CN108793218A - The preparation method of barium carbonate and the barium carbonate prepared by the preparation method - Google Patents
The preparation method of barium carbonate and the barium carbonate prepared by the preparation method Download PDFInfo
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- CN108793218A CN108793218A CN201810808754.8A CN201810808754A CN108793218A CN 108793218 A CN108793218 A CN 108793218A CN 201810808754 A CN201810808754 A CN 201810808754A CN 108793218 A CN108793218 A CN 108793218A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/186—Strontium or barium carbonate
- C01F11/188—Barium carbonate
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Abstract
The present invention provides a kind of preparation methods of barium carbonate, including：By yellow water natural subsidence, subsequent press filtration obtains pure yellow water；Desulfurizing agent is added into pure yellow water to be pre-processed, wherein desulfurizing agent is sodium hydroxide solution or soluble sodium salting liquid, as Na in reaction solution+Concentration stops pretreatment when reaching 0.01mol/L to 0.025mol/L, obtains by pretreated yellow water；Pretreated yellow water will be passed through and carry out Continuous convective synthetic reaction with process recycled water, stop reaction when the pH value of reaction paste reaches 9.5-11.5, reaction paste carries out continuous sedimentation curing, is then separated by solid-liquid separation, and collects solid；The solid of collection obtains barium carbonate product by washing, drying.The present invention also provides the barium carbonate product prepared using this method, barium carbonate contents >=99.48wt%.The method of the present invention prepares industrial potassium titanate by carrying out decarburization recycling to the recycled process water, improves the barium carbonate production rate of recovery to greatest extent and reduces solid waste generation, meets the requirement that country economizes on resources and lowers discharge.
Description
Technical field
The invention belongs to resources to reuse technical field, in particular it relates to which a kind of the recycled process water prepares carbon
The method of sour barium, and the barium carbonate that is prepared by the preparation method.
Background technology
Barium carbonate belongs to inorganic chemicals industry staple product, is widely used in magnetic material, PTC electronic ceramics, liquid crystal base
Glass sheet, architectural pottery, purification of water quality and other barium salt basic materials, the optimization of production technology is for reducing cost and subtracting
Few waste discharge is of great significance.
Traditional industrial potassium titanate technique passes through dispensing, roasting, leaching, carbon mostly using barite and anthracite as raw material
Change, the technique productions such as drying and obtain, but this production method is not recycled process the recycled process water and causes part
Barium carbonate, which enters, becomes solid waste in barium slag, be unfavorable to reducing cost and reducing solid waste.
For the above problem present in barium carbonate production technology, it is badly in need of one kind at present by being taken off to the recycled process water
The method that carbon recycling prepares industrial potassium titanate is given up so as to improve the barium carbonate production rate of recovery to greatest extent and reduce solid
The generation of gurry, to meet the national requirement to economize on resources and lower discharge.
Invention content
It is an object of the invention in view of the drawbacks of the prior art, provide a kind of method preparing barium carbonate and by this
The barium carbonate product that preparation method is prepared.
On the one hand, the present invention provides a kind of preparation method of barium carbonate, this method includes：
(1) by yellow water sedimentation, press filtration, pure yellow water is obtained；
(2) desulfurizing agent is added into pure yellow water to be pre-processed, wherein desulfurizing agent is sodium hydroxide solution or solvable
Property sodium salt solution, as Na in reaction solution+Stop pretreatment when concentration reaches 0.01mol/L to 0.025mol/L, obtain by
Pretreated yellow water；
(3) pretreated yellow water will be passed through and carries out Continuous convective synthetic reaction with process recycled water, as the pH of reaction paste
Value stops reaction when reaching 9.5 to 11.5, reaction paste carries out continuous sedimentation curing, is then separated by solid-liquid separation, and collects solid；
(4) solid collected obtains barium carbonate product by washing, drying.
The concentration of preparation method above-mentioned, the desulfurizing agent is 0.1mol/L to 0.5mol/L.
Preparation method above-mentioned, the soluble sodium salt are Na2CO3Or NaOH.
Preparation method above-mentioned, the pure yellow water are the barium sulfide solutions of a concentration of 30g/L to 80g/L.
Preparation method above-mentioned, the pure yellow water is the barium sulfide solution of a concentration of 30g/L to 50g/L, in step
(2) in, as Na in reaction solution+Concentration stops pretreatment when reaching 0.01mol/L to 0.015mol/L.
Preparation method above-mentioned, the pure yellow water is the barium sulfide solution of a concentration of 50g/L to 80g/L, in step
(2) in, as Na in reaction solution+Concentration stops pretreatment when reaching 0.015mol/L to 0.02mol/L.
Preparation method above-mentioned, in step (3), the flow-rate ratio by pretreated yellow water and process recycled water is 1:
(3-7)。
Preparation method above-mentioned carries out Continuous convective conjunction in step (3) by pretreated yellow water and process recycled water
Time at reaction is 10 minutes to 60 minutes.
Preparation method above-mentioned, in step (3), the time that reaction paste carries out continuous sedimentation curing is 2 hours to 5 small
When.
On the other hand, the present invention provides the barium carbonate products being prepared using preparation method above-mentioned, wherein carbonic acid
Barium content >=99.48wt%.
Barium carbonate above-mentioned, wherein Strontium carbonate contents≤0.27wt%, total sulfur content≤0.25wt%, iron content≤
0.0021wt%, hydrochloric acid insoluble substance content≤0.09wt%, carbonate content≤0.030wt%, D50It is 2.0 μm to 3.0 μm.
Compared with the prior art, technical scheme of the present invention has the advantages that：
1. the method for the present invention solves the recycled process water and consumes yellow water and the technology as barium slag in leaching containing carbonic acid
Problem, it is proposed that the decarburization technique and decarburization barium carbonate product Quality Control Technology turned waste into wealth have work in barium carbonate
Skill technological progress and demonstration leading action.
2. social benefit：It is expected that after the method implement scale application of the present invention, it is possible to provide a considerable amount of job opportunities, solution
The certainly problem of employment of some of the staff to local social stability and improves Living consumption with good promotion meaning.
3. economic benefit：It is expected that after the method for the present invention enters the stable industrial production stage, remanufacture carbon may be implemented
Sour 500 ton/month of barium product, economic value about 9,000,000/year bring more economic benefits under extremely low cost.
4. environmental benefit：It is expected that after the method for the present invention practices, the row of 6000 tons of industrial barium slag can be reduced every year
It puts, reduces the processing cost of barium slag, there is larger environmental benefit.
Description of the drawings
Fig. 1 is the process flow chart of the method for the present invention.
Fig. 2 is the process flow chart for producing barium carbonate in the prior art.
Fig. 3 is the integrated artistic flow chart that barium carbonate is produced after the method for the present invention is implemented.
Specific implementation mode
In order to fully understand the purpose of the present invention, feature and effect, by following specific implementation modes, the present invention is made detailed
It describes in detail bright.For the process of the present invention in addition to following the description, remaining is all made of the conventional method or device of this field.Unless otherwise
Illustrate, otherwise the technical term involved in the present invention all has the normally understood meaning of those skilled in the art.
Currently, in the preparation process of barium carbonate, in barium sulphide leaching process surface there are a large amount of white powder slurries and
As barium slag waste, inventors discovered through research that, reason mainly recycles in leaching water and is dissolved with certain density carbonic acid
Root and carbon dioxide.For there are the problem of, the present invention proposes " synthesis of low concentration yellow water purification-pretreatment-Continuous convective "
Optimize technique carries out carbonization treatment to process recycled water using certain density barium sulfide solution, prepares and meet downstream application
Barium carbonate product, improve leaching the barium sulphide rate of recovery, reduce barium slag yield, realize industrialized production, to carry
High resource utilization.
The barium carbonate preparation method of the present invention is described in detail with reference to Fig. 1.
The present invention barium carbonate preparation method include：
The first step, the purification of low concentration yellow water：By yellow water sedimentation, press filtration, pure yellow water is obtained.
In the present invention, yellow water refers to the leaching solution that barite reduction roasting generates BaS clinkers, and main component is Ba
(OH)2、Ba(HS)2, the yellow water concentration that refers in the art usually indicates that this is the one of this field with barium sulphide concentration
The usual expression-form of kind.
Specifically, leaching low concentration yellow water is squeezed into low concentration yellow water settling tank, clarification purpose is reached by natural subsidence,
Because it also obtains pure yellow water containing fine impure suspended matter by plate and frame filter press press filtration.It is handled by sedimentation and press filtration
Later, the impurity such as the insoluble matter in yellow water, suspended matter are removed, and barium sulphide ingredient is retained, thus the pure yellow water is dense
Degree is the barium sulfide solution of 30g/L to 80g/L.
Second step, pretreatment：Pure yellow water is pre-processed using desulfurizing agent.Specifically, with constant flow pump to pure
Yellow water in concentration is added is that the desulfurizing agent of 0.1mol/L to 0.5mol/L is pre-processed, wherein desulfurizing agent is sodium carbonate or hydrogen
Sodium oxide molybdena, as Na in reaction solution+Concentration stops pretreatment when reaching 0.01mol/L to 0.025mol/L, obtains by locating in advance
The yellow water of reason.
Desulfurizing agent is optimized in the present invention, successfully introduces a kind of sodium salt as desulfurizing agent, and optimize desulfurizing agent
Concentration so that solbar is converted to sodium polysulfide in subsequent Continuous convective building-up process, then passes through separation of solid and liquid
The sodium polysulfide is removed with solution, to realize the control to total sulfur, product quality will not be impacted.Specifically, exist
In this step, by introducing sodium ion in the pure yellow water to low concentration, and make Na ion concentration control 0.01mol/L extremely
0.025mol/L ranges make sodium ion form soluble coordination with polysulfide or sulphur in follow-up synthetic reaction process
Object is closed, thus by product quality total sulfur norm controlling 0.3% hereinafter, meeting downstream client's needs.
Na in reaction solution+Concentration can be adjusted according to the concentration of yellow water.In a specific embodiment, pure
Net yellow water is the barium sulfide solution of a concentration of 30g/L to 50g/L, as Na in reaction solution+Concentration reaches 0.01mol/L extremely
Stop pretreatment when 0.015mol/L.In another embodiment specific implementation mode, pure yellow water is a concentration of 50g/L to 80g/L
Barium sulfide solution, as Na in reaction solution+Concentration stops pretreatment when reaching 0.015mol/L to 0.02mol/L.
Third walks：Continuous convective synthesizes：Pretreated yellow water will be passed through to synthesize instead with process recycled water progress Continuous convective
It answers, then reaction paste carries out continuous sedimentation curing, is then separated by solid-liquid separation, and collects solid.
In the present invention, process recycled water refers to yellow water and CO2It is solid that reaction generation barium carbonate slurries are carried out in carbonators
The water that liquid separation generates, process water cycle leach BaS clinkers, and main component is containing carbonate, carbon dioxide
Aqueous solution.
In the third step, the chemical reaction of generation is mainly：
BaS+H2O+CO2→BaCO3+H2S
H2O+BaS+O2→BaSx+1+2OH-
BaSx+1+H2O+CO2→BaCO3+S+H2S
BaSx+1+2Na++CO3 2-→BaCO3+Na2Sx+1
In this step, inventor creatively carries out decarburization to make using by pretreated yellow water to process recycled water
Standby barium carbonate.By studying, carbon dioxide is carbonated in process recycled water difference link and the mechanism that balances each other, reinforcement follow technique
The carbonization treatment of ring water generates barium carbonate again, reduces barium resource waste and pollution, improves barium resource utilization.Also, it uses
Convection current chemical combination, barium carbonate product stable crystal formation, product pattern is uniform, and is carried out to the barium carbonate of generation using four-stage grading sedimentation
Crystalline form curing controls, gained barium carbonate powder even particle size distribution, does not generate reunion between particle, product physical and chemical performance obtains
To larger raising.
In addition, reaction speed, the uniformity, reaction end etc. are optimized.Specifically, by pretreated yellow water with
The flow-rate ratio (speed ratio that i.e. the two is added) of process recycled water is 1: (3-7) (preferably 1: 4-6)；When the two is reacted
Reaction paste pH value stops reaction when reaching 9.5 to 11.5 (preferably 10.0-11.0)；By pretreated yellow water and process cycles
The time that water carries out Continuous convective synthetic reaction is approximately 10 minutes to 60 minutes (preferably 30-45 minutes)；After synthetic reaction stops,
The time that reaction paste carries out continuous sedimentation curing is 2 hours to 5 hours (preferably 3-4 hours).By to reaction speed, uniformly
The optimization of degree, reaction end, finally obtained barium carbonate product exist in particle-size distribution, total sulfur, pattern, impurity level etc.
In indication range, even better than general professional standard；In addition, the carbonate and carbon dioxide recovery in process recycled water are complete,
Decarburization effect is ideal.Due to being controlled reaction time and reaction end, to make the total sulfur index of product obtain very well
Control；Since speed ratio and sedimentation curing time is added in control yellow water and process recycled water reaction mass, to ensure to give birth to
Produce efficiency while, make product microcosmic particle pattern uniformly, size distribution concentrate.
4th step：The solid collected to third step is washed and is dried, to obtain barium carbonate product.Washing and drying
The conventional method that this field can be used carries out.For example, washing can be according to solid and liquid weight using 50-80 DEG C of hot water than 1:
(3-6) (such as 1: 4) carries out hot wash 1-3 times (such as 2 times), and drying can be done in 100-160 DEG C of (such as 105 DEG C) baking oven
4-10 hours dry (such as 6 hours).
The method of the present invention can also bring good economic benefit and environmental benefit.Fig. 2 is to produce carbonic acid in the prior art
The process flow chart of barium, Fig. 3 are the integrated artistic flow charts that barium carbonate is produced after the method for the present invention is implemented.By comparing Fig. 2 and
The method that Fig. 3 can be seen that the present invention is generated by optimizing for process conditions to recycle in existing barium carbonate production
Waste, perfect technological process, and produce the barium carbonate product of high-quality, to reduce production cost, reduce
The discharge of industrial barium slag the like waste reduces the processing cost of barium slag and improves environment.
Method using the present invention, can prepare the barium carbonate product of high-quality, and barium carbonate content >=
99.48wt%, Strontium carbonate contents≤0.27wt%, total sulfur content is (with SO4Meter)≤0.25wt%, iron content is (with Fe2O3Meter)≤
0.0021wt%, hydrochloric acid insoluble substance content≤0.09wt%, carbonate content≤0.030wt%, D50It is 2.0 μm to 3.0 μm.
Embodiment
It is further illustrated the present invention below by the mode of embodiment, but does not therefore limit the present invention to the reality
It applies among a range.In the following examples, the experimental methods for specific conditions are not specified, according to conventional methods and conditions, or according to quotient
Product specification selects.
The yellow water and process recycled water used in following embodiments is that applicant enterprise produces barium carbonate using conventional method
It generates in the process.
Barium carbonate product analyzes reference in following embodiments《GB/T1614-2011 industrial potassium titanates》Assay method is surveyed
It is fixed；Particle size analysis methods：With the average grain diameter for the volume reference that wet type laser method measures, granularmetric analysis device：2000MU type grains
Diameter instrument, Britain's Ma Erda corporations.
Embodiment 1
(1) yellow water is squeezed into low concentration yellow water settling tank, clarification purpose is reached by natural subsidence, then passes through sheet frame pressure
Filter press filtration obtains pure low concentration yellow water to remove fine impure suspended matter, is the BaS solution that concentration is 50g/L.
(2) 0.3mol/L sodium hydroxide solutions are added into pure yellow water with constant flow pump, control Na+It is a concentration of
0.015mol/L stops pretreatment.
(3) pretreated BaS solution and process recycled water will be passed through pair add and react, BaS solution and process recycled water
Flow be 3m respectively3/ h and 15m3/ h, it is 11 that 15 minutes reaction time, which controlled reaction end pH value, and then natural subsidence 2 is small
When, slurries are filtered after the completion, collect solid, solution, which keeps sample, does carbonate detection.
(4) solid is washed twice with hot water by solid-to-liquid ratio 1: 4, and obtained solid is placed in 105 DEG C of oven dryings 4 hours, is obtained
Barium carbonate sample 1#.
Embodiment 2
(1) yellow water is squeezed into low concentration yellow water settling tank, clarification purpose is reached by natural subsidence, then passes through sheet frame pressure
Filter press filtration obtains pure low concentration yellow water to remove fine impure suspended matter, is the BaS solution that concentration is 30g/L.
(2) 0.1mol/L sodium hydroxide solutions are added into pure yellow water with constant flow pump, control Na+It is a concentration of
0.01mol/L stops pretreatment.
(3) pretreated BaS solution and process recycled water will be passed through pair add and react, BaS solution and process recycled water
Flow be 3m respectively3/ h and 10m3/ h, it is 9.5 that 30 minutes reaction time, which controlled reaction end pH value, and then natural subsidence 5 is small
When, slurries are filtered after the completion, collect solid, solution, which keeps sample, does carbonate detection.
(4) solid is washed twice with hot water by solid-to-liquid ratio 1: 4, and obtained solid is placed in 105 DEG C of oven dryings 4 hours, is obtained
Barium carbonate sample 2#.
Embodiment 3
(1) yellow water is squeezed into low concentration yellow water settling tank, clarification purpose is reached by natural subsidence, then passes through sheet frame pressure
Filter press filtration obtains pure low concentration yellow water to remove fine impure suspended matter, is the BaS solution that concentration is 80g/L.
(2) 0.5mol/L sodium carbonate liquors are added into pure yellow water with constant flow pump, control Na+A concentration of 0.02mol/
L stops pretreatment.
(3) pretreated BaS solution and process recycled water will be passed through pair add and react, BaS solution and process recycled water
Flow be 2.5m respectively3/ h and 10m3/ h, it is 10 that 55 minutes reaction time, which controlled reaction end pH value, then natural subsidence 3.5
Hour, slurries are filtered after the completion, collect solid, solution, which keeps sample, does carbonate detection.
(4) solid is washed twice with hot water by solid-to-liquid ratio 1: 4, and obtained solid is placed in 105 DEG C of oven dryings 4 hours, is obtained
Barium carbonate sample 3#.
1 barium carbonate of table analyzes testing result
| Detection project | Internal control index | 1# | 2# | 3# |
| Barium carbonate content | >=99.00% | 99.60 | 99.52 | 99.48 |
| Strontium carbonate contents | ≤ 1.0% | 0.24 | 0.22 | 0.27 |
| Total sulfur is (with SO4Meter) | ≤ 0.03% | 0.18 | 0.25 | 0.21 |
| Iron is (with Fe2O3Meter) | ≤ 0.004% | 0.0021 | 0.0019 | 0.0014 |
| Hydrochloric acid insoluble substance | ≤ 0.3% | 0.08 | 0.08 | 0.09 |
| NaCO3 | ≤ 0.01% | 0.0024 | 0.030 | 0.0027 |
| D50 | μm | 2.4 | 2.4 | 2.3 |
Barium carbonate product prepared by method using the present invention, which is can be seen that, from the data of table 1 complies fully with existing industry
Standard, also, in terms of certain detection projects, barium carbonate product prepared by method using the present invention is better than current standard.
Constituent content inspection result in 2 process recycled water of table
The method that can be seen that the present invention from the data of table 2 effectively realizes process recycled water decarburization.
The present invention is hereinbefore disclosed with preferred embodiment, but it should be understood by those skilled in the art that, these
Embodiment is only used for describing the present invention, and should not be construed as limiting the scope of the invention.It should be noted that every implement with these
Example equivalent variation and displacement, should all be set as being covered by scope of the presently claimed invention.Therefore, protection scope of the present invention
The range that should be subject to defined in claims.
Claims (11)
1. a kind of preparation method of barium carbonate, which is characterized in that this method includes：
(1) by yellow water sedimentation, press filtration, pure yellow water is obtained；
(2) desulfurizing agent is added into pure yellow water to be pre-processed, wherein desulfurizing agent is sodium hydroxide solution or soluble sodium
Salting liquid, as Na in reaction solution+Concentration stops pretreatment when reaching 0.01mol/L to 0.025mol/L, obtains by locating in advance
The yellow water of reason；
(3) pretreated yellow water will be passed through and carries out Continuous convective synthetic reaction with process recycled water, when the pH value of reaction paste reaches
To reaction is stopped when 9.5 to 11.5, reaction paste carries out continuous sedimentation curing, is then separated by solid-liquid separation, and collects solid；
(4) solid collected obtains barium carbonate product by washing, drying.
2. preparation method according to claim 1, which is characterized in that the concentration of the desulfurizing agent be 0.1mol/L extremely
0.5mol/L。
3. preparation method according to claim 1, which is characterized in that the soluble sodium salt is Na2CO3Or NaOH.
4. preparation method according to claim 1, which is characterized in that the pure yellow water be a concentration of 30g/L extremely
The barium sulfide solution of 80g/L.
5. preparation method according to claim 4, which is characterized in that the pure yellow water be a concentration of 30g/L extremely
The barium sulfide solution of 50g/L, in step (2), as Na in reaction solution+When concentration reaches 0.01mol/L to 0.015mol/L
Stop pretreatment.
6. preparation method according to claim 4, which is characterized in that the pure yellow water be a concentration of 50g/L extremely
The barium sulfide solution of 80g/L, in step (2), as Na in reaction solution+When concentration reaches 0.015mol/L to 0.02mol/L
Stop pretreatment.
7. preparation method according to claim 1, which is characterized in that in step (3), by pretreated yellow water and work
The flow-rate ratio of skill recirculated water is 1: (3-7).
8. preparation method according to claim 1, which is characterized in that in step (3), by pretreated yellow water and work
The time that skill recirculated water carries out Continuous convective synthetic reaction is 10 minutes to 60 minutes.
9. preparation method according to claim 1, which is characterized in that in step (3), reaction paste carries out continuous sedimentation
The time of curing is 2 hours to 5 hours.
10. the barium carbonate being prepared using claim 1-9 any one of them preparation methods, which is characterized in that barium carbonate
Content >=99.48wt%.
11. barium carbonate according to claim 10, which is characterized in that Strontium carbonate contents≤0.27wt%, total sulfur content≤
0.25wt%, iron content≤0.0021wt%, hydrochloric acid insoluble substance content≤0.09wt%, carbonate content≤0.030wt%, D50
It is 2.0 μm to 3.0 μm.
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| CN201810808754.8A CN108793218B (en) | 2018-07-23 | 2018-07-23 | Method for preparing barium carbonate and barium carbonate prepared by the same |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114180610A (en) * | 2021-12-28 | 2022-03-15 | 贵州红星发展股份有限公司 | Method for preparing large-particle-size barium carbonate by four-tower series carbonization method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1058199A (en) * | 1990-07-14 | 1992-01-29 | 化学工业部天津化工研究院 | The manufacture method of high-pruity barium carbonate |
| CN103058251A (en) * | 2013-01-22 | 2013-04-24 | 贵州红星发展股份有限公司 | Method for preparing low-sulfur barium carbonate and prepared barium carbonate product |
| CN103435083A (en) * | 2013-08-29 | 2013-12-11 | 贵州红星发展股份有限公司 | Narrowly distributed subsphaeroidal low-sulfur barium carbonate and preparation method thereof |
-
2018
- 2018-07-23 CN CN201810808754.8A patent/CN108793218B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1058199A (en) * | 1990-07-14 | 1992-01-29 | 化学工业部天津化工研究院 | The manufacture method of high-pruity barium carbonate |
| CN103058251A (en) * | 2013-01-22 | 2013-04-24 | 贵州红星发展股份有限公司 | Method for preparing low-sulfur barium carbonate and prepared barium carbonate product |
| CN103435083A (en) * | 2013-08-29 | 2013-12-11 | 贵州红星发展股份有限公司 | Narrowly distributed subsphaeroidal low-sulfur barium carbonate and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114180610A (en) * | 2021-12-28 | 2022-03-15 | 贵州红星发展股份有限公司 | Method for preparing large-particle-size barium carbonate by four-tower series carbonization method |
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