CN107162035A - A kind of preparation method of blanc fixe - Google Patents
A kind of preparation method of blanc fixe Download PDFInfo
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- CN107162035A CN107162035A CN201710418557.0A CN201710418557A CN107162035A CN 107162035 A CN107162035 A CN 107162035A CN 201710418557 A CN201710418557 A CN 201710418557A CN 107162035 A CN107162035 A CN 107162035A
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- blanc fixe
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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
- C01F11/46—Sulfates
- C01F11/462—Sulfates of Sr or Ba
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Life Sciences & Earth Sciences (AREA)
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- Inorganic Chemistry (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The present invention provides a kind of preparation method of blanc fixe, and preparation process is as follows：（1）Barium carbonate is added in stirring-type ball grinder, water is added, while adding ball milling pearl, stirring obtains solution A；（2）Sodium sulphate is added in aqueous beaker, 60 DEG C of magnetic agitation 30min are configured to metabisulfite solution, are designated as solution B stand-by；（3）By EDTA 2Na it is slow at the uniform velocity be added to step（1）Solution A in, stir 0.5 3h, obtain solution C；（4）Will（2）Middle prep solution B is added to（3）Solution C in, after completion of dropping with H2SO4/NaOH control pH value of solution between 5 10,500rpm stir 0.5 9h, obtain slurries D；（5）Will（4）Obtained slurries D is through washing, centrifugation, drying to blanc fixe.
Description
Technical field
The present invention relates to a kind of preparation method of blanc fixe.
Background technology
Barium sulfate is one of chemical products important now, its chemical property stabilization, strong inert, acid and alkali-resistance, high specific gravity, height
Whiteness and the advantages of X-ray can be absorbed it is of great interest, be mainly used in paint, ink, plastics, poster paint, cosmetic
The raw material or filler of product, battery.For example, barium sulfate, which can be used in rubber, makees filler and reinforcing agent；Used in polychlorostyrene
Make filler and weighting agent in ethane resin；Make surface smears used in photographic pape and art paper；Make starching used in textile industry
Agent；It is used as fining agent used in glassware, froth breaking and increase gloss can be played.
China Patent Publication No. CN 101643232A disclose a kind of preparation method of blanc fixe, this method be by
Barium carbonate and sodium sulphate are dissolved with certain proportion to be stirred, and blanc fixe is can obtain after centrifugal filtration, washing drying and crushing.
But the method has that the blanc fixe particle diameter prepared is not small enough, reaction production rate is relatively low, the reaction time is longer and energy resource consumption
It is larger to wait not enough.
Open bright etc.（EDTA methods synthesize barium sulfate particles, China YouSe Acta Metallurgica Sinica, 2009,19（8）：1511-1515）Carry
A kind of method for preparing barium sulfate particles is gone out, this method is using barium chloride and sodium sulphate as raw material, and EDTA is chelating agent, is prepared
Particle diameter is 1 μm of barium sulfate particle.But the method influences the factor of complex reaction many in preparation process, can cause to prepare
Blanc fixe properties of product it is unstable.
To sum up, the blanc fixe that prepared by existing process has that fineness is inadequate, technology controlling and process is difficult, product quality is stable
The inadequate defect of property, so as to have impact on the application of barium sulfate product.
The content of the invention
There is provided a kind of preparation method of blanc fixe for problem above by the present invention.
Goal of the invention is realized by following scheme：A kind of preparation method of blanc fixe, preparation process is as follows：
（1）0.2-1mol barium carbonate is added in stirring-type ball grinder, 600-1000ml water is added, while adding ball milling
Pearl, 300-500rpm rotating speeds stirring 0.5-1h, obtains solution A；
（2）In the beaker that 0.2-1.2mol sodium sulphate is added to 100-400ml water, 60 DEG C of magnetic agitation 30min are configured to
Metabisulfite solution, is designated as solution B stand-by；
（3）By the appropriate EDTA-2Na for 0.1-1mol it is slow at the uniform velocity be added to step（1）Solution A in, stir 0.5-3h,
Obtain solution C；
（4）Will（2）Middle prep solution B is added to 10-100ml/min rate of addition（3）Solution C in, after completion of dropping
PH value of solution is controlled between 5-10 with H2SO4/NaOH, and 500rpm stirring 0.5-9h obtain slurries D；
（5）Will（4）Obtained slurries D is through washing, centrifugation, drying to blanc fixe.
Further, step（1）In ball milling pearl ratio of grinding media to material be 5:1-1:1.
Further, step（1）In addition water amount be 700-800ml.
Further, step（2）In be added in the beaker of 200-300ml water.
Further, step（3）In mixing speed be 150-500rpm.
Further, step（3）In mixing time be 0.5-2h.
Further, step（4）In metathesis reaction be according to barium carbonate chemically react metering 1-1.2 times add
Sodium sulphate, is the course of reaction that barium carbonate is converted into barium sulfate.
Further, step（4）In mixing time be 1-7h.
Further, step（4）In pH value of solution be 6-9.
Further, step（5）In drying temperature be 60-100 DEG C.
The beneficial effects of the present invention are：Using barium carbonate, sodium sulphate as raw material, Ba2+ is controlled by complexing agent of EDTA-2Na
And SO42- combination speed, prepared under certain raw material proportioning and certain wet ball grinding preparation process condition particle diameter it is small and
The blanc fixe being evenly distributed.This method preparation technology is simple and convenient, and preparation process is without high temperature without high pressure, efficiency high, it is easy to
Industrialized production, reaction filtrate is reusable after processing, nontoxic in preparation process, pollution-free.
Brief description of the drawings
Fig. 1 is flow chart of the invention.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described：
With reference to accompanying drawing 1, a kind of embodiment 1, the preparation method of blanc fixe of the invention, preparation process is as follows：
（1）0.2-1mol barium carbonate is added in stirring-type ball grinder, 600-1000ml water is added, while adding ball milling
Pearl, 300-500rpm rotating speeds stirring 0.5-1h, obtains solution A；
（2）In the beaker that 0.2-1.2mol sodium sulphate is added to 100-400ml water, 60 DEG C of magnetic agitation 30min are configured to
Metabisulfite solution, is designated as solution B stand-by；
（3）By the appropriate EDTA-2Na for 0.1-1mol it is slow at the uniform velocity be added to step（1）Solution A in, stir 0.5-3h,
Obtain solution C；
（4）Will（2）Middle prep solution B is added to 10-100ml/min rate of addition（3）Solution C in, after completion of dropping
PH value of solution is controlled between 5-10 with H2SO4/NaOH, and 500rpm stirring 0.5-9h obtain slurries D；
（5）Will（4）Obtained slurries D is through washing, centrifugation, drying to blanc fixe.
A kind of preparation method of blanc fixe, step（1）In ball milling pearl ratio of grinding media to material be 5:1-1:1.
A kind of preparation method of blanc fixe, step（1）In addition water amount be 700-800ml.
A kind of preparation method of blanc fixe, step（2）In be added in the beaker of 200-300ml water.
A kind of preparation method of blanc fixe, step（3）In mixing speed be 150-500rpm.
A kind of preparation method of blanc fixe, step（3）In mixing time be 0.5-2h.
A kind of preparation method of blanc fixe, step（4）In metathesis reaction be according to barium carbonate chemically react count
The sodium sulphate that 1-1.2 times of amount is added, is the course of reaction that barium carbonate is converted into barium sulfate.
A kind of preparation method of blanc fixe, step（4）In mixing time be 1-7h.
A kind of preparation method of blanc fixe, step（4）In pH value of solution be 6-9.
A kind of preparation method of blanc fixe, step（5）In drying temperature be 60-100 DEG C.
A kind of preparation method of blanc fixe, EDTA-2Na and Ba2+ can form complexing network, control Ba2+ with
SO42- combination speed, so as to control reaction speed, the reunion to the barium sulfate particles of generation plays certain inhibitory action.
In drying course, EDTA-2Na also plays a part of that barium sulfate particles hard aggregation can be suppressed, so that the precipitation prepared
Barium sulfate has preferable granularity and narrower size distribution, also ensure that the stability of barium sulfate product.
A kind of preparation method of blanc fixe, the blanc fixe prepared is spherical barium sulfate, and average grain diameter is
0.5-1.4 μm, good dispersion property exists without substantially reuniting.
A kind of preparation method of blanc fixe, reaction principle of the invention is as follows：
Ba2++EDTA=Ba2+—EDTA
Ba2+—EDTA+SO42−= BaSO4+EDTA
Embodiment 2, a kind of preparation method of blanc fixe,
（1）39.468g barium carbonates are weighed respectively and 712g zirconium oxide ball milling pearls are placed in stirring-type ball grinder, add 700ml water,
500rpm stirs 0.5h.Weigh 28.412g sodium sulphate to be placed in beaker, add 100ml water, 60 DEG C of magnetic agitation 30min are stand-by.
（2）Weigh 74.446gEDTA-2Na and slowly at the uniform velocity add step（1）In barium carbonate solution, 150rpm stirrings 0.5h.
（3）By step（1）The metabisulfite solution of middle preparation is at the uniform velocity added drop-wise to step with 20ml/min speed（2）Solution
In, control pH value of solution to stir 4h for 7 with rotating speed 500rpm after completion of dropping, through washing, centrifugation, 90 DEG C of dryings to precipitated sulfur
Sour barium.
The blanc fixe prepared is spherical, and D50 is 0.503 μm.
Embodiment 3, a kind of preparation method of blanc fixe,
78.936g barium carbonates are weighed respectively and 1050g zirconium oxide ball milling pearls are placed in stirring-type ball grinder, add 900ml water,
400rpm stirs 1h.Weigh 56.824g sodium sulphate to be placed in beaker, add 200ml water, 60 DEG C of stirring 30min are stand-by.
Weigh 74.446gEDTA-2Na and slowly at the uniform velocity add step（1）In barium carbonate solution, 300rpm stirrings 1h.
（3）By step（1）The metabisulfite solution of middle preparation is at the uniform velocity added drop-wise to step with 20ml/min speed（2）Solution
In, it is 9 that pH value of solution is controlled after completion of dropping, and 2h is stirred with rotating speed 500rpm, through washing, centrifugation, 100 DEG C of dryings to precipitation
Barium sulfate.
（4）The blanc fixe prepared is spherical, and D50 is 0.627 μm.
Embodiment 4, a kind of preparation method of blanc fixe,
（1）78.936g barium carbonates are weighed respectively and 864g zirconium oxide ball milling pearls are placed in stirring-type ball grinder, add 800ml water,
300rpm stirs 0.5h.Weigh 56.824g sodium sulphate to be placed in beaker, add 400ml water, 60 DEG C of stirring 1h are stand-by.
（2）Weigh 37.223gEDTA-2Na and slowly at the uniform velocity add step（1）In barium carbonate solution, 500rpm stirring stirrings
0.5h。
（3）By step（1）The metabisulfite solution of middle preparation is at the uniform velocity added drop-wise to step with 10ml/min speed（2）Solution
In, it is 6 that pH value of solution is controlled after completion of dropping, and 6h is stirred with rotating speed 500rpm, through washing, centrifugation, 80 DEG C of dryings to precipitation
Barium sulfate.
The blanc fixe prepared is spherical, and D50 is 0.808 μm.
Embodiment 5, a kind of preparation method of blanc fixe,（1）39.3468g barium carbonates and 1050g oxidations are weighed respectively
Zirconium ball milling pearl is placed in stirring-type ball grinder, adds 1000ml water, 500rpm stirrings 0.5h.Weigh 34.09g sodium sulphate and be placed in burning
In cup, 200ml water is added, 60 DEG C of stirring 1h are stand-by.
（2）Weigh 37.223gEDTA-2Na and slowly at the uniform velocity add step（1）In barium carbonate solution, 150rpm stirring stirrings
3h。
（3）By step（1）The metabisulfite solution of middle preparation is at the uniform velocity added drop-wise to step with 10ml/min speed（2）Solution
In, controlled after completion of dropping pH value of solution be 10, with rotating speed 500rpm stir 9h, through washing, centrifugation, 120 DEG C of dryings to sink
Shallow lake barium sulfate.
The blanc fixe prepared is spherical, and D50 is 0.770 μm.
Although the present invention is described by reference to preferred embodiment, those of ordinary skill in the art should
Work as understanding, the description of above-described embodiment can be not limited to, in the range of claims, can make each in form and details
Plant change.
Claims (10)
1. a kind of preparation method of blanc fixe, it is characterised in that：Preparation process is as follows：
（1）0.2-1mol barium carbonate is added in stirring-type ball grinder, 600-1000ml water is added, while adding ball milling
Pearl, 300-500rpm rotating speeds stirring 0.5-1h, obtains solution A；
（2）In the beaker that 0.2-1.2mol sodium sulphate is added to 100-400ml water, 60 DEG C of magnetic agitation 30min are configured to
Metabisulfite solution, is designated as solution B stand-by；
（3）By the appropriate EDTA-2Na for 0.1-1mol it is slow at the uniform velocity be added to step（1）Solution A in, stir 0.5-3h,
Obtain solution C；
（4）Will（2）Middle prep solution B is added to 10-100ml/min rate of addition（3）Solution C in, after completion of dropping
PH value of solution is controlled between 5-10 with H2SO4/NaOH, and 500rpm stirring 0.5-9h obtain slurries D；
（5）Will（4）Obtained slurries D is through washing, centrifugation, drying to blanc fixe.
2. a kind of preparation method of blanc fixe according to claim 1, it is characterised in that：Step（1）In ball milling
The ratio of grinding media to material of pearl is 5:1-1:1.
3. a kind of preparation method of blanc fixe according to claim 1, it is characterised in that：Step（1）In addition
The amount of water is 700-800ml.
4. a kind of preparation method of blanc fixe according to claim 1, it is characterised in that：Step（2）In be added to
In the beaker of 200-300ml water.
5. a kind of preparation method of blanc fixe according to claim 1, it is characterised in that：Step（3）In stirring
Speed is 150-500rpm.
6. a kind of preparation method of blanc fixe according to claim 1, it is characterised in that：Step（3）In stirring
Time is 0.5-2h.
7. a kind of preparation method of blanc fixe according to claim 1, it is characterised in that：Step（4）In subdivision
Solution reaction is the sodium sulphate added according to 1-1.2 times of barium carbonate chemical reaction metering, is that barium carbonate is converted into the anti-of barium sulfate
Answer process.
8. a kind of preparation method of blanc fixe according to claim 1, it is characterised in that：Step（4）In stirring
Time is 1-7h.
9. a kind of preparation method of blanc fixe according to claim 1, it is characterised in that：Step（4）In solution
PH is 6-9.
10. a kind of preparation method of blanc fixe according to claim 1, it is characterised in that：Step（5）In drying
Temperature is 60-100 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710418557.0A CN107162035A (en) | 2017-06-06 | 2017-06-06 | A kind of preparation method of blanc fixe |
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| CN201710418557.0A CN107162035A (en) | 2017-06-06 | 2017-06-06 | A kind of preparation method of blanc fixe |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111544822A (en) * | 2020-04-13 | 2020-08-18 | 上海圣珑环境修复技术有限公司 | Barium slag stabilizing treatment method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1398789A (en) * | 2002-08-13 | 2003-02-26 | 华北工学院 | Prepn of nano barium sulfate |
| CN101643231A (en) * | 2009-06-08 | 2010-02-10 | 王嘉兴 | Method for preparing co-production sodium carbonate of nano barium sulfate |
| CN105293556A (en) * | 2015-10-12 | 2016-02-03 | 中南大学 | Method for extracting tungsten from tungsten-containing sodium carbonate solution and comprehensively utilizing extracted solution |
-
2017
- 2017-06-06 CN CN201710418557.0A patent/CN107162035A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1398789A (en) * | 2002-08-13 | 2003-02-26 | 华北工学院 | Prepn of nano barium sulfate |
| CN101643231A (en) * | 2009-06-08 | 2010-02-10 | 王嘉兴 | Method for preparing co-production sodium carbonate of nano barium sulfate |
| CN105293556A (en) * | 2015-10-12 | 2016-02-03 | 中南大学 | Method for extracting tungsten from tungsten-containing sodium carbonate solution and comprehensively utilizing extracted solution |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111544822A (en) * | 2020-04-13 | 2020-08-18 | 上海圣珑环境修复技术有限公司 | Barium slag stabilizing treatment method |
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Application publication date: 20170915 |
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