acid-basetitration organic phase to be measured
The concentration of phosphonic acids extractant, and then determine standard curve and equation corresponding to the concentration；Measure its extraction to corresponding rare earth feed liquid
After taking performance, by referring to standard curve and equation, long-chain fat alcohol content in organic phospho acid solution can be calculated.
Embodiment 1
Prepare what a series of different isooctanol concentration were fixed with two (2- ethylhexyls) phosphonic acids-single 2-ethyl hexyl ester concentration
Mixed organic solvents, actual conditions are as follows：The concentration of two (2- ethylhexyls) phosphonic acids-single 2-ethyl hexyl esters is 1.20mol/L,
Volume fraction is 40%；Isooctanol volume fraction is respectively 0%, 3%, 6%, 9%, 12%, 15%；Kerosene volume fraction is distinguished
For 60%, 57%, 54%, 51%, 48%, 45%；Aqueous phase liquid be certain enterprise south ionic ore deposit heavy rare earth Ho, Y, Er, Tm,
Yb, lutetium mixing rich material liquid, rare earth total concentration are 0.10mol/L, acidity 0.80mol/L.Take respectively above-mentioned six kinds it is organic
Phase 15mL and feed liquid 15mL, is mixed in 60mL separatory funnels, and at room temperature, 180rpm vibrates 30 minutes.After standing split-phase, remove
Layer aqueous phase clear liquid, with its raffinate aqueous phase middle rare earth concentration of disodium EDTA volumetric determination, then passes through minusing
Obtain organic phase and extracted rare earth concentration, calculate to obtain extraction yield.Draw under 1.20mol/L P507 concentration, extraction yield is with different different pungent
The standard curve of determining alcohol change.Standard straight-line and equation shown in solid obtained by the embodiment in Fig. 1.
Embodiment 2
Prepare what a series of different isooctanol concentration were fixed with two (2- ethylhexyls) phosphonic acids-single 2-ethyl hexyl ester concentration
Mixed organic solvents, actual conditions are as follows：The concentration of two (2- ethylhexyls) phosphonic acids-single 2-ethyl hexyl esters is 1.35mol/L,
Volume fraction is 33%；Isooctanol volume fraction is respectively 0%, 3%, 6%, 9%, 12%, 15%；Kerosene volume fraction is distinguished
For 67%, 64%, 61%, 58%, 55%, 52%；Aqueous phase liquid be certain enterprise south ionic ore deposit heavy rare earth Ho, Y, Er, Tm,
Yb, lutetium mixing rich material liquid, rare earth total concentration are 0.10mol/L, acidity 0.80mol/L.Take respectively above-mentioned six kinds it is organic
Phase 15mL and feed liquid 15mL, is mixed in 60mL separatory funnels, and at room temperature, 180rpm vibrates 30 minutes.After standing split-phase, remove
Layer aqueous phase clear liquid, with its raffinate aqueous phase middle rare earth concentration of disodium EDTA volumetric determination, then passes through minusing
Obtain organic phase and extracted rare earth concentration, calculate to obtain extraction yield.Draw under 1.35mol/L P507 concentration, extraction yield is with different different pungent
The standard curve of determining alcohol change.Dotted line show standard straight-line and equation obtained by the embodiment in Fig. 1.
Embodiment 3
Serial various concentrations two (2- ethylhexyls) phosphonic acids-single 2-ethyl hexyl ester is prepared to mix with same isooctanol concentration
Organic solution, actual conditions are as follows：The volume fraction of two (2- ethylhexyls) phosphonic acids-single 2-ethyl hexyl esters is respectively 30%,
33%th, 35%, 37%, 41%, 45%；Isooctanol volume fraction is 10%；Kerosene volume fraction is respectively 60%, 57%,
55%th, 53%, 49%, 45%；Aqueous phase liquid is certain enterprise south ionic ore deposit heavy rare earth Ho, Y, Er, Tm, Yb, lutetium mixing
Rich material liquid, rare earth total concentration are 0.10mol/L, acidity 0.80mol/L.Above-mentioned six kinds of organic phase 15mL and feed liquid are taken respectively
15mL, 60mL separatory funnels are mixed in, at room temperature, 180rpm vibrates 30 minutes.After standing split-phase, a layer aqueous phase clear liquid is removed,
With its raffinate aqueous phase middle rare earth concentration of disodium EDTA volumetric determination, organic phase has then been obtained by minusing
Extract rare earth concentration, calculate to obtain extraction yield.Extraction yield is drawn to extract with different two (2- ethylhexyls) phosphonic acids-single 2-ethyl hexyl esters
The standard curve of agent concentration change.Fig. 2 show standard curve and equation obtained by the embodiment.Illustrate that extractant is dense in organic phase
Degree is also continually changing.
Embodiment 4
Appropriate organic phase sample to be analyzed is taken, determines (2- ethylhexyls) phosphine two in organic phase first using acid-base titration
The concentration of acid-single 2-ethyl hexyl ester.At room temperature, by 15mL organic phases to be measured and 15mL aqueous phase material same as the previously described embodiments
Liquid vibrates 30 minutes in 60mL separatory funnels, 180rpm.After standing split-phase, a layer aqueous phase clear liquid is removed, with ethylenediamine tetra-acetic acid two
Its raffinate aqueous phase middle rare earth concentration of sodium salt volumetric determination, organic phase is then obtained by minusing and has extracted rare earth concentration, is calculated
Obtain extraction yield.According to the concentration of extractant two (2- ethylhexyls) phosphonic acids-single 2-ethyl hexyl ester, it is determined that the standard of institute's reference is bent
Line and equation, after extraction yield is substituted into equation, calculate and solve isooctanol concentration.
Organic phospho acid extractant described in above-described embodiment can also be two (2- ethylhexyls) phosphonic acids, 2,4,4- trimethyls
Amyl group phosphonic acids or other have conventional machine phosphonic acid extractant；The long-chain fatty alcohol can also be other conventional in the art
Long-chain fatty alcohol；The diluent can also be other diluents commonly used in the art, and the organic phospho acid extractant is dense
Degree can also be the arbitrary value in the range of 0.2-1.5mol/L, and the long-chain fat alcohol content, which can also be that the standard is to be measured, to be had
Arbitrary value in the range of the 0%-30% of machine phosphonic acid overall solution volume, the acidity of the rare earth feed liquid is 0.4-1.0mol/L scopes
Interior arbitrary value；Here no longer enumerate.
Obviously, above-described embodiment is only intended to clearly illustrate example, and is not the restriction to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of change or
Change.There is no necessity and possibility to exhaust all the enbodiments.And the obvious change thus extended out or
Among changing still in the protection domain of the invention.
Claims (6)
- A kind of 1. method for determining long-chain fat alcohol content in organic phospho acid solution, it is characterised in that comprise the following steps：Step 1, prepare series standard organic phospho acid solution to be measured and determine its extraction yield to rare earth feed liquidThe standard organic phospho acid solution to be measured includes organic phospho acid extractant, long-chain fatty alcohol and diluent, three's volume integral Number summation is 100%；The organic phospho acid extractant concentration is 0.2-1.5mol/L, and the long-chain fat alcohol content is calculated as institute by volume fraction The 0%-30% of standard organic phospho acid overall solution volume to be measured is stated, is in a ratio of 1：1；Add in calculating standard organic phospho acid solution to be measured Add extraction yield of the different content long-chain fatty alcohol to rare earth feed liquid；The rare earth feed liquid is actual process feed liquid, acidity 0.4-1.0mol/L；Step 2, the above-mentioned extraction yield data of fitting, draw extraction yield with organic phospho acid extractant and length in extraction organic phospho acid solution The rule of chain fatty alcohol additive level change, linear regression equation, is made standard control curve；Step 3, for unknown organic phase to be measured in practical application, determine the dense of organic phospho acid extractant in organic phase to be measured first Degree, and then determine standard curve and equation corresponding to the concentration；Then after the extraction yield for measuring its corresponding rare earth feed liquid, ginseng is passed through Sighting target directrix curve and equation, long-chain fat alcohol content in organic phospho acid solution can be calculated.
- 2. according to the method for claim 1, it is characterised in that calculate in step 1 and add in standard organic phospho acid solution to be measured Add different content long-chain fatty alcohol concretely comprising the following steps to the extraction yield of rare earth feed liquid：Standard containing different content long-chain fatty alcohol organic phospho acid solution to be measured is mixed with rare earth feed liquid, vibrated, stands and divides Xiang Hou, a layer aqueous phase clear liquid is removed, with its raffinate aqueous phase middle rare earth concentration of disodium EDTA volumetric determination, Ran Houtong Cross minusing acquisition organic phase and extracted rare earth concentration, addition different content long-chain in standard organic phospho acid solution to be measured is calculated Extraction yield of the fatty alcohol to rare earth feed liquid.
- 3. method according to claim 1 or 2, it is characterised in that the organic phospho acid extractant is two (2- ethyl hexyls Base) phosphonic acids, two (2- ethylhexyls) phosphonic acids-single 2-ethyl hexyl ester (P507) or 2,4,4- tri-methyl-amyl phosphonic acids.
- 4. method according to claim 1 or 2, it is characterised in that the long-chain fatty alcohol is isooctanol.
- 5. method according to claim 1 or 2, it is characterised in that the diluent is kerosene.
- 6. method according to claim 1 or 2, it is characterised in that to be measured organic using determination of acid-basetitration in step 3 The concentration of organic phospho acid extractant in phase.
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| JP2011225893A (en) * | 2002-08-08 | 2011-11-10 | Nippon Synthetic Chem Ind Co Ltd:The | Production method of aqueous polymer dispersion liquid |
| CN102676853A (en) * | 2012-05-28 | 2012-09-19 | 五矿（北京）稀土研究院有限公司 | Rare earth separation method with material linkage cyclic utilization function |
| CN103215448A (en) * | 2013-04-16 | 2013-07-24 | 内蒙古科技大学 | Method for extracting scandium from scandium-containing iron-rich acid liquor through P507 |
| CN103468950A (en) * | 2013-08-23 | 2013-12-25 | 中国科学院过程工程研究所 | Method for removing metal ion purity of rare earth aqueous solution extraction |
| CN104087750A (en) * | 2014-07-14 | 2014-10-08 | 厦门稀土材料研究所 | Rare earth extraction and separation method |
-
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- 2017-09-05 CN CN201710788284.9A patent/CN107478767B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011225893A (en) * | 2002-08-08 | 2011-11-10 | Nippon Synthetic Chem Ind Co Ltd:The | Production method of aqueous polymer dispersion liquid |
| CN102676853A (en) * | 2012-05-28 | 2012-09-19 | 五矿（北京）稀土研究院有限公司 | Rare earth separation method with material linkage cyclic utilization function |
| CN103215448A (en) * | 2013-04-16 | 2013-07-24 | 内蒙古科技大学 | Method for extracting scandium from scandium-containing iron-rich acid liquor through P507 |
| CN103468950A (en) * | 2013-08-23 | 2013-12-25 | 中国科学院过程工程研究所 | Method for removing metal ion purity of rare earth aqueous solution extraction |
| CN104087750A (en) * | 2014-07-14 | 2014-10-08 | 厦门稀土材料研究所 | Rare earth extraction and separation method |
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