CN101759219A - Preparing method of Sr(0H)2.8H2O - Google Patents
Preparing method of Sr(0H)2.8H2O Download PDFInfo
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- CN101759219A CN101759219A CN200910159961A CN200910159961A CN101759219A CN 101759219 A CN101759219 A CN 101759219A CN 200910159961 A CN200910159961 A CN 200910159961A CN 200910159961 A CN200910159961 A CN 200910159961A CN 101759219 A CN101759219 A CN 101759219A
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- strontium hydroxide
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Abstract
The present invention relates to a preparing method of strontium hydroxide. In the method, quantitative manganese oxide powdered ore is added into Sr(HS)2 solution of which the concentration is 0.20 to 0.55 mol/L, and the reaction temperature is maintained within 60 DEG C to 85 DEG C ; the mixture is stirred closely for 1.5 to 3 hours to be separated in a solid-liquid way; filtered liquid is cooled closely to 25 DEG C to 35 DEG C, and is separated in the solid-liquid way to obtain crude Sr(0H)2.8H2O; the obtained solid is dissolved by de-ionized water according to concentration of 0.5 to 0.8 mol/L [Sr2+]; 27.5% of H2O2 is added according to the proportion of 2 to 5mol/L to be heated and boiled for 15 to 30 minutes, and the solution is filtered and separated; the obtained filtered liquid is closely cooled and crystallized to 35 DEG C to 45 DEG C, and is separated in a centrifugal way; and solid is dried to obtain the final product of Sr(0H)2.8H2O. The Sr(HS)2 solution generated by hydrolyzing SrS is extracted twice, which can obtain strontium hydroxide with low cost.
Description
Technical field
The present invention relates to a kind of Sr (OH)
28H
2The preparation method of O particularly utilizes Sr (HS)
2Prepare Sr (OH)
28H
2The method of O.
Background technology
Along with the development of liquid-crystal display and sensitive ceramic, to high-quality SrCO
3Need also increases Sr (OH) thereupon
2Operational path carbonization synthetic SrCO
3Can satisfy the physical and chemical quality requirement of above-mentioned industry, the Sr (OH) of traditional hydrochloric acid-liquid caustic soda route and pyrolytic decomposition extract technology path of preparing
2Because cost factor has not had competitive capacity.
Mainly contain manganese and iron in the Manganse Dioxide breeze, the content of other metal is with respect to very low can the ignoring of content of manganese in suitability for industrialized production.
The applicant has been to have disclosed first extraction Sr (OH) in 200910158214.0 at the number of patent application in first to file
28H
2The method of O quotes in full to do reference herein.In first to file, disclose from SrS solution through cooling off the method for direct separation of hydrogen strontium oxide at this.The Sr (OH) that it utilizes the SrS hydrolysis to produce
2With Sr (HS)
2Solution obtains Sr (OH) through refrigerated separation
28H
2The O crude product obtains Sr (OH) through the removal of impurities recrystallization again
28H
2The O product is able to low-cost industrial production Sr (OH)
28H
2The O product, the Sr (OH) that utilizes mother liquor or crystallization to go out then
28H
2O is water-soluble to carry out carbonization and obtains SrCO
3Product.The main chemical reactions formula that should relate in first to file is: 2SrS+2H
2O → Sr (OH)
2+ Sr (HS)
2So, once extracted Sr (OH)
2After, be left Sr (HS)
2Solution.
Summary of the invention
A Sr (OH) has been extracted in utilization of the present invention
2The Sr (HS) that the back is remaining
2Solution and manganese oxide react, and further obtain Sr (OH)
28H
2The O product, thus Sr (OH) greatly reduced
28H
2The preparation cost of O.
The objective of the invention is with manganese oxide and Sr (HS)
2Thereby carry out the low-cost preparation of redox reaction Sr (OH)
28H
2The O product.
The chemical equation Sr (HS) that the present invention relates generally to
2+ MnO
2→ Sr (OH)
2+ SrS
x+ MnO, its technical process as shown in Figure 1.
Concrete technical scheme of the present invention is:
With Sr (HS)
2Strength of solution is adjusted to 0.20~0.55mol/L, is preferably 0.40~0.55mol/L;
With above-mentioned Sr (HS)
2Solution and manganese oxide powder are pressed manganese: sulphur=1: 1~1.1, and iron: react sulphur=1: 1.5~1.65, keeps temperature of reaction 60~85 ℃ of scopes, airtight stirring 1.5~3 hours, solid-liquid separation, filter residue reclaims preparation MnSO
4Product, filtrate is airtight to be cooled to 25~35 ℃, is preferably 30~35 ℃, carries out solid-liquid separation then, gets thick Sr (OH)
28H
2O;
With the thick Sr of gained (OH)
28H
2O is according to 0.5~0.8mo l/L[Sr
2+] use deionized water dissolving, add 27.5 weight %H according to the ratio of 2~5ml/L
2O
2Sulphur removal, heated and boiled was also kept 15~30 minutes, filtering separation, filter residue is abandoned, the airtight crystallisation by cooling to 35 of filtrate~45 ℃ carries out centrifugation after being preferably 40~45 ℃, the oven dry solid, the finished product Sr (OH)
28H
2O.
Description of drawings
Fig. 1 is a main technique schema of the present invention.
Embodiment
Embodiment 1
Sr (HS) with 0.47mol/L
2Solution 4000ml places the 5000ml beaker, stirs to add 752g manganese oxide powder (MnO down
225.1%, Fe 7.8%), electric furnace heating also maintains 70 ℃, airtight stirring 2 hours stops to stir, and draws upper clear supernate with emulsion tube after the sedimentation, add the reaction of 1000ml hot deionized water and agitator treating after, suction strainer separates, filter residue prepares MnSO
4Product, merging filtrate airtightly is cooled to 35 ℃.
Solution suction strainer after the above-mentioned cooling is separated, and SrCO is reclaimed in the filtrate carbonization
3, thick Sr (OH)
28H
2O presses 0.8mol/L[Sr
2+] add the deionized water heating for dissolving, add 27.5%H in the 3ml/L ratio
2O
2Boiling 15 minutes is also kept in sulphur removal, heated and boiled, and with qualitative filter paper filtration at a slow speed, filter residue is abandoned, and filtrate is airtight to be cooled to 40 ℃.
Solution centrifugal after the above-mentioned cooling is separated, and Recycling Mother Solution is used, and crystallization obtains Sr (OH)
28H
2O places 65 ℃ of convection oven oven dry to obtain Sr (OH) in 6 hours
28H
2O sample 1
#
With 0.55mol/L Sr (HS)
2Solution 4000ml places the 5000ml beaker, stirs to add 628g manganese oxide powder (MnO down
238.7%, Fe 8.6%), the electric furnace heating also maintains 80 ℃ of temperature, and confined reaction 2 hours stops to stir, and siphon supernatant liquor after the sedimentation is added dilution of 1000ml hot deionized water and washery slag, and suction strainer separates, and filter residue prepares MnSO
4, merging filtrate is airtight to be cooled to 30 ℃.
Solution suction strainer after the above-mentioned cooling is separated, and SrCO is reclaimed in the filtrate carbonization
3, thick Sr (OH)
28H
2O presses 0.7mo l/L[Sr
2+] with the hot deionized water dissolving, add 3ml/L 27.5%H
2O
2Sulphur removal, heated and boiled, and kept 25 minutes, with qualitative filter paper filtration at a slow speed, filter residue is abandoned, and filtrate is airtight to be cooled to 45 ℃.
Solution centrifugal after the above-mentioned cooling is separated, and Recycling Mother Solution is used, Sr (OH)
28H
2O places 65 ℃ of convection oven oven dry to obtain Sr (OH) in 6 hours
28H
2O sample 2
#
Embodiment 3
With 0.40mol/L Sr (HS)
2Solution 4000ml places the 5000ml beaker, stirs to add 474g manganese oxide powder (MnO down
238.7%, Fe 8.6%), the electric furnace heating also maintains 85 ℃ of temperature, and confined reaction 2 hours stops to stir, and siphon supernatant liquor after the sedimentation is added dilution of 1000ml hot deionized water and washery slag, and suction strainer separates, and filter residue prepares MnSO
4, merging filtrate is airtight to be cooled to 32 ℃.
Solution suction strainer after the above-mentioned cooling is separated, and SrCO is reclaimed in the filtrate carbonization
3, thick Sr (OH)
28H
2O presses 0.7mol/L[Sr
2+] with the hot deionized water dissolving, add 3ml/L 27.5%H
2O
2Sulphur removal, heated and boiled, and kept 25 minutes, with qualitative filter paper filtration at a slow speed, filter residue is abandoned, and filtrate is airtight to be cooled to 43 ℃.
Solution centrifugal after the above-mentioned cooling is separated, and Recycling Mother Solution is used, Sr (OH)
28H
2O places 65 ℃ of convection oven oven dry to obtain Sr (OH) in 6 hours
28H
2O sample 3
#
Embodiment 4
With 0.20mol/L Sr (HS)
2Solution 4000ml places the 5000ml beaker, stirs to add 237g manganese oxide powder (MnO down
238.7%, Fe 8.6%), the electric furnace heating also maintains 60 ℃ of temperature, and confined reaction 2 hours stops to stir, and siphon supernatant liquor after the sedimentation is added dilution of 1000ml hot deionized water and washery slag, and suction strainer separates, and filter residue prepares MnSO
4, merging filtrate is airtight to be cooled to 25 ℃.
Solution suction strainer after the above-mentioned cooling is separated, and SrCO is reclaimed in the filtrate carbonization
3, thick Sr (OH)
28H
2O presses 0.7mo l/L[Sr
2+] with the hot deionized water dissolving, add 3ml/L 27.5%H
2O
2Sulphur removal, heated and boiled, and kept 30 minutes, with qualitative filter paper filtration at a slow speed, filter residue is abandoned, and filtrate is airtight to be cooled to 35 ℃.
Solution centrifugal after the above-mentioned cooling is separated, and Recycling Mother Solution is used, Sr (OH)
28H
2O places 65 ℃ of convection oven oven dry to obtain Sr (OH) in 6 hours
28H
2O sample 4
#
More than each embodiment gained sample Sr (OH)
28H
2O content and foreign matter content data such as following table:
Content | ??1 # | ??2 # | ??3 # | ??4 # |
??Sr(OH) 2·8H 2O (weight %) | ??97.21 | ??99.18 | ??99.05 | ??98.78 |
??K | ??<20ppm | ??<20ppm | ??<20ppm | ??<20ppm |
??Na | ??<10ppm | ??<10ppm | ??<10ppm | ??<10ppm |
??Ca | ??<100pp | ??<100ppm | ??<100ppm | ??<100ppm |
??Mg | ??<10ppm | ??<10ppm | ??<10ppm | ??<10ppm |
??Fe | ??<10ppm | ??<10ppm | ??<10ppm | ??<10ppm |
Claims (5)
1. the preparation method of a strontium hydroxide, it comprises step:
A is with Sr (HS)
2The concentration of solution is adjusted to 0.20~0.55mol/L;
B is with above-mentioned Sr (HS)
2Solution adds manganese oxide powder and presses manganese: sulphur=1: 1~1.1, and iron: react sulphur=1: 1.5~1.65, keeps temperature of reaction 60~85 ℃ of scopes, airtight stirring 1.5~3 hours, solid-liquid separation gets filtrate;
C is cooled to 25~35 ℃ with above-mentioned gained filtrate is airtight, carries out solid-liquid separation then, thick Sr (OH)
28H
2O;
D is with the thick Sr of gained (OH)
28H
2O is by 0.5~0.8mol/L[Sr
2+] use deionized water dissolving, add 27.5 weight %H according to the ratio of 2~5ml/L
2O
2, heated and boiled was also kept 15~30 minutes, and filtering separation gets filtrate;
E carries out centrifugation with behind the airtight crystallisation by cooling to 35 of gained filtrate~45 ℃, the oven dry solid, the finished product Sr (OH)
28H
2O.
2. the preparation method of strontium hydroxide as claimed in claim 1, wherein Sr (HS) in the steps A
2The concentration of solution is adjusted to 0.40~0.55mol/L.
3. the preparation method of strontium hydroxide as claimed in claim 1 or 2, wherein keeping temperature of reaction among the step C is 30~35 ℃.
4. the preparation method of strontium hydroxide as claimed in claim 1 or 2 wherein carries out centrifugation behind the gained filtrate crystallisation by cooling to 40 in the step e~45 ℃.
5. the preparation method of strontium hydroxide as claimed in claim 3 wherein carries out centrifugation behind the gained filtrate crystallisation by cooling to 40 in the step e~45 ℃.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102765739A (en) * | 2012-08-13 | 2012-11-07 | 贵州红星发展股份有限公司 | High-purity strontium oxide and preparation method thereof |
CN102765740A (en) * | 2012-06-19 | 2012-11-07 | 南京金焰锶业有限公司 | Preparation method of strontium carbonate with high purity |
CN105293554A (en) * | 2015-11-10 | 2016-02-03 | 青海民族大学 | Method for preparing high-purity strontium dihydroxide by utilizing strontium slag |
-
2009
- 2009-07-27 CN CN200910159961A patent/CN101759219A/en active Pending
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102765740A (en) * | 2012-06-19 | 2012-11-07 | 南京金焰锶业有限公司 | Preparation method of strontium carbonate with high purity |
CN102765740B (en) * | 2012-06-19 | 2014-03-05 | 南京金焰锶业有限公司 | Preparation method of strontium carbonate with high purity |
CN102765739A (en) * | 2012-08-13 | 2012-11-07 | 贵州红星发展股份有限公司 | High-purity strontium oxide and preparation method thereof |
CN102765739B (en) * | 2012-08-13 | 2014-10-29 | 贵州红星发展股份有限公司 | High-purity strontium oxide and preparation method thereof |
CN105293554A (en) * | 2015-11-10 | 2016-02-03 | 青海民族大学 | Method for preparing high-purity strontium dihydroxide by utilizing strontium slag |
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Application publication date: 20100630 |