CN102718245B - One-step production of barium hydroxide and sodium sulfide by using barium sulfide and sodium hydroxide - Google Patents
One-step production of barium hydroxide and sodium sulfide by using barium sulfide and sodium hydroxide Download PDFInfo
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- CN102718245B CN102718245B CN201110248303.1A CN201110248303A CN102718245B CN 102718245 B CN102718245 B CN 102718245B CN 201110248303 A CN201110248303 A CN 201110248303A CN 102718245 B CN102718245 B CN 102718245B
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Abstract
The invention provides a one-step production of barium hydroxide and sodium sulfide by using barium sulfide and sodium hydroxide, that is, industrial barium sulfide is utilized to directly react with an alkaline liquor to produce a barium hydroxide product and a byproduct sodium sulfide. The method comprises the following steps: leaching barium sulfide raw materials, carrying out slag removal on the leachate, then heating and preserving heat, determining the amount of barium ions, adding an alkali lye with the amount of caustic soda being 1-3 times of the amount of the barium ions, and separating the obtained product to obtain barium hydroxide and sodium sulfide. According to the invention, the final product can be obtained by only one step; compared with traditional process routes, the process provided by the invention is more economic, saves equipment cost and production time, omits the step of using hydrochloric acid to process barium sulfide in traditional processes, discharges without harmful gas hydrogen sulfide, is environmentally friendly, fully utilizes raw materials, and realizes atom economy.
Description
Technical field
The oxyhydroxide that the present invention relates to barium is produced, and particularly one utilizes barium sulphide and alkali lye to react, and a step generates the method for hydrated barta.
Background technology
Hydrated barta is important industrial chemicals.At present, the method for generation hydrated barta mainly contains barium sulphide method and heavy arsenic bloom method.
The record that the 5th edition " Chemicals handbook--Inorganic Chemicals fascicle " publishing for 2008 according to Chemical Industry Press is 55 pages: barium sulphide method will be by barite roasting, the barium sulphide that leaching obtains, strength of solution is controlled at 14～16 ° of Be, leave standstill clarification, clear liquid and hydrochloric acid reaction, the barium chloride solution of generation is heated to 70～90 ℃ and carries out replacement(metathesis)reaction with excessive caustic soda in 100～110 ℃; Through concentrated, crystallisation by cooling, centrifugation, dry, obtain barium hydroxide finished product.The method need to be by adding hydrochloric acid, adding caustic soda two steps processing just can obtain finished product, and operational path is long, consumes hydrochloric acid, is unfavorable for the recycling of sulphur.In addition, in the time adopting the method to produce, need to spend cost obnoxious flavour hydrogenchloride is dealt carefully with, otherwise pollute the environment.
Witherite method is after ore grinding, to carry out calcination, through leaching. filter, purify; Crystallization, dehydration.The dry product that obtains.This method is owing to being subject in heavy arsenic bloom the impurity effects such as calcium, aluminium, iron larger, and the product purity obtaining is influenced.And in recent years, heavy arsenic bloom resource exhaustion, the method scope of application is limited.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, a kind of technique of producing hydrated barta is provided.Utilize barium sulphide and alkali lye direct reaction, produce qualified hydrated barta product.Barium sulphide in described raw material, can be to adopt reductive agent to react the product of gained with barite, can be industrial barium sulphide grey black.Described alkali lye is caustic soda soln.
Particularly, a kind of method of utilizing barium sulphide and sodium hydroxide one step to produce hydrated barta and sodium sulphite, comprises following methods and step:
1), molten soaking: adopt the hot water of 70 ~ 100 ℃ as leaching liquid, raw material barium sulphide is leached to obtain barium sulphide leach liquor;
2), pre-treatment: by step 1) in the barium sulphide leach liquor of gained remove waste residue, heating and thermal insulation to 70 ~ 100 ℃, obtain barium sulfide solution;
3), measure: measure through step 2) amount of substance of barium ion in pretreated barium sulphide;
4), add alkali reaction: in the barium sulfide solution after step 3) is measured, add caustic soda, 1～3 times of the amount of substance that the amount of substance of the hydroxide ion in described caustic soda is the barium ion measured in step 3);
5), separate: after the reaction of step 4) completes, solution is joined to whizzer, be down to after 70 ℃ until temperature, centrifugation is to obtain hydrated barta.
" raw material barium sulphide " used in this specification sheets is to adopt reductive agent to react prepared with barite.As the product of the Containing Sulfur barium 65% obtaining after 59th～60 pages of employing coals of being recorded of version " Chemicals handbook--Inorganic Chemicals fascicle " in 2008 and barite roasting, i.e. industrial barium sulphide grey black.
" single stage method " provided by the present invention, directly adopts alkali lye to react with barium sulphide and produces hydrated barta product, and " two step method " of first reacting with barium sulphide, reacting with caustic soda with hydrochloric acid compared with traditional technology is more economical.Both save raw material hydrochloric acid, shortened again operational path.Meanwhile, present method is without noxious gas emission, environmentally safe.
Because impurity in industrial barium sulphide grey black is more, and barium sulphide solubleness is less, therefore, in described step 1), raw material barium sulphide is leached repeatedly, until in residue the content of barium sulphide lower than 1%.
For enhancing productivity and saving water of productive use, in described leaching process repeatedly, the barium sulphide leach liquor for concentration lower than 20 ° of Be, cyclically joins in raw material raw material is leached.
Heating makes barium sulfide solution concentration higher than 30 ° of Be.To guarantee that in the reaction process of step 4), barium sulfide solution has higher concentration, efficiency is higher.
Step 4) in, temperature of reaction is lower than 115 ℃, to prevent that reaction solution from splashing.
The method according to this invention, for arriving technique effect, in described step 4), the sodium hydroxide solution that the alkali lye adding is.Especially can adopt content is 15～30% caustic soda soln.Apply this technical scheme, can obtain byproduct sodium sulfide.
For making full use of raw material, realize atom economy.Step 5) in, from isolating hydrated barta, by solution evaporation crystallization, obtain sodium sulphite.With respect to traditional " barium sulphide method ", not only save hydrochloric acid, be more preferably the sodium-chlor that the value of the byproduct that adopts this technical scheme to obtain--sodium sulphite obtains usually above " barium sulphide method ".
Accompanying drawing explanation
The indefiniteness embodiment that the present invention can provide by accompanying drawing further illustrates.
Fig. 1 is process route chart of the present invention;
Fig. 2 is barium sulphide solubility curve figure;
Fig. 3 is barium hydroxide octahydrate solubility curve figure.
Embodiment
Three specific embodiments of the present invention are provided below, and the present invention is described in further detail, only limits to following embodiment but should not be construed the above-mentioned subject area of the present invention.Without departing from the idea case in the present invention described above, according to ordinary skill knowledge and customary means, make various replacements and change, all should be included in the scope of the present invention.
embodiment 1:
The industrial barium sulphide grey black that is 65% by 2kg barium sulphide content packs the container soaking for molten into, adds 3.5L hot water to this container, and the temperature of described hot water is more than 95 ℃.Molten soaking in process, can heat container, to guarantee water temperature.
In above-mentioned steps, on the one hand, the leaching of raw material is carried out repeatedly, until in raw material residue the content of barium sulphide lower than 1%.On the other hand, need, lower than the leach liquor of 20 ° of Be, cyclically join in described container, as leaching liquid, raw material be carried out to molten soaking for concentration.
After molten having soaked, by leach liquor slagging-off, join in groove, leave standstill, insulation, to 95 ℃, is concentrated to 30 ° more than Be.
The leach liquor leaving standstill after insulation is joined in reactive tank, measure barium ion wherein amount of substance, add the alkali lye of hydroxyl-containing ion for 25 times of measured barium ions.In the present embodiment, slowly adding 2.05kg concentration is 30% sodium hydroxide solution, fully reacts.In reaction process, temperature of reactor is controlled at 105 ℃.
After the sufficient reacting in above-mentioned steps carries out, product is carried out to Crystallization Separation.Be cooled to 60 degrees Celsius, by centrifugal and dry after, to obtain content be 99.1% barium hydroxide octahydrate 2.31kg.Described barium hydroxide octahydrate meets check and the quality standard thereof of HG/T2566-2006.
Isolated sodium sulfide solution is concentrated, obtain content and be 60% sodium sulphite 0.92kg.Described sodium sulphite meets check and the quality standard thereof of GB10500-2009.
embodiment 2:
The industrial barium sulphide grey black that is 55% by 2kg barium sulphide content packs the container soaking for molten into, adds 3.5L hot water to this container, and the temperature of described hot water is more than 70 ℃.Molten soaking in process, can heat container, to guarantee water temperature.
In above-mentioned steps, on the one hand, the leaching of raw material is carried out repeatedly, until in raw material residue the content of barium sulphide lower than 1%.On the other hand, need, lower than the leach liquor of 20 ° of Be, cyclically join in described container, as leaching liquid, raw material be carried out to molten soaking for concentration.
After molten having soaked, by leach liquor slagging-off, join in groove, leave standstill, insulation, to 80 ℃, is concentrated to 30 ° more than Be.
The leach liquor leaving standstill after insulation is joined in reactive tank, measure barium ion wherein amount of substance, add the alkali lye of hydroxyl-containing ion for 1～3 times of measured barium ion.In the present embodiment, slowly adding 1.75kg concentration is 30% sodium hydroxide solution, fully reacts.In reaction process, temperature of reactor is controlled at 115 ℃.
After the sufficient reacting in above-mentioned steps carries out, product is carried out to Crystallization Separation.Be cooled to 70 degrees Celsius, by centrifugal and dry after, to obtain content be 99% barium hydroxide octahydrate 1.9kg.Described barium hydroxide octahydrate meets check and the quality standard thereof of HG/T2566-2006.
Isolated sodium sulfide solution is concentrated, obtain content and be 60% sodium sulphite 0.77kg.Described sodium sulphite meets check and the quality standard thereof of GB10500-2009.
embodiment 3:
The industrial barium sulphide grey black that is 60% by 2kg barium sulphide content packs the container soaking for molten into, adds 3.5L hot water to this container, and the temperature of described hot water is more than 90 ℃.Molten soaking in process, can heat container, to guarantee water temperature.
In above-mentioned steps, on the one hand, the leaching of raw material is carried out repeatedly, until in raw material residue the content of barium sulphide lower than 1%.On the other hand, need, lower than the leach liquor of 20 ° of Be, cyclically join in described container, as leaching liquid, raw material be carried out to molten soaking for concentration.
After molten having soaked, by leach liquor slagging-off, join in groove, leave standstill, insulation, to 90 ℃, is concentrated to 30 ° more than Be.
The leach liquor leaving standstill after insulation is joined in reactive tank, measure barium ion wherein amount of substance, add the alkali lye of hydroxyl-containing ion for 2～3 times of measured barium ions.In the present embodiment, slowly adding 1.9kg concentration is 30% sodium hydroxide solution, fully reacts.In reaction process, temperature of reactor is controlled at 110 ℃.
After the sufficient reacting in above-mentioned steps carries out, product is carried out to Crystallization Separation.Be cooled to room temperature, by centrifugal and dry after, to obtain content be 99% barium hydroxide octahydrate 2.12kg.Described barium hydroxide octahydrate meets check and the quality standard thereof of HG/T2566-2006.
Isolated sodium sulfide solution is concentrated, obtain content and be 60% sodium sulphite 0.84kg.Described sodium sulphite meets check and the quality standard thereof of GB10500-2009.
Claims (5)
1. a method of utilizing barium sulphide and sodium hydroxide one step to produce hydrated barta and sodium sulphite, is characterized in that, comprises following methods and step:
1), molten soaking: adopt the hot water of 70 ~ 100 ℃ as leaching liquid, primary industry barium sulphide grey black is leached to obtain barium sulphide leach liquor;
2), pre-treatment: by step 1) in the leach liquor of barium sulphide of gained remove waste residue, heating and thermal insulation to 70 ~ 100 ℃, obtain barium sulfide solution;
3), measure: measure through step 2) amount of substance of barium ion in the barium sulfide solution that obtains of pre-treatment;
4), add alkali reaction: in the barium sulfide solution after step 3) is measured, add caustic soda, 1～3 times of the amount of substance that the amount of substance of the hydroxide ion in described caustic soda is the barium ion measured in step 3); Temperature of reaction is lower than 115 ℃;
5), separate: after the reaction of step 4) completes, solution is joined to whizzer, be down to after 70 ℃ until temperature, centrifugation is to obtain hydrated barta; By to isolating the solution evaporation crystallization after hydrated barta, obtain sodium sulphite.
2. a kind of method of utilizing barium sulphide and sodium hydroxide one step to produce hydrated barta and sodium sulphite according to claim 1, it is characterized in that: in described step 1), primary industry barium sulphide grey black is leached repeatedly, until in residue the content of barium sulphide lower than 1%.
3. a kind of method of utilizing barium sulphide and sodium hydroxide one step to produce hydrated barta and sodium sulphite according to claim 2, it is characterized in that: in described leaching process repeatedly, barium sulphide leach liquor for concentration lower than 20 ° of Be, circulation joins in raw material raw material is leached.
4. a kind of method of utilizing barium sulphide and sodium hydroxide one step to produce hydrated barta and sodium sulphite according to claim 1, is characterized in that: in described step 2) in, heating makes barium sulfide solution concentration higher than 30 ° of Be.
5. a kind of method of utilizing barium sulphide and sodium hydroxide one step to produce hydrated barta and sodium sulphite according to claim 1, is characterized in that: in described step 4), the caustic soda adding is that concentration is 30% sodium hydroxide solution.
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| CN201110248303.1A CN102718245B (en) | 2011-08-26 | 2011-08-26 | One-step production of barium hydroxide and sodium sulfide by using barium sulfide and sodium hydroxide |
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| CN201110248303.1A CN102718245B (en) | 2011-08-26 | 2011-08-26 | One-step production of barium hydroxide and sodium sulfide by using barium sulfide and sodium hydroxide |
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| CN104326499B (en) * | 2014-10-13 | 2016-04-27 | 南风化工集团股份有限公司 | By the method for three molten leaching grey black raising sodium sulfide solution concentration |
| CN110153156B (en) * | 2019-04-10 | 2021-09-28 | 东莞市珠江海咸水淡化研究所有限公司 | Non-toxic and recycling treatment process for barium slag |
| CN114380707A (en) * | 2022-01-20 | 2022-04-22 | 南京科瑞健医药科技有限公司 | Preparation method of trans-tranexamic acid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3966894A (en) * | 1973-09-25 | 1976-06-29 | Produits Chimiques Ugine Kuhlmann | Method of preparing barium hydroxide |
| CN86104945A (en) * | 1986-07-31 | 1988-02-10 | 张新球 | Produce the method for oxyhydroxide, thiosulphate, vitriol, sulphur |
| CN1962451A (en) * | 2006-12-11 | 2007-05-16 | 李守德 | Preparation method of barium hydroxide |
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- 2011-08-26 CN CN201110248303.1A patent/CN102718245B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3966894A (en) * | 1973-09-25 | 1976-06-29 | Produits Chimiques Ugine Kuhlmann | Method of preparing barium hydroxide |
| CN86104945A (en) * | 1986-07-31 | 1988-02-10 | 张新球 | Produce the method for oxyhydroxide, thiosulphate, vitriol, sulphur |
| CN1962451A (en) * | 2006-12-11 | 2007-05-16 | 李守德 | Preparation method of barium hydroxide |
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