CN106745158A - A kind of method for preparing big particle diameter barium sulfate - Google Patents
A kind of method for preparing big particle diameter barium sulfate Download PDFInfo
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- CN106745158A CN106745158A CN201611112002.5A CN201611112002A CN106745158A CN 106745158 A CN106745158 A CN 106745158A CN 201611112002 A CN201611112002 A CN 201611112002A CN 106745158 A CN106745158 A CN 106745158A
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- particle diameter
- barium sulfate
- big particle
- barium
- suspension
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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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a kind of method for preparing big particle diameter barium sulfate.The present invention is with BaCl2And CaSO4It is raw material, it is respectively prepared barium chloride solution and suspension of calcium sulfate, suspension of calcium sulfate is put into constant-temperature heating magnetic stirring apparatus, design temperature, stirring is opened, using constant flow pump to barium chloride solution is gradually added dropwise in suspension, continues to stir after completion of dropping, filtering, washing, drying, get product barium sulfate.The method can be used to prepare the barium sulfate of big particle diameter, and the method is simple to operate, and equipment investment is few, raw materials used cheap and easy to get, be a kind of economic and practical method.
Description
Technical field
The invention belongs to chemical material field, it is related to field of inorganic nonmetallic material, mainly one kind to prepare big particle diameter sulphur
The method of sour barium.
Background technology
Barium sulfate is the powder of white-amorphous, due to its be easy to exploitation, it is with low cost, with compared with soft and oil suction
Numerous superior functions such as value, nontoxic, of light color, brightness is high, anti-soda acid, light resistance and good dispersion, have been developed as one kind
Indispensable inorganic chemical industry material.And the performance that the nanometer barium sulfate grains of different-grain diameter have has obvious difference, it is applicable
In different aspects.Only when the barium sulfate particle diameter for obtaining could well be used its advantage within the limits prescribed, play
Its effect.Update shows that big particle diameter barium sulfate is very popular in many emerging industries, and its market price ratio is common sulphur
Sour barium is higher by a lot, therefore, the development very Worth Expecting of this respect.
Calcium sulfate be in phosphoric acid production with sulfuric acid treating phosphorite when the main component of solid slag ardealite that produces, mesh
Preceding annual production is very big, but comprehensive utilization ratio is very low.Therefore barium sulfate is prepared by raw material of calcium sulfate, principle is extremely cheap and easy to get.
China Patent Publication No. CN1398789A discloses a kind of method for preparing barium sulfate, and the invention uses complex-precipitation
Barium sulfate average grain diameter prepared by method is 25nm.
China Patent Publication No. CN101254938A discloses a kind of method for preparing barium sulfate, and the invention uses soluble
The barium sulfate average grain diameter that barium salt is prepared with soluble sulphate reaction is 200-500nm.
China Patent Publication No. CN101754932A discloses a kind of method for preparing barium sulfate, and the invention uses solid hydrogen
Barium monoxide prepares the barium sulfate and lithium hydroxide solution that average grain diameter is for 0.5-1 μm with the soluble sulphate reaction containing lithium.
In the method for blanc fixe made above, raw material sources do not enrich, complex process, and generally existing product cut size
It is small, the phenomenon such as skewness.
The content of the invention
A kind of present invention problem present in the current technology of solution, there is provided method for preparing big particle diameter barium sulfate.Use
The inventive method prepares barium sulfate, and with low cost, simple to operate and pollution-free, particle diameter is big.
The present invention is achieved using following technical scheme：
A kind of method for preparing big particle diameter barium sulfate of the present invention, it comprises the following steps：
1) barium chloride solution and suspension of calcium sulfate are prepared, it is standby；The barium chloride solution concentration is
0.1~2.5mol/L；The amount ratio of material is 1 when the calcium sulfate mixes with barium chloride:1~2；
2) suspension of calcium sulfate is put into constant-temperature heating magnetic stirring apparatus, design temperature is 25~100 DEG C, opens stirring；
3) using constant flow pump to barium chloride solution is added dropwise in suspension of calcium sulfate；
4) continue stirring reaction after completion of dropping, be aged；
5) filter, wash, dry, get product barium sulfate, the drying temperature is 80-120 DEG C.
Preferably, step 1) described in suspension of calcium sulfate solid content be 68~408g/L.
Preferably, step 2) described in reaction design temperature be most preferably 50 DEG C.
Preferably, step 2) described in reaction mixing speed be 5~25r/min.
Preferably, step 3) described in barium chloride solution rate of addition be 0.35~6.92mL/min.
Preferably, step 3) described in the amount ratio of calcium sulfate material when mixing with barium chloride be 1:1.2.
Step 4) described in digestion time be 0.5~4h.
Preferably, step 5) in, the drying temperature is 110 DEG C.
Preferably, step 5) described in drying time be 1~4h.
Most preferably, a kind of method for preparing big particle diameter barium sulfate of the present invention includes step in detail below：
1) it is suspension of calcium sulfate of 136g/L to prepare the barium chloride solution and solid content that concentration is 0.5mol/L respectively；
2) suspension of calcium sulfate is put into constant-temperature heating magnetic stirring apparatus, sets bath temperature as 50 DEG C, mixing speed is
12.5r/min；
3) constant flow pump is utilized, to barium chloride solution, rate of addition 1.47mL/min are added dropwise in suspension of calcium sulfate；
4) stirring reaction is continued after completion of dropping, digestion time is 4h；
5) filter, washed with absolute ethyl alcohol, 110 DEG C drying 4h, obtain final product big particle diameter barium sulfate product.
Prominent effect of the invention is：
Barium sulfate is prepared by raw material of calcium sulfate, raw material sources are abundant, cheap and easy to get, process is simple, it is easy to operate.With this
Method can prepare the barium sulfate of big particle diameter, reach 850nm, and Granularity Distribution is uniform.
Brief description of the drawings
Fig. 1 is the XRD spectra of barium sulfate particle prepared by the inventive method.
Fig. 2 is the SEM figures that barium sulfate prepared by the inventive method amplifies 20000 times.
Fig. 3 is the SEM figures of 60000 times of barium sulfate method prepared by the inventive method.
Specific embodiment
Make further full and accurate explanation to the present invention below by the drawings and specific embodiments.
Embodiment 1
A kind of method for preparing big particle diameter barium sulfate, it comprises the following steps：
1) it is suspension of calcium sulfate of 68g/L to prepare the barium chloride solution and solid content that concentration is 0.1mol/L respectively；
2) suspension of calcium sulfate is put into constant-temperature heating magnetic stirring apparatus, sets bath temperature as 25 DEG C, mixing speed is
5r/min；
3) constant flow pump is utilized, to barium chloride solution, rate of addition 1.47mL/min are added dropwise in suspension of calcium sulfate；
4) stirring reaction is continued after completion of dropping, digestion time is 30min；
5) filter, washed with absolute ethyl alcohol, 80 DEG C drying 1h, obtain final product average grain diameter be 258nm barium sulfate.
Embodiment 2
A kind of method for preparing big particle diameter barium sulfate, it comprises the following steps：
1) it is suspension of calcium sulfate of 136g/L to prepare the barium chloride solution and solid content that concentration is 0.5mol/L respectively；
2) suspension of calcium sulfate is put into constant-temperature heating magnetic stirring apparatus, sets bath temperature as 50 DEG C, mixing speed is
12.5r/min；
3) constant flow pump is utilized, to barium chloride solution, rate of addition 1.47mL/min are added dropwise in suspension of calcium sulfate；
4) stirring reaction is continued after completion of dropping, digestion time is 4h；
5) filter, washed with absolute ethyl alcohol, 110 DEG C drying 4h, obtain final product average grain diameter be 850nm barium sulfate.
Embodiment 3
A kind of method for preparing big particle diameter barium sulfate, it comprises the following steps：
1) it is suspension of calcium sulfate of 136g/L to prepare the barium chloride solution and solid content that concentration is 1.0mol/L respectively；
2) suspension of calcium sulfate is put into constant-temperature heating magnetic stirring apparatus, sets bath temperature as 75 DEG C, mixing speed is
12.5r/min；
3) constant flow pump is utilized, to barium chloride solution, rate of addition 1.47mL/min are added dropwise in suspension of calcium sulfate；
4) stirring reaction is continued after completion of dropping, digestion time is 30min；
5) filter, washed with absolute ethyl alcohol, 120 DEG C drying 3h, obtain final product average grain diameter be 740nm barium sulfate.
Embodiment 4
A kind of method for preparing big particle diameter barium sulfate, it comprises the following steps：
1) it is suspension of calcium sulfate of 408g/L to prepare the barium chloride solution and solid content that concentration is 2.5mol/L respectively；
2) suspension of calcium sulfate is put into constant-temperature heating magnetic stirring apparatus, sets bath temperature as 100 DEG C, mixing speed is
25r/min；
3) constant flow pump is utilized, to barium chloride solution, rate of addition 5.86mL/min are added dropwise in suspension of calcium sulfate；
4) stirring reaction is continued after completion of dropping, digestion time is 2h；
5) filter, washed with absolute ethyl alcohol, 110 DEG C drying 3h, obtain final product average grain diameter be 430nm barium sulfate.
In the present invention, Fig. 1 is the XRD spectra of barium sulfate prepared by the inventive method.Fig. 2 is sulphur prepared by the inventive method
Sour barium amplifies 20000 times of SEM figures.Fig. 3 is the SEM figures of 60000 times of barium sulfate method prepared by the inventive method.
By Fig. 1 and standard spectrogram comparative illustration, barium sulfate purity prepared by this method is big compared with high, particle diameter, the grain of barium sulfate
Footpath can reach 850nm, be can be seen that by embodiment 2.
Be can be seen that according to this method with calcium sulfate as raw material by embodiment data and Fig. 2, Fig. 3, big particle diameter can be obtained
Barium sulfate product, and Granularity Distribution is more uniform.
Claims (10)
1. a kind of method for preparing big particle diameter barium sulfate, it is characterized in that comprising the following steps：
1) barium chloride solution and suspension of calcium sulfate are prepared, it is standby；The barium chloride solution concentration is 0.1~2.5mol/L；Institute
The amount ratio for stating material when calcium sulfate mixes with barium chloride is 1:1~2；
2) suspension of calcium sulfate is put into constant-temperature heating magnetic stirring apparatus, design temperature is 25~100 DEG C, opens stirring；
3) using constant flow pump to barium chloride solution is added dropwise in suspension of calcium sulfate；
4) continue stirring reaction after completion of dropping, be aged；
5) filter, wash, dry, get product barium sulfate, the drying temperature is 80-120 DEG C.
2. a kind of method for preparing big particle diameter barium sulfate according to claim 1, it is characterized in that：Step 1) described in sulfuric acid
The solid content of calcium suspension is 68~408g/L.
3. a kind of method for preparing big particle diameter barium sulfate according to claim 1, it is characterized in that：Step 2) described in react
Design temperature is most preferably 50 DEG C.
4. a kind of method for preparing big particle diameter barium sulfate according to claim 1, it is characterized in that：Step 2) described in react
Mixing speed is 5~25r/min.
5. a kind of method for preparing big particle diameter barium sulfate according to claim 1, it is characterized in that：Step 3) described in chlorination
The rate of addition of barium solution is 0.35~6.92mL/min.
6. a kind of method for preparing big particle diameter barium sulfate according to claim 1, it is characterized in that：Step 3) described in sulfuric acid
The amount ratio of material is 1 when calcium mixes with barium chloride:1.2.
7. a kind of method for preparing big particle diameter barium sulfate according to claim 1, it is characterized in that：Step 4) described in be aged
Time is 0.5~4h.
8. a kind of method for preparing big particle diameter barium sulfate according to claim 1, it is characterized in that：Step 5) in, the baking
Dry temperature is 110 DEG C.
9. a kind of method for preparing big particle diameter barium sulfate according to claim 1, it is characterized in that：Step 5) described in dry
Time is 1~4h.
10. a kind of method for preparing big particle diameter barium sulfate according to claim 1, it is characterized in that, including walk in detail below
Suddenly：
1) it is suspension of calcium sulfate of 136g/L to prepare the barium chloride solution and solid content that concentration is 0.5mol/L respectively；
2) suspension of calcium sulfate is put into constant-temperature heating magnetic stirring apparatus, sets bath temperature as 50 DEG C, mixing speed is
12.5r/min；
3) constant flow pump is utilized, to barium chloride solution, rate of addition 1.47mL/min are added dropwise in suspension of calcium sulfate；
4) stirring reaction is continued after completion of dropping, digestion time is 4h；
5) filter, washed with absolute ethyl alcohol, 110 DEG C drying 4h, obtain final product big particle diameter barium sulfate product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201611112002.5A CN106745158B (en) | 2016-12-06 | 2016-12-06 | A method of preparing big partial size barium sulfate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611112002.5A CN106745158B (en) | 2016-12-06 | 2016-12-06 | A method of preparing big partial size barium sulfate |
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| CN106745158A true CN106745158A (en) | 2017-05-31 |
| CN106745158B CN106745158B (en) | 2019-01-15 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4880498A (en) * | 1972-02-01 | 1973-10-27 | ||
| CN101254938A (en) * | 2008-03-31 | 2008-09-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of superfine barium sulfate |
| CN102381724A (en) * | 2010-09-01 | 2012-03-21 | 中国科学院化学研究所 | Preparation method of shape controllable monodisperse barium sulfate crystal particles |
| CN103073042A (en) * | 2013-02-04 | 2013-05-01 | 河北科技大学 | Preparation method of submicron-grade barium sulfate |
| CN103130260A (en) * | 2013-03-19 | 2013-06-05 | 冉金友 | Production method of barium sulfate |
-
2016
- 2016-12-06 CN CN201611112002.5A patent/CN106745158B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4880498A (en) * | 1972-02-01 | 1973-10-27 | ||
| CN101254938A (en) * | 2008-03-31 | 2008-09-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of superfine barium sulfate |
| CN102381724A (en) * | 2010-09-01 | 2012-03-21 | 中国科学院化学研究所 | Preparation method of shape controllable monodisperse barium sulfate crystal particles |
| CN103073042A (en) * | 2013-02-04 | 2013-05-01 | 河北科技大学 | Preparation method of submicron-grade barium sulfate |
| CN103130260A (en) * | 2013-03-19 | 2013-06-05 | 冉金友 | Production method of barium sulfate |
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