CN106698345A - Lithium deuteride production process and purity detection method of lithium deuteride - Google Patents
Lithium deuteride production process and purity detection method of lithium deuteride Download PDFInfo
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- CN106698345A CN106698345A CN201611222148.5A CN201611222148A CN106698345A CN 106698345 A CN106698345 A CN 106698345A CN 201611222148 A CN201611222148 A CN 201611222148A CN 106698345 A CN106698345 A CN 106698345A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
- C01B6/04—Hydrides of alkali metals, alkaline earth metals, beryllium or magnesium; Addition complexes thereof
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/14—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference
- G01N7/18—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference by allowing the material to react
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Abstract
The invention discloses a lithium deuteride production process and a concentration detection method of lithium deuteride. A reaction boat is put into a reaction device, metal lithium is added, the reaction device is sealed with a cover, the temperature is increased, and argon is introduced. The lithium deuteride production process has the beneficial effects that optimal production conditions can be confirmed, the production efficiency of the lithium deuteride can be improved, meanwhile the purity of the lithium deuteride can be precisely measured, and the product quality can be improved.
Description
Technical field
The present invention relates to industrial chemicals production field, the production technology of particularly a kind of lithium deuteride and its Concentration Testing side
Method.
Background technology
Lithium deuteride is a kind of special chemical products, molecular formula LiD, molecular weight 8.96, and outward appearance is in blue or greyish white toner
End.CAS：13587-16-1. density：0.906. 680 DEG C of fusing point, spontaneous combustion or ignite 200 DEG C of temperature, stablize at normal temperatures and pressures,
Must not be contacted with the object of oxide, acid, moisture (including humid air) and alcohol.Must be stored in ventilation shady and cool dry lazy
In property gas.
Deuterium is the isotope of hydrogen, and with the fast development of China's economy, the demand to lithium deuteride is growing day by day, and China
Production without deuteride before this, we develop the study on the synthesis of lithium deuteride in China first.
The content of the invention
The invention aims to solve the above problems, the production technology and its Concentration Testing of a kind of lithium deuteride are devised
Method.Specific design scheme is：
Lithium metal at a certain temperature with deuterium direct reaction, generate lithium deuteride, its reaction equation is：
In a reaction unit, a reaction boat is put into, adds lithium metal, sealed, started to warm up, be passed through argon gas.
Influence factor in lithium deuteride building-up process includes same position in reaction temperature, lithium metal purity, deuterium purity, deuterium
Plain abundance,
The reaction temperature of lithium deuteride synthesis is 690 DEG C -760 DEG C；
The reaction time of lithium deuteride synthesis is 7h-9h.
Detecting step is：
Step one, the conical flask for taking a dried and clean, the correct amount in a ten thousandth assay balance.
Step 2, take the sample that quality is w and be put into conical flask, it is tight to add a cover plug, correct amount.
Step 3, the mixed liquor of water and dioxane is added in constant pressure funnel.
Step 4, by constant pressure funnel with equipped with sample conical flask and gas constant pressure capacity tester be connected to become obturator
System.
Step 5, by the water level of barostat and graded tube to flat, accurately write down the ml numbers in each scale；
Step 6, the conical flask that will be equipped with sample are placed in ice-water bath；
Step 7, the water in constant pressure funnel and dioxane mixed liquor are added on the sample of conical flask, and note observation
Graded tube SEA LEVEL VARIATION；
Step 8, sample and water stand 10-20min in ice-water bath after completion of the reaction, and 0.4- is then stood at normal temperatures
0.6h；
Step 9, the water level of barostat and graded tube to flat, accurately write down the ml numbers in each graded tube.
Measuring principle is：
The measure of lithium deuteride purity is the measure according to active deuterium content, is computed and draws.Its principle is according to deuterate
Lithium can release deuterium, hydrogen with water reaction, determine the volume of deuterium and hydrogen and draw, reactive chemistry formula is：.
2LiD+2H2O→2LiOH+D2↑+H2↑。
Lithium deuteride purity detecting formula is：
In formula：
V1For sample not with the cumulative volume of gas in water reacting precursor system；
V2It is the volume of gas in system after sample and water reaction；
PtThe atmospheric pressure of environment during to determine；
PH2oThe saturated vapour pressure of water during to determine under environment temperature；
T0It is the temperature 273k under standard state；
TtSystem temperature (273+ room temperatures) k during to determine；
P0It is the gas pressure 1013.2472Pa under standard state；
W is the weight g of sample；
22400：Be constant, i.e., 1 molar any gas volume in normal conditions.
9：Be constant, i.e. the molecular weight of lithium deuteride.
In step 3, the volume parts of water and dioxane are：- 4 parts of water, -6 parts of dioxane；
In step one, weighing precision is a ten thousandth gram；
In step 2, weighing precision is a ten thousandth gram.
Cumulative volume V before sample reacts with water is obtained by step 51；
Sample and the reacted cumulative volume V of water are obtained by step 92。
The production technology and its concentration detection method of a kind of lithium deuteride obtained by above-mentioned technical proposal of the invention, its
Beneficial effect is：
Optimum producting condition can be determined, the production efficiency of lithium deuteride is improved, while being carried out accurately to the purity of lithium deuteride
Measurement, improve product quality.
Brief description of the drawings
Fig. 1 is the result figure that lithium deuteride production of the present invention is reacted at different conditions；
Specific embodiment
The present invention is specifically described below in conjunction with the accompanying drawings.
Lithium metal at a certain temperature with deuterium direct reaction, generate lithium deuteride, its reaction equation is：
In a reaction unit, a reaction boat is put into, adds lithium metal, sealed, started to warm up, be passed through argon gas.
Influence factor in lithium deuteride building-up process includes same position in reaction temperature, lithium metal purity, deuterium purity, deuterium
Plain abundance,
The reaction temperature of lithium deuteride synthesis is 700 DEG C -760 DEG C；
The reaction time of lithium deuteride synthesis is 7h-9h.
Detecting step is：
Step one, the conical flask for taking a dried and clean, the correct amount in a ten thousandth assay balance；
Step 2, take the sample that quality is w and be put into conical flask, it is tight to add a cover plug, correct amount；
Step 3, the mixed liquor of water and dioxane is added in constant pressure funnel；
Step 4, by constant pressure funnel with equipped with sample conical flask and gas constant pressure capacity tester be connected to become obturator
System；
Step 5, by the water level of barostat and graded tube to flat, accurately write down the ml numbers in each scale；
Step 6, the conical flask that will be equipped with sample are placed in ice-water bath；
Step 7, the water in constant pressure funnel and dioxane mixed liquor are added on the sample of conical flask, and note observation
Graded tube SEA LEVEL VARIATION；
Step 8, sample and water stand 10-20min in ice-water bath after completion of the reaction, and 0.4- is then stood at normal temperatures
0.6h；
Step 9, the water level of barostat and graded tube to flat, accurately write down the ml numbers in each graded tube.
Measuring principle is：
The measure of lithium deuteride purity is the measure according to active deuterium content, is computed and draws.Its principle is according to deuterate
Lithium can release deuterium, hydrogen with water reaction, determine the volume of deuterium and hydrogen and draw, reactive chemistry formula is：.
2LiD+2H2O→2LiOH+D2↑+H2↑。
Lithium deuteride purity detecting formula is：
In formula：
V1For sample not with the cumulative volume of gas in water reacting precursor system；
V2It is the volume of gas in system after sample and water reaction；
PtThe atmospheric pressure of environment during to determine；
PH2oThe saturated vapour pressure of water during to determine under environment temperature；
T0It is the temperature 273k under standard state；
TtSystem temperature (273+ room temperatures) k during to determine；
P0It is the gas pressure 1013.2472Pa under standard state；
W is the weight g of sample；
22400：Be constant, i.e., 1 molar any gas volume in normal conditions.
9：Be constant, i.e. the molecular weight of lithium deuteride.
In step 3, the volume parts of water and dioxane are：- 4 parts of water, -6 parts of dioxane；
In step one, weighing precision is a ten thousandth gram；
In step 2, weighing precision is a ten thousandth gram.
Cumulative volume V before sample reacts with water is obtained by step 51；
Sample and the reacted cumulative volume V of water are obtained by step 92。
Embodiment 1
In a reaction unit, a reaction boat is put into, adds 100g lithium metals, sealed, started to warm up, be passed through argon
Gas.
Fig. 1 is the result figure that lithium deuteride production of the present invention is reacted at different conditions, as shown in figure 1,
Reaction temperature is a vital factor, and at 600 DEG C or so, reaction, it is impossible to carry out can in 650 DEG C of reactions
To carry out, but speed is very slow, can preferably be carried out in 690 DEG C of reactions.Reaction efficiency is significantly improved more than 700 DEG C, 740
DEG C when reflect best results.
Above-mentioned technical proposal only embodies the optimal technical scheme of technical solution of the present invention, those skilled in the art
Some that to be made to some of which part variations embody principle of the invention, belong to protection scope of the present invention it
It is interior.
Claims (8)
1. a kind of synthetic method of lithium deuteride, it is characterised in that lithium metal at a certain temperature with deuterium direct reaction, generate deuterium
Change lithium, its reaction equation is：
2. the synthetic method of the lithium deuteride according to claim 1, it is characterised in that in a reaction unit, be put into
One reaction boat, adds lithium metal, seals, and starts to warm up, and is passed through argon gas.
3. the synthetic method of the lithium deuteride according to claim 1, it is characterised in that the influence in lithium deuteride building-up process
Factor includes isotope abundance in reaction temperature, lithium metal purity, deuterium purity, deuterium,
The reaction temperature of lithium deuteride synthesis is 690 DEG C -760 DEG C；
The reaction time of lithium deuteride synthesis is 7h-9h.
4. a kind of lithium deuteride method for detecting purity, it is characterised in that detecting step is：
Step one, the conical flask for taking a dried and clean, the correct amount in a ten thousandth assay balance；
Step 2, take the sample that quality is w and be put into conical flask, it is tight to add a cover plug, correct amount；
Step 3, the mixed liquor of water and dioxane is added in constant pressure funnel；
Step 4, by constant pressure funnel with equipped with sample conical flask and gas constant pressure capacity tester be connected to become closed system；
Step 5, by the water level of barostat and graded tube to flat, accurately write down the ml numbers in each scale；
Step 6, the conical flask that will be equipped with sample are placed in ice-water bath；
Step 7, the water in constant pressure funnel and dioxane mixed liquor are added on the sample of conical flask, and note observing scale
Pipe SEA LEVEL VARIATION；
Step 8, sample and water stand 10-20min in ice-water bath after completion of the reaction, and 0.4-0.6h is then stood at normal temperatures；
Step 9, the water level of barostat and graded tube to flat, accurately write down the ml numbers in each graded tube.
5. the lithium deuteride method for detecting purity according to claim 4, it is characterised in that measuring principle is：
The measure of lithium deuteride purity is the measure according to active deuterium content, is computed and draws.Its principle is can according to lithium deuteride
Deuterium, hydrogen are released with water reaction, the volume of deuterium and hydrogen is determined and is drawn, reactive chemistry formula is：.
2LiD+2H2O→2LiOH+D2↑+H2↑。
6. the lithium deuteride method for detecting purity according to claim 4, it is characterised in that
Lithium deuteride purity detecting formula is：
In formula：
V1For sample not with the cumulative volume of gas in water reacting precursor system；
V2It is the volume of gas in system after sample and water reaction；
PtThe atmospheric pressure of environment during to determine；
PH2oThe saturated vapour pressure of water during to determine under environment temperature；
T0It is the temperature 273k under standard state；
TtSystem temperature (273+ room temperatures) k during to determine；
P0It is the gas pressure 1013.2472Pa under standard state；
W is the weight g of sample；
22400：Be constant, i.e., 1 molar any gas volume in normal conditions.
9：Be constant, i.e. the molecular weight of lithium deuteride.
7. the lithium deuteride method for detecting purity according to claim 4, it is characterised in that in step 3, water and dioxy six
The volume parts of ring are：- 4 parts of water, -6 parts of dioxane；
In step one, weighing precision is a ten thousandth gram；
In step 2, weighing precision is a ten thousandth gram.
8. the lithium deuteride method for detecting purity according to claim 4, it is characterised in that
Cumulative volume V before sample reacts with water is obtained by step 51；
Sample and the reacted cumulative volume V of water are obtained by step 92。
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| CN201611222148.5A CN106698345A (en) | 2016-12-19 | 2016-12-19 | Lithium deuteride production process and purity detection method of lithium deuteride |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108358167A (en) * | 2018-02-11 | 2018-08-03 | 庄英俊 | A kind of preparation of deuterate aluminium lithium and detection method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102901796A (en) * | 2011-07-28 | 2013-01-30 | 车瀛照 | Gas constant pressure capacity tester |
| CN104176749A (en) * | 2014-07-02 | 2014-12-03 | 北京理工大学 | Method for preparing lithium deuteride by using high-temperature direct manner |
-
2016
- 2016-12-19 CN CN201611222148.5A patent/CN106698345A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102901796A (en) * | 2011-07-28 | 2013-01-30 | 车瀛照 | Gas constant pressure capacity tester |
| CN104176749A (en) * | 2014-07-02 | 2014-12-03 | 北京理工大学 | Method for preparing lithium deuteride by using high-temperature direct manner |
Non-Patent Citations (1)
| Title |
|---|
| 连培生编著: "《原子能工业》", 31 May 2002, 原子能出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108358167A (en) * | 2018-02-11 | 2018-08-03 | 庄英俊 | A kind of preparation of deuterate aluminium lithium and detection method |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20180112 Address after: No. 204, No. 53 building, Southwest Village, Nankai University, Tianjin, Nankai District, Tianjin Applicant after: Che Yingzhao Address before: 300071 Nankai University, Nankai District, Southwest Village, building 3, building 2, No. 204, No. Applicant before: Che Rongrui |
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| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170524 |