CN112678782A - Continuous leaching process for barium sulfide - Google Patents
Continuous leaching process for barium sulfide Download PDFInfo
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- CN112678782A CN112678782A CN202011609035.7A CN202011609035A CN112678782A CN 112678782 A CN112678782 A CN 112678782A CN 202011609035 A CN202011609035 A CN 202011609035A CN 112678782 A CN112678782 A CN 112678782A
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- CN
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- Prior art keywords
- barium sulfide
- pulping
- hot water
- barium
- leaching process
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- CJDPJFRMHVXWPT-UHFFFAOYSA-N barium sulfide Chemical compound [S-2].[Ba+2] CJDPJFRMHVXWPT-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 238000002386 leaching Methods 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 56
- 238000004537 pulping Methods 0.000 claims abstract description 55
- 239000007788 liquid Substances 0.000 claims abstract description 37
- 239000000706 filtrate Substances 0.000 claims abstract description 34
- 241000565357 Fraxinus nigra Species 0.000 claims abstract description 31
- 238000000498 ball milling Methods 0.000 claims abstract description 28
- 239000002002 slurry Substances 0.000 claims abstract description 22
- 238000003825 pressing Methods 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 238000005086 pumping Methods 0.000 claims abstract description 7
- 238000010009 beating Methods 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 9
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims description 7
- 229910001626 barium chloride Inorganic materials 0.000 claims description 7
- 230000020477 pH reduction Effects 0.000 claims description 6
- 238000004064 recycling Methods 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 3
- 238000010924 continuous production Methods 0.000 abstract description 7
- 238000000605 extraction Methods 0.000 abstract description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 8
- 230000001376 precipitating effect Effects 0.000 description 7
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 6
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 4
- 229910001863 barium hydroxide Inorganic materials 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- 239000001569 carbon dioxide Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 3
- RHZUVFJBSILHOK-UHFFFAOYSA-N anthracen-1-ylmethanolate Chemical compound C1=CC=C2C=C3C(C[O-])=CC=CC3=CC2=C1 RHZUVFJBSILHOK-UHFFFAOYSA-N 0.000 description 3
- 239000003830 anthracite Substances 0.000 description 3
- 229910052601 baryte Inorganic materials 0.000 description 3
- 239000010428 baryte Substances 0.000 description 3
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 3
- -1 sulfur ions Chemical class 0.000 description 3
- 229920002101 Chitin Polymers 0.000 description 2
- 229920001661 Chitosan Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 229910001422 barium ion Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008236 heating water Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 230000019086 sulfide ion homeostasis Effects 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to a continuous leaching process of barium sulfide, black ash coming from a calcining kiln is ball-milled with hot water, slurry after ball-milling enters a pulping leaching barrel, the hot water is added for pulping, plate-frame filter pressing is carried out after pulping, and obtained filtrate I directly enters a barium sulfide liquid pool; and adding hot water into the obtained filter residue I, pulping again, performing filter pressing again after pulping, recovering the obtained filtrate II to perform ball milling, adding hot water into the filter residue II again, pulping again, and pumping the pulped pulp into a reaction post. The invention realizes continuous production and continuous extraction.
Description
Technical Field
The invention relates to the technical field of barium sulfide production, in particular to a barium sulfide leaching process.
Background
The existing barium sulfide manufacturing process comprises the following steps: after the barite is crushed and sieved to the granularity of less than or equal to 5mm, the barite is sent into a barite powder bin, and the anthracite is transported to the anthracite powder bin by a bucket elevator. The barite and anthracite powder are weighed and mixed according to a certain proportion and then fed into a rotary kiln for reduction roasting. The obtained crude barium sulfide black ash is transported to a leaching tank by a winch, hot water is added for repeated leaching, the leached high material (BaS concentration of 175g/L) is clarified and then is sent to a barium chloride workshop, the low material (BaS concentration of 135 g/L) is clarified and then is sent to a barium sulfate and barium carbonate workshop, and leaching residues are manually cleared and sent to a residue field for stacking. Namely, the massive black ash blocks are placed in a leaching tank for standing and soaking, and the standing is required to be carried out for more than 4-12h at the temperature of 80-95 ℃, so that the time is consumed, and the production efficiency is low.
Disclosure of Invention
In order to solve the technical problem, the barium sulfide leaching process is provided, and the carbon dioxide gas produced by the barium carbonate ore is fully recycled.
The technical scheme of the invention is as follows:
a continuous leaching process for barium sulfide, the process comprising the steps of:
s1: ball milling barium sulfide black ash and hot water from a calcining kiln, feeding the ball-milled slurry into a pulping and leaching barrel, adding hot water for primary pulping, and performing plate-frame filter pressing after the primary pulping to obtain filtrate I which directly enters a barium sulfide liquid pool;
s2: adding hot water into the filter residue I obtained in the step S1, pulping for the second time, performing filter pressing after the second pulping, recycling the obtained filtrate II to the ball mill in the step S1, repeating the operation of S1, adding hot water into the filter residue II again, performing third pulping, and pumping the slurry subjected to the third pulping to a barium chloride reaction post for secondary acidification;
and completing the continuous leaching of the barium sulfide.
Preferably, in the steps S1 and S2, the hot water temperature is 55-80 ℃.
Preferably, the particle size of the barium sulfide black ash in the step S1 is 0.075-0.198 mm.
Preferably, the solid-to-liquid ratio of the black ash to the hot water in the ball milling in the step S1 is 160-220 (g/L), the ball milling time is 45-90 minutes, and the particle size of the slurry after the ball milling is 0.065-0.085 mm.
Preferably, the solid-to-liquid ratio of the slurry to the hot water in the first beating of the step S1 is 150-170 (g/L), and the first beating time is 40-50 minutes.
Preferably, the solid-liquid ratio of the filter residue I to the hot water in the step S2 is 170-190 (g/L), and the second pulping time is 25-35 minutes.
Preferably, the filtrate I directly enters a barium sulfide liquid pool to obtain barium sulfide filtrate, and the barium sulfide filtrate is subjected to standing, filtering and subsequent process production.
Further preferably, standing for precipitation for 30-60min, and then filtering to obtain barium sulfide leachate.
The invention has the beneficial effects that:
1. the invention adopts the steps of ball milling, pulping and plate-and-frame filter pressing of the barium sulfide black ash from the calcining kiln and hot water to obtain barium sulfide liquid, heating water on filter residues, pulping and filter pressing again, recovering the obtained filtrate to the ball mill, repeatedly operating, continuously leaching, removing impurities and filtering to obtain barium sulfide leachate, thereby changing the prior barium sulfide standing leaching process, realizing continuous production, saving leaching time and improving leaching efficiency.
2. The temperature of beating hot water is 55-80 ℃, and is lower than the extraction temperature of standing extraction at 95-100 ℃, so that energy can be saved.
3. The particle size of the barium sulfide black ash is 0.075-0.198mm, the particle size of the barium sulfide black ash is smaller, the particle size of slurry after ball milling is reduced to 0.065-0.085mm, normally, the smaller the particle size of the barium sulfide black ash is, the better the contact chance of reaction materials is increased, the leaching speed is accelerated, but the too fine materials cause the porosity of the whole reaction materials to be small, the contact area with water is reduced, and the leaching is not facilitated. The leaching rate of the barium sulfide black ash reaches more than 90 percent, the final leaching concentration of the barium sulfide solution is 160-220g/L, and the time of the whole continuous process is within 1.5 hours.
4. In the working procedure of the invention, the barium sulfide filtrate obtained after the filtrate I directly enters the barium sulfide liquid pool is subjected to impurity removal and then is subjected to subsequent process production, and the obtained barium sulfide has high purity.
Detailed Description
The invention will be further illustrated by the following examples. The examples are intended to illustrate the invention only and do not limit the scope of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any methods and materials similar or equivalent to those described herein can be used in the practice of the present invention, and the preferred embodiments described herein are exemplary only.
Example 1
A continuous leaching process for barium sulfide, the process comprising the steps of:
s1: ball milling barium sulfide black ash and hot water from a calcining kiln, feeding the ball-milled slurry into a pulping and leaching barrel, adding hot water for primary pulping, and performing plate-frame filter pressing after the primary pulping to obtain filtrate I which directly enters a barium sulfide liquid pool;
s2: adding hot water into the filter residue I obtained in the step S1, pulping for the second time, performing filter pressing after the second pulping, recycling the obtained filtrate II to the ball mill in the step S1, repeating the operation of S1, adding hot water into the filter residue II again, performing third pulping, and pumping the slurry subjected to the third pulping to a barium chloride reaction post for secondary acidification;
and completing the continuous leaching of the barium sulfide.
Preferably, in the steps S1 and S2, the hot water temperature is 80 ℃.
Preferably, the particle size of the barium sulfide black ash in the step S1 is 0.198 mm.
Preferably, the solid-to-liquid ratio of the black ash to the hot water in the ball milling in step S1 is 220 (g/L), the ball milling time is 45 minutes, and the particle size of the slurry after ball milling is 0.085 mm.
Preferably, the solid-to-liquid ratio of the pulp to the hot water in the first beating of the step S1 is 170 (g/L), and the first beating time is 40 minutes.
Preferably, the solid-to-liquid ratio of the filter residue I to the hot water in the step S2 is 190 (g/L), and the second pulping time is 35 minutes.
Preferably, the filtrate I directly enters a barium sulfide liquid pool to obtain barium sulfide filtrate, and the barium sulfide filtrate is subjected to standing, filtering and subsequent process production.
Further preferably, standing and precipitating for 30min, and then filtering to obtain barium sulfide leaching liquid.
By adopting the embodiment, the leaching rate of the barium sulfide black ash reaches 93%, the leaching concentration of the final barium sulfide solution is 160 g/L, and the time of the whole continuous process is 46 min.
Example 2
A continuous leaching process for barium sulfide, the process comprising the steps of:
s1: ball milling barium sulfide black ash and hot water from a calcining kiln, feeding the ball-milled slurry into a pulping and leaching barrel, adding hot water for primary pulping, and performing plate-frame filter pressing after the primary pulping to obtain filtrate I which directly enters a barium sulfide liquid pool;
s2: adding hot water into the filter residue I obtained in the step S1, pulping for the second time, performing filter pressing after the second pulping, recycling the obtained filtrate II to the ball mill in the step S1, repeating the operation of S1, adding hot water into the filter residue II again, performing third pulping, and pumping the slurry subjected to the third pulping to a barium chloride reaction post for secondary acidification;
and completing the continuous leaching of the barium sulfide.
Preferably, in the steps S1 and S2, the hot water temperature is 55 ℃.
Preferably, the particle size of the barium sulfide black ash in the step S1 is 0.075 mm.
Preferably, the solid-to-liquid ratio of the black ash to the hot water in the ball milling in step S1 is 160 (g/L), the ball milling time is 90 minutes, and the particle size of the slurry after ball milling is 0.065 mm.
Preferably, the solid-to-liquid ratio of the pulp to the hot water in the first beating of the step S1 is 150 (g/L), and the first beating time is 50 minutes.
Preferably, the solid-to-liquid ratio of the filter residue I to the hot water in the step S2 is 170 (g/L), and the second beating time is 25 minutes.
Preferably, the filtrate I directly enters a barium sulfide liquid pool to obtain barium sulfide filtrate, and the barium sulfide filtrate is subjected to standing, filtering and subsequent process production.
Further preferably, standing and precipitating for 30min, and then filtering to obtain barium sulfide leaching liquid.
By adopting the embodiment, the leaching rate of the barium sulfide black ash reaches 94%, the leaching concentration of the final barium sulfide solution is 165 g/L, and the time of the whole continuous process is 55 min.
Example 3
A continuous leaching process for barium sulfide, the process comprising the steps of:
s1: ball milling barium sulfide black ash and hot water from a calcining kiln, feeding the ball-milled slurry into a pulping and leaching barrel, adding hot water for primary pulping, and performing plate-frame filter pressing after the primary pulping to obtain filtrate I which directly enters a barium sulfide liquid pool;
s2: adding hot water into the filter residue I obtained in the step S1, pulping for the second time, performing filter pressing after the second pulping, recycling the obtained filtrate II to the ball mill in the step S1, repeating the operation of S1, adding hot water into the filter residue II again, performing third pulping, and pumping the slurry subjected to the third pulping to a barium chloride reaction post for secondary acidification;
and completing the continuous leaching of the barium sulfide.
Preferably, in the steps S1 and S2, the hot water temperature is 60 ℃.
Preferably, the particle size of the barium sulfide black ash in the step S1 is 0.085 mm.
Preferably, the solid-to-liquid ratio of the black ash to the hot water in the ball milling in step S1 is 180 (g/L), the ball milling time is 65 minutes, and the particle size of the slurry after ball milling is 0.075 mm.
Preferably, the solid-to-liquid ratio of the pulp to the hot water in the first beating of the step S1 is 160 (g/L), and the first beating time is 45 minutes.
Preferably, the solid-to-liquid ratio of the filter residue I to the hot water in the step S2 is 180 (g/L), and the second beating time is 30 minutes.
Preferably, the filtrate I directly enters a barium sulfide liquid pool to obtain barium sulfide filtrate, and the barium sulfide filtrate is subjected to standing, filtering and subsequent process production.
Further preferably, standing and precipitating for 30min, and then filtering to obtain barium sulfide leaching liquid.
By adopting the embodiment, the leaching rate of the barium sulfide black ash reaches 93%, the leaching concentration of the final barium sulfide solution is 160 g/L, and the time of the whole continuous process is 50 min.
Example 4
A continuous leaching process for barium sulfide, the process comprising the steps of:
s1: ball milling barium sulfide black ash and hot water from a calcining kiln, feeding the ball-milled slurry into a pulping and leaching barrel, adding hot water for primary pulping, and performing plate-frame filter pressing after the primary pulping to obtain filtrate I which directly enters a barium sulfide liquid pool;
s2: adding hot water into the filter residue I obtained in the step S1, pulping for the second time, performing filter pressing after the second pulping, recycling the obtained filtrate II to the ball mill in the step S1, repeating the operation of S1, adding hot water into the filter residue II again, performing third pulping, and pumping the slurry subjected to the third pulping to a barium chloride reaction post for secondary acidification;
and completing the continuous leaching of the barium sulfide.
Preferably, in the steps S1 and S2, the hot water temperature is 60 ℃.
Preferably, the particle size of the barium sulfide black ash in the step S1 is 0.085 mm.
Preferably, the solid-to-liquid ratio of the black ash to the hot water in the ball milling in step S1 is 180 (g/L), the ball milling time is 65 minutes, and the particle size of the slurry after ball milling is 0.075 mm.
Preferably, the solid-to-liquid ratio of the pulp to the hot water in the first beating of the step S1 is 160 (g/L), and the first beating time is 45 minutes.
Preferably, the solid-to-liquid ratio of the filter residue I to the hot water in the step S2 is 180 (g/L), and the second beating time is 30 minutes.
Preferably, the filtrate I directly enters a barium sulfide liquid pool to obtain barium sulfide filtrate, and the barium sulfide filtrate is subjected to standing, filtering and subsequent process production.
Further preferably, standing and precipitating for 30min, and then filtering to obtain barium sulfide leaching liquid.
By adopting the embodiment, the leaching rate of the barium sulfide black ash reaches 93%, the leaching concentration of the final barium sulfide solution is 163 g/L, and the time of the whole continuous process is 53 min.
Example 5
On the basis of example 4, before standing, precipitating and separating, carbon dioxide gas is firstly introduced into the obtained barium sulfide solution for 10min, then the barium sulfide solution is subjected to standing, precipitating and separating for 30min, and then the barium sulfide leaching solution is obtained by filtering.
By adopting the embodiment, the leaching rate of the barium sulfide black ash reaches 97%, and the leaching concentration of the final barium sulfide leaching solution is 178 g/L. In the pulping and leaching process, barium sulfide is not hydrolyzed completely, because barium ions, sulfur ions, hydroxyl ions and hydrogen ions react to produce barium hydroxide and hydrogen sulfide in the pulping and leaching process, the generated ba (oh)2 still remains in the solution and is not precipitated, so that hydrolysis is inhibited from being completely performed, and the leaching concentration of barium sulfide is reduced.
Example 6
On the basis of the example 5, before standing, precipitating and separating, hydrogen sulfide gas is firstly introduced into the obtained barium sulfide solution for 10min, chitosan is added, the addition amount of the chitosan is 120mg/L, the mixture is stirred uniformly, barium hydroxide solution is added to adjust the pH value to 7, carbon dioxide gas is then introduced for 10min, and then the barium sulfide solution is stood, precipitated and separated for 18min to obtain barium sulfide leachate.
The settling process time is longer, by adopting the scheme of the embodiment, firstly, hydrogen sulfide gas is introduced to reduce the pH value of the solution to about 3, so that the deacetylated chitin is fully dissolved in the barium sulfide solution, after the barium hydroxide solution is added to adjust the pH value to 7, the deacetylated chitin begins to flocculate impurities in the solution, then, carbon dioxide gas is continuously introduced, the barium hydroxide is converted into barium carbonate for precipitation, the impurities in the solution are rapidly precipitated, and the settling time is shortened to 18 min.
The above-described embodiments are merely preferred embodiments of the present invention, and should not be construed as limiting the present invention, and features in the embodiments and examples in the present application may be arbitrarily combined with each other without conflict. The protection scope of the present invention is defined by the claims, and includes equivalents of technical features of the claims. I.e., equivalent alterations and modifications within the scope hereof, are also intended to be within the scope of the invention.
Claims (8)
1. A continuous leaching process for barium sulfide, said process comprising the steps of:
s1: ball milling barium sulfide black ash and hot water from a calcining kiln, feeding the ball-milled slurry into a pulping and leaching barrel, adding hot water for primary pulping, and performing plate-frame filter pressing after the primary pulping to obtain filtrate I which directly enters a barium sulfide liquid pool;
s2: adding hot water into the filter residue I obtained in the step S1, pulping for the second time, performing filter pressing after the second pulping, recycling the obtained filtrate II to the ball mill in the step S1, repeating the operation of S1, adding hot water into the filter residue II again, performing third pulping, and pumping the slurry subjected to the third pulping to a barium chloride reaction post for secondary acidification;
and completing the continuous leaching of the barium sulfide.
2. The continuous leaching process of barium sulfide according to claim 1, characterized in that: in the steps S1 and S2, the hot water temperature is 55-80 ℃.
3. The continuous leaching process of barium sulfide according to claim 1, characterized in that: and in the step S1, the particle size of the barium sulfide black ash is 0.075-0.198 mm.
4. The continuous leaching process of barium sulfide according to claim 1, characterized in that: the solid-liquid ratio of the black ash to the hot water in the ball milling in the step S1 is 160-220 (g/L), the ball milling time is 45-90 minutes, and the particle size of the slurry after the ball milling is 0.065-0.085 mm.
5. The continuous leaching process of barium sulfide according to claim 1, characterized in that: the solid-to-liquid ratio of the slurry and the hot water in the first beating of the step S1 is 150-170 (g/L), and the first beating time is 40-50 minutes.
6. The continuous leaching process of barium sulfide according to claim 1, characterized in that: the solid-liquid ratio of the filter residue I to the hot water in the step S2 is 170-190 (g/L), and the second pulping time is 25-35 minutes.
7. The continuous leaching process of barium sulfide according to claim 1, characterized in that: and (3) directly feeding the filtrate I into a barium sulfide liquid pool to obtain barium sulfide filtrate, standing, filtering and then carrying out the production of the subsequent process.
8. The continuous leaching process of barium sulfide according to claim 7, wherein: standing for precipitation for 30-60min, and filtering to obtain barium sulfide leaching solution.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110092357A (en) * | 2019-04-23 | 2019-08-06 | 贵州红星发展股份有限公司 | A kind of preparation method of high-purity barium sulphide |
| US20200295399A1 (en) * | 2019-03-13 | 2020-09-17 | Ningde Amperex Technology Limited | Solid electrolyte and preparation method thereof, and electrochemical device and electronic device comprising same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20200295399A1 (en) * | 2019-03-13 | 2020-09-17 | Ningde Amperex Technology Limited | Solid electrolyte and preparation method thereof, and electrochemical device and electronic device comprising same |
| CN110092357A (en) * | 2019-04-23 | 2019-08-06 | 贵州红星发展股份有限公司 | A kind of preparation method of high-purity barium sulphide |
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