CN1090217A - Method with separating Li isotope with titanium hydrogen diphosphate - Google Patents
Method with separating Li isotope with titanium hydrogen diphosphate Download PDFInfo
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- CN1090217A CN1090217A CN 93101205 CN93101205A CN1090217A CN 1090217 A CN1090217 A CN 1090217A CN 93101205 CN93101205 CN 93101205 CN 93101205 A CN93101205 A CN 93101205A CN 1090217 A CN1090217 A CN 1090217A
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- titanium
- isotope
- separating
- titanium hydrogen
- phosphoric acid
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Abstract
The present invention relates to a kind of method with separating Li isotope with titanium hydrogen diphosphate, amorphous phosphoric acid titanium is added in the phosphoric acid, reaction makes crystalline form two water titanium hydrogen diphosphates under HTHP, and the interlamellar spacing of its molecule is 7.6 dusts; With its granulation and make chromatographic column,, exchange the nitric acid wash-out cylinder of saturated back, but the light isotope of enriching lithium ion in the outflow liquid can make just after the multi-stage separation with 0.15-0.25mol with the lithium nitrate solution of the 0.15-0.25mol cylinder of flowing through
6Li obtains enrichment greatly; The elemental lithium that obtains with this method
7Li/
6The abundance ratio of Li is higher; And the exchange capacity of potassium, rubidium, caesium is improved; With this method separating Li element isotope with compare nontoxicly, harmless with the mercurial method, production method is simple, cost is low, suitability for industrialized production has more advantage.
Description
The present invention relates to a kind of method with separating Li isotope with titanium hydrogen diphosphate; Earlier titanium tetrachloride is added in phosphoric acid and the hydrochloric acid, reaction at normal temperatures and pressures makes amorphous phosphoric acid titanium.
Synthesized titanium hydrogen diphosphate (Ti(HPO at E.Kobayashi in 1975
4)
2NH
2O), (n=0,0.5), anhydrous and hemihydrate; And find that they have higher exchange capacity to the bigger potassium ion of ionic radius; But be applied to elemental lithium isotopic separation technology and do not find similar techniques by retrieval as yet, most of elemental lithiums separation all adopt the mercurial method to separate, but the mercurial method is harmful.
The objective of the invention is to provide that a kind of isolation technics is simple, cost of material is low for fear of above-mentioned the deficiencies in the prior art part, harmless, nontoxic, can improve method with separating Li isotope with titanium hydrogen diphosphate to the isotopic separation factor of elemental lithium and alkali metal ion exchange capacity and isotopic separation factor.
Purpose of the present invention can realize by following measure:
A kind of method with separating Li isotope with titanium hydrogen diphosphate; Earlier titanium tetrachloride is added in phosphoric acid and the hydrochloric acid, reaction at normal temperatures and pressures makes amorphous phosphoric acid titanium; Amorphous phosphoric acid titanium is added in the phosphoric acid, and reaction makes crystalline form two water titanium hydrogen diphosphates under HTHP, and its molecular formula is Ti(HPO
4)
22H
2O, the interlamellar spacing of molecule shortens to 7.6 dusts; Titanium hydrogen diphosphate is granulated, make ion-exchange chromatography, flow through in the post with the hydrochloric acid solution of 0.1-0.2mol, make it be transformed into hydrogen (H) type, be neutrality or subacidity (PH=5-7) with the deionized water washing to flowing out liquid then, again with the nitrate solution of the lithium of the 0.15-0.25mol cylinder of flowing through, exchange saturated after, do not have lithium ion with the deionized water washing in the liquid to flowing out; Use the nitric acid liquid wash-out cylinder of 0.15-0.25mol then, but flow out enrichment ' Li in the liquid; Just can make after the multi-stage separation ' Li obtains enrichment greatly.
Purpose of the present invention also can realize by following measure:
With the method for separating Li isotope with titanium hydrogen diphosphate, the temperature of synthetic crystalline form titanium hydrogen diphosphate is 150-175 ℃, and pressure is 30-40 atmospheric pressure, reaction time 5-72 hour; P in the titanium hydrogen diphosphate of crystalline form
2O
5, TiO
2With H
2The mol ratio of O is 1: (0.96～1.02): (2.01～2.08), also the acceptable salts pickling is taken off cylinder and is obtained the light isotope of the lithium ion of enrichment, and titanium hydrogen diphosphate also can improve exchange capacity and its isotopic separation factor of potassium, rubidium, cesium element in addition.
The present invention has following advantage compared to existing technology:
1, the present invention adopts two synthetic quartzy shape titanium hydrogen diphosphates of pressure to make chromatographic column, makes the nitrate solution of the lithium cylinder of flowing through, exchange saturated after, get final product enrichment ' Li through wash-out and multistage operations, the method for separated isotopes is simple.
2, the present invention shortens to 7.6 dusts in the molecular layer spacing of two synthetic hydration crystalline form titanium hydrogen diphosphates of pressure by former 11.8 dusts, the isotopic separating effect of elemental lithium is greatly improved, and its exchange capacity is had by a relatively large margin raising.
3, to adopt separating Li isotope with titanium hydrogen diphosphate to compare with amalgam process safe and harmless, nontoxic in the present invention.
4, the present invention also can improve the exchange capacity and the separation factor of alkali family metallic element potassium, rubidium, caesium.
5, cost of material of the present invention is low, and industrialized production has advantage.
The present invention also will be described in further detail in conjunction with the embodiments:
Embodiment one:
Earlier make amorphous phosphoric acid titanium at normal temperatures and pressures, the phosphoric acid that to get 1 part of amorphous phosphoric acid titanium and 5 parts of concentration be 10.4mol/l adds in the autoclave, under 150 ℃ of temperature, pressure is 30 atmospheric pressure, react and made two quartzy shape titanium hydrogen diphosphates in 5 hours; Its molecular formula is Ti(HPO
4)
22H
2O, the interlamellar spacing of molecule is 7.6 dusts; P in the titanium hydrogen diphosphate that obtains
2O
5, TiO
3With H
2The mol ratio of O is 1.00: 1.02: 2.08; Titanium hydrogen diphosphate is made chromatographic column, and the hydrochloric acid stream of using 0.1mol makes it be transformed into hydrogen (H) type in post, is neutral with the deionized water washing in the liquid to flowing out again, uses the LiNO of 0.15mol again
3Flow of solution is adsorbed saturated lithium ion through cylinder on the exchange column; And then with the nitric acid wash-out exchange column of 0.15mol, eluting temperature is that 18 ℃, flow velocity are 15mol/h, and flowing out the liquid measurement result is Li
+Concentration (mg/ml) 0.369, the abundance ratio of ' Li/ ' Li are 11.7809, and separation factor is the 1.023(single-stage), wherein separating factor in 1.023 districts, Li
+Amount accounts for 91.62% of total discharge.
Embodiment two:
Charge ratio is 30 atmospheric pressure, reaction time to be to make two quartzy shape titanium hydrogen diphosphates in 8 hours at 175 ℃ of temperature, pressure with example together; P in the product
2O
5, TiO
2With H
2The mol ratio of O is 1.00: 0.96: 2.01, and its interlamellar spacing is 7.6 dusts; Titanium hydrogen diphosphate is made chromatographic column is transformed into hydrogen (H) type, again with the lithium nitrate solution of 0.25mol flow through cylinder exchange saturated after, with the hydrochloric acid wash-out cylinder of 0.25mol; Flowing out the liquid measurement result is 11: 6087 for the abundance ratio of ' Li/ ' Li, and separation factor is 1.038.
Embodiment three:
Measure its exchange capacity with adding the two hydration titanium hydrogen diphosphates that are pressed into static method to potassium ion, the result shows: equal at the reaction medium pH value under 4.29 the acidity, its exchange capacity reaches 10.51meq/g, descends the exchange capacity of synthetic dihydrate to improve nearly 5 times than normal pressure; With comparing with and the exchange capacity semihydrate that is celebrated big to potassium ion exchange capacity is its 2.5 times; Potassium ion solution is Klorvess Liquid, and the exchange reaction time is under 24 hours, the 20 ℃ conditions, regulates pH value with KOH.
Embodiment four:
Add the dihydrate that is pressed into, with the exchange capacity of static method mensuration lithium ion, the reaction medium pH value is 5.62 o'clock, and its exchange capacity is 9.48meq/g, descends the exchange capacity of synthetic dihydrate to exceed nearly 3 times than normal pressure; Lithium solution is LiNO
3Preparation, the reaction medium pH value is regulated with LiOH, and reaction temperature is that 20 ℃, reaction time are 24 hours.
Claims (4)
1, a kind of method with separating Li isotope with titanium hydrogen diphosphate; Earlier titanium tetrachloride is added in phosphoric acid and the hydrochloric acid, reaction at normal temperatures and pressures makes amorphous phosphoric acid titanium; It is characterized in that amorphous phosphoric acid titanium is added in the phosphoric acid, reaction makes crystalline form two water titanium hydrogen diphosphates under HTHP, and its molecular formula is Ti (HPO
4)
22H
2O, the interlamellar spacing of molecule shortens to 7.6 dusts; Titanium hydrogen diphosphate is granulated, make ion-exchange chromatography, flow through in the post with the hydrochloric acid solution of 0.1-0.2mol, make it be transformed into hydrogen (H) type, be neutrality or subacidity (PH=5-7) with the deionized water washing to flowing out liquid then, again with the nitrate solution of the lithium of the 0.15-0.25mol cylinder of flowing through, exchange saturated after, do not have lithium ion with the deionized water washing in the liquid to flowing out; Use the nitric acid liquid wash-out cylinder of 0.15-0.25mol then, but flow out enrichment light isotope in the liquid
6Li; Just can make after the multi-stage separation
6Li obtains enrichment greatly.
2, the method with separating Li isotope with titanium hydrogen diphosphate as claimed in claim 1 is characterized in that the temperature of synthetic crystalline form two water titanium hydrogen diphosphates is 150-175 ℃, and pressure is 30-40 atmospheric pressure, reaction time 5-72 hour; P in the two water titanium hydrogen diphosphates of crystalline form
2O
5, TiO
2With H
2The mol ratio of O is 1: (0.96～1.02): (2.01～2.08).
3, the method with separating Li isotope with titanium hydrogen diphosphate as claimed in claim 1, it is characterized in that going back the acceptable salts pickling take off cylinder and obtain enrichment ' Li.
4, as claim 1,2 described methods, it is characterized in that titanium hydrogen diphosphate also can improve the exchange capacity of potassium, rubidium, cesium element with separating Li isotope with titanium hydrogen diphosphate; Also can improve the separation factor of potassium, rubidium, cesium isotope simultaneously.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93101205 CN1090217A (en) | 1993-01-18 | 1993-01-18 | Method with separating Li isotope with titanium hydrogen diphosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93101205 CN1090217A (en) | 1993-01-18 | 1993-01-18 | Method with separating Li isotope with titanium hydrogen diphosphate |
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| Publication Number | Publication Date |
|---|---|
| CN1090217A true CN1090217A (en) | 1994-08-03 |
Family
ID=4983466
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93101205 Pending CN1090217A (en) | 1993-01-18 | 1993-01-18 | Method with separating Li isotope with titanium hydrogen diphosphate |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0975676A (en) * | 1995-09-08 | 1997-03-25 | Agency Of Ind Science & Technol | Lithium isotope separating agent |
| CN102430338A (en) * | 2011-12-16 | 2012-05-02 | 江南大学 | Method for extracting and separating lithium isotope aqueous solution |
| CN103736395A (en) * | 2013-12-18 | 2014-04-23 | 中国原子能科学研究院 | Lithium isotope separation method and single-stage separation factor measurement method thereof |
| CN103754899A (en) * | 2014-01-14 | 2014-04-30 | 中国科学院青海盐湖研究所 | Method for extracting caesium from mixed-salt solution |
| CN104147929A (en) * | 2013-06-17 | 2014-11-19 | 中国科学院上海有机化学研究所 | Novel reflux cascade technology for producing lithium-7 isotopes |
| CN104310364A (en) * | 2014-10-11 | 2015-01-28 | 昆明理工大学 | Comprehensive utilization method of phosphoric acid sludge |
| CN105498542A (en) * | 2015-12-17 | 2016-04-20 | 中国科学院青海盐湖研究所 | Method for extracting lithium isotopes |
-
1993
- 1993-01-18 CN CN 93101205 patent/CN1090217A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0975676A (en) * | 1995-09-08 | 1997-03-25 | Agency Of Ind Science & Technol | Lithium isotope separating agent |
| JP2775412B2 (en) | 1995-09-08 | 1998-07-16 | 工業技術院長 | Lithium isotope separating agent |
| CN102430338A (en) * | 2011-12-16 | 2012-05-02 | 江南大学 | Method for extracting and separating lithium isotope aqueous solution |
| CN102430338B (en) * | 2011-12-16 | 2014-08-13 | 江南大学 | Method for extracting and separating lithium isotope aqueous solution |
| CN104147929A (en) * | 2013-06-17 | 2014-11-19 | 中国科学院上海有机化学研究所 | Novel reflux cascade technology for producing lithium-7 isotopes |
| CN103736395A (en) * | 2013-12-18 | 2014-04-23 | 中国原子能科学研究院 | Lithium isotope separation method and single-stage separation factor measurement method thereof |
| CN103754899A (en) * | 2014-01-14 | 2014-04-30 | 中国科学院青海盐湖研究所 | Method for extracting caesium from mixed-salt solution |
| CN104310364A (en) * | 2014-10-11 | 2015-01-28 | 昆明理工大学 | Comprehensive utilization method of phosphoric acid sludge |
| CN104310364B (en) * | 2014-10-11 | 2017-01-18 | 昆明理工大学 | Comprehensive utilization method of phosphoric acid sludge |
| CN105498542A (en) * | 2015-12-17 | 2016-04-20 | 中国科学院青海盐湖研究所 | Method for extracting lithium isotopes |
| CN105498542B (en) * | 2015-12-17 | 2017-07-28 | 中国科学院青海盐湖研究所 | The method for extracting lithium isotope |
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