CN102417199A - Preparation method of spectroscopically pure strontium chloride - Google Patents
Preparation method of spectroscopically pure strontium chloride Download PDFInfo
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- CN102417199A CN102417199A CN2011102543140A CN201110254314A CN102417199A CN 102417199 A CN102417199 A CN 102417199A CN 2011102543140 A CN2011102543140 A CN 2011102543140A CN 201110254314 A CN201110254314 A CN 201110254314A CN 102417199 A CN102417199 A CN 102417199A
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- strontium chloride
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Abstract
The invention relates to a preparation method of spectroscopically pure strontium chloride. The method comprises steps of: placing strontium carbonate in a stainless steel vessel, adding distilled water, dissolving, filtering, filling a filtrate into the stainless steel vessel, adding hydrochloric acid till end of CO2 generation to obtain a strontium chloride solution, wherein a reaction terminal point has a pH of 4.5-5 and a solution concentration of 30-32 Be; heating the strontium chloride solution to 90-95 DEG C, adding dilute sulfuric acid and hydrogen peroxide successively, stopping heating, standing for 40-60 min and filtering to obtain a strontium chloride solution A; carrying out concentration on the solution A till a solution concentration of 40-42 Be, stopping heating, cooling for crystallization and drying the crystallization to obtain the spectroscopically pure strontium chloride. According to the preparation method of the spectroscopically pure strontium chloride, a reaction between strontium carbonate and hydrochloric acid is employed, and a reaction terminal point is controlled; product impurities, soluble barium and iron are deprived by adding sulfuric acid and hydrogen peroxide, so as to prepare the spectroscopically pure strontium chloride.
Description
Technical field
The present invention relates to mineral compound preparation method field, especially a kind of preparation method of spectroscopically pure strontium chloride.
Background technology
The spectroscopically pure strontium chloride is applied in production of kinescope, also is used for the production of fireworks and medicine.At present; The method for preparing employing of spectroscopically pure strontium chloride is a double decomposition, and it utilizes strontium nitrate solution and hydrochloric acid reaction, generates strontium chloride; The strontium chloride purity that this kind method is produced is low, foreign matter content is high, can not satisfy the needs of high request product in the electronic industry.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, the preparation method of the spectroscopically pure strontium chloride that a kind of foreign matter content is low, purity is high, process step is simple, production efficiency is higher is provided.
The present invention solves its technical problem and takes following technical scheme to realize:
A kind of preparation method of spectroscopically pure strontium chloride, preparing method's concrete steps are:
(1) removal of impurity, synthesizing chlorinated strontium solution
Strontium carbonate powder is placed Stainless Steel Ware, add zero(ppm) water, be heated to 60-70 ℃ and dissolve, filter, in the impouring Stainless Steel Ware of will filtrating again, add hydrochloric acid, until no longer producing CO
2Till, reaction end is pH=4.5-5, strength of solution is 30-32Be, obtains strontium chloride solution; Again strontium chloride solution is heated to 90-95 ℃, successively adds dilute sulphuric acid and ydrogen peroxide 50,, stop heating, leave standstill 40-60min, filter, the strontium chloride solution A obtains filtrating;
The dilute sulphuric acid that adds, ydrogen peroxide 50 are 0.01: 0.02: 1 with the weight ratio of Strontium carbonate powder respectively;
(2) preparation spectroscopically pure strontium chloride
Strontium chloride solution A with step (1) obtains concentrates, to strength of solution be 40-42Be, stop the heating, crystallisation by cooling, crystallization obtains the spectroscopically pure strontium chloride through drying.
And Strontium carbonate powder in the said step (1): zero(ppm) water: the weight ratio of hydrochloric acid is 1: 3: 3.
And Strontium carbonate powder is an analytical pure in the said step (1).
And, the specific density 1.18 of hydrochloric acid in the said step (1), the hydrochloric acid massfraction is 31%.
And the container in the said step (1) is a stainless steel cask; Use B to filter during filtration; Under constantly stirring, slowly add when adding hydrochloric acid.
And the thickening temperature in the said step (2) is 230-250 ℃; Crystallization uses drier to dry.
And the weight fraction of said dilute sulphuric acid is 6-8%, the mark 28-30% of ydrogen peroxide 50.
Advantage of the present invention and beneficial effect are:
1, the preparation method of this spectroscopically pure strontium chloride adopts Strontium carbonate powder and hydrochloric acid reaction, controls reaction end, reaches through adding dilute sulphuric acid and ydrogen peroxide 50 and removes product impurity, solubility barium and iron, makes the spectroscopically pure strontium chloride.
2, the spectroscopically pure strontium chloride purity that makes of the present invention is high, foreign matter content is low, preparation technology is simple, better results.
Embodiment
Do further detailed description below in conjunction with embodiment, following examples are descriptive, are not determinate, can not limit protection scope of the present invention with this.
Embodiment 1
A kind of preparation method of spectroscopically pure strontium chloride, preparing method's concrete steps are:
(1) removal of impurity, synthesizing chlorinated strontium solution
2kg puts into stainless steel cask with the analytical pure Strontium carbonate powder; Put into zero(ppm) water 6kg, heat 60 ℃ and dissolve, filter with B; Again filtrating is put into stainless steel cask; Under constantly stirring, slowly add hydrochloric acid (specific density is 1.18, and the hydrochloric acid massfraction is 31%) 6kg, until no longer producing CO
2Till.Reaction end is pH value of solution=4, and strength of solution is 30Be, obtains strontium chloride solution; This solution is heated to 90 ℃; Successively add the dilute sulphuric acid of 0.02kg 6wt% and the ydrogen peroxide 50 of 0.04kg 28wt%, stop heating, leave standstill 40min; Filtrating is filtered (to remove soluble barium salt and iron) with B, and the strontium chloride solution A obtains filtrating;
(2) preparation spectroscopically pure strontium chloride
Strontium chloride solution A with step (1) obtains concentrates, and thickening temperature is 230 ℃, is 40Be through being concentrated into strength of solution, stops heating, crystallisation by cooling, and crystallization dries through drier and obtains the spectroscopically pure strontium chloride.
Embodiment 2
A kind of preparation method of spectroscopically pure strontium chloride, preparing method's concrete steps are:
(1) removal of impurity, synthesizing chlorinated strontium solution
3kg puts into stainless steel cask with the analytical pure Strontium carbonate powder; Put into zero(ppm) water 9kg, heat 70 ℃ and dissolve, filter with B; Again filtrating is put into stainless steel cask; Under constantly stirring, slowly add hydrochloric acid (specific density is 1.18, and the hydrochloric acid massfraction is 31%) 9kg, until no longer producing CO
2Till.Reaction end is pH value of solution=5, and strength of solution is 32Be, obtains strontium chloride solution; And this solution is heated under 95 ℃ of situation; Successively add the dilute sulphuric acid of 0.03kg8wt% and the ydrogen peroxide 50 of 0.06kg30wt%, stop heating, leave standstill 60min; Filtrating is filtered (to remove soluble barium salt and iron) with B, and the strontium chloride solution A obtains filtrating;
(2) preparation spectroscopically pure strontium chloride
Strontium chloride solution A with step (1) obtains concentrates, and thickening temperature is 250 ℃, is 42Be through being concentrated into strength of solution, stops heating, crystallisation by cooling, and crystallization dries through drier and obtains the spectroscopically pure strontium chloride.
Claims (7)
1. the preparation method of a spectroscopically pure strontium chloride, it is characterized in that: preparing method's concrete steps are:
(1) removal of impurity, synthesizing chlorinated strontium solution
Strontium carbonate powder is placed Stainless Steel Ware, add zero(ppm) water, be heated to 60-70 ℃ and dissolve, filter, in the impouring Stainless Steel Ware of will filtrating again, add hydrochloric acid, until no longer producing CO
2Till, reaction end is pH=4.5-5, strength of solution is 30-32Be, obtains strontium chloride solution; Again strontium chloride solution is heated to 90-95 ℃, successively adds dilute sulphuric acid and ydrogen peroxide 50,, stop heating, leave standstill 40-60min, filter, the strontium chloride solution A obtains filtrating;
The dilute sulphuric acid that adds, ydrogen peroxide 50 are 0.01: 0.02: 1 with the weight ratio of Strontium carbonate powder respectively;
(2) preparation spectroscopically pure strontium chloride
Strontium chloride solution A with step (1) obtains concentrates, to strength of solution be 40-42Be, stop the heating, crystallisation by cooling, crystallization obtains the spectroscopically pure strontium chloride through drying.
2. the preparation method of spectroscopically pure strontium chloride according to claim 1 is characterized in that: Strontium carbonate powder in the said step (1): zero(ppm) water: the weight ratio of hydrochloric acid is 1: 3: 3.
3. the preparation method of spectroscopically pure strontium chloride according to claim 1 is characterized in that: Strontium carbonate powder is an analytical pure in the said step (1).
4. the preparation method of spectroscopically pure strontium chloride according to claim 1 is characterized in that: the specific density 1.18 of hydrochloric acid in the said step (1), the hydrochloric acid massfraction is 31%.
5. the preparation method of spectroscopically pure strontium chloride according to claim 1 is characterized in that: the container in the said step (1) is a stainless steel cask; Use B to filter during filtration; Under constantly stirring, slowly add when adding hydrochloric acid.
6. the preparation method of spectroscopically pure strontium chloride according to claim 1 is characterized in that: the thickening temperature in the said step (2) is 230-250 ℃; Crystallization uses drier to dry.
7. the preparation method of spectroscopically pure strontium chloride according to claim 1 is characterized in that: the weight fraction of said dilute sulphuric acid is 6-8%, the mark 28-30% of ydrogen peroxide 50.
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| CN201110254314.0A CN102417199B (en) | 2011-08-31 | 2011-08-31 | A kind of preparation method of spectroscopically pure strontium chloride |
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| CN201110254314.0A CN102417199B (en) | 2011-08-31 | 2011-08-31 | A kind of preparation method of spectroscopically pure strontium chloride |
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| CN102417199A true CN102417199A (en) | 2012-04-18 |
| CN102417199B CN102417199B (en) | 2015-12-02 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058444A (en) * | 2014-06-17 | 2014-09-24 | 民乐富源化工有限责任公司 | Method for preparing strontium chloride by using strontium slag |
| CN106409373A (en) * | 2016-10-31 | 2017-02-15 | 中国核动力研究设计院 | <89>SrCl2 solution production device |
| CN106745150A (en) * | 2017-03-06 | 2017-05-31 | 中国科学院青海盐湖研究所 | The preparation method of toothpaste strontium chloride |
| CN109011670A (en) * | 2018-09-13 | 2018-12-18 | 中国核动力研究设计院 | It is a kind of89SrCl2The enrichment facility and its method for concentration of solution |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102092759A (en) * | 2009-12-09 | 2011-06-15 | 贵州红星发展股份有限公司 | Method for preparing strontium dichloride hexahydrate |
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2011
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102092759A (en) * | 2009-12-09 | 2011-06-15 | 贵州红星发展股份有限公司 | Method for preparing strontium dichloride hexahydrate |
Non-Patent Citations (1)
| Title |
|---|
| 李坤: "化学－溶剂萃取联合法制备高纯碳酸锶", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058444A (en) * | 2014-06-17 | 2014-09-24 | 民乐富源化工有限责任公司 | Method for preparing strontium chloride by using strontium slag |
| CN106409373A (en) * | 2016-10-31 | 2017-02-15 | 中国核动力研究设计院 | <89>SrCl2 solution production device |
| CN106409373B (en) * | 2016-10-31 | 2017-09-29 | 中国核动力研究设计院 | A kind of 89SrCl2 solution process units |
| CN106745150A (en) * | 2017-03-06 | 2017-05-31 | 中国科学院青海盐湖研究所 | The preparation method of toothpaste strontium chloride |
| CN106745150B (en) * | 2017-03-06 | 2018-12-25 | 中国科学院青海盐湖研究所 | The preparation method of toothpaste strontium chloride |
| CN109011670A (en) * | 2018-09-13 | 2018-12-18 | 中国核动力研究设计院 | It is a kind of89SrCl2The enrichment facility and its method for concentration of solution |
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| CN102417199B (en) | 2015-12-02 |
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Address after: 300240 Tianjin Admiralty street Dongli District Xu Zhuangzi Patentee after: TIANJIN CHEMICAL REAGENT RESEARCH INSTITUTE CO., LTD. Address before: 300240 Tianjin Admiralty street Dongli District Xu Zhuangzi Patentee before: Tianjin chemical research institute |
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