CN110330046A - The technique that nano barium sulfate is prepared by microreactor as raw material using barium carbonate - Google Patents
The technique that nano barium sulfate is prepared by microreactor as raw material using barium carbonate Download PDFInfo
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- CN110330046A CN110330046A CN201910426174.7A CN201910426174A CN110330046A CN 110330046 A CN110330046 A CN 110330046A CN 201910426174 A CN201910426174 A CN 201910426174A CN 110330046 A CN110330046 A CN 110330046A
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- barium sulfate
- microreactor
- barium
- barium carbonate
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Organic Chemistry (AREA)
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- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses the techniques for preparing nano barium sulfate by microreactor as raw material using barium carbonate comprising following primary raw material: barium carbonate and sulfuric acid.The technique prepares certain density barium carbonate suspension and sulfuric acid solution first, then make barium carbonate suspension and dilute sulfuric acid are efficient, are sufficiently mixed simultaneously precipitation reaction barium sulfate suspension is made by microreactor, obtained barium sulfate suspension is stirred, aging in aging kettle, is finally filtered, washed, is dried to obtain barium sulfate finished product.It is smaller using the obtained barium sulfate material particle size of the present invention and particle diameter distribution is relatively narrow, it can be evenly dispersed in aqueous solution, it is hardly settled in for 24 hours, compared with traditional preparation method, this technique can more accurately control the various conditions in production, realize fine, quick, controllable production mode.
Description
Technical field
It is received the present invention relates to barium sulfate field of material technology, in particular to using barium carbonate as raw material by microreactor preparation
The technique of nano-barium sulfate.
Background technique
Barium sulfate is a kind of important inorganic chemical industry material, is widely used in the industries such as filler, ceramics.Nano barium sulfate is made
For one of the major product of barium compound series of products, it is widely used in pigment, coating, ink, paint, rubber, plastics electric power storage
The raw materials such as pond and filler.Since nano barium sulfate material has its excellent performance, countries in the world are to barium sulphate nano material
Preparation method and application studied.
Currently, the traditional preparation methods of barium sulfate material have: solid-phase synthesis, gas phase synthesis method, sol-gel method, liquid
Phase coprecipitation.Wherein liquid-phase coprecipitation is used widely since technique is relatively simple, reaction condition is relatively mild.It is main
Processing step is that one of reaction solution is added in stirred tank, and another reaction solution is added dropwise under high speed agitation, and
It reacts at a certain temperature, finally filters, is dry, barium sulfate product is prepared.Since the method two-phase mixtures intensity is poor,
It is difficult to meet the needs of rapid precipitation reaction, therefore obtained barium sulfate grain growth is not easy to control, grain graininess is big, partial size point
Cloth is wider, and pattern is irregular, and the stability between batch is poor.In addition, the barium sulfate dispersibility that traditional handicraft obtains is poor, very
Hardly possible is used for the dispersing agent of colored pigment, and application is restricted.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the above technological deficiency, provides and pass through micro- reaction by raw material of barium carbonate
Device prepares the technique of nano barium sulfate, compensates for the defect in traditional barium sulfate preparation process, changes the performance of barium sulfate,
Obtained the preferable nano barium sulfate material of uniform particle diameter, dispersibility, can be evenly dispersed in aqueous solution, for 24 hours in almost
It does not settle, and the technique can more accurately control the various conditions in production, realize fine, quick, controllable production
Mode.
In order to achieve the above object of the invention, the technical solution adopted by the present invention are as follows: pass through micro- reaction by raw material of barium carbonate
The technique that device prepares nano barium sulfate, comprising the following steps:
(1) preparation of barium sulfate suspension: certain density barium carbonate suspension and aqueous sulfuric acid are prepared first, in carbon
Nitric acid is added in sour barium suspension as catalyst, then barium carbonate suspension is mobile phase, and sulfuric acid solution is dispersed phase, is passed through
Film disperses microreactor and uniformly, quickly mixes, and reacts under certain temperature and pH, and barium sulfate suspension is prepared；
(2) aging of barium sulfate suspension: the barium sulfate suspension being prepared in step (1) is put into aging kettle,
Continuation is stirred at a certain temperature, and aging terminates after a certain period of time；
(3) finished product is made: the suspension after aging in step (2) being centrifugated, and with pure water, finally
It is dry, obtain barium sulfate finished material.
Further, the concentration of barium carbonate aqueous solution is 0.5~1.5mol/L in step (1), and the concentration of sulfuric acid solution is
0.5~1.5mol/L；Barium carbonate rate of circulating flow is 200~250ml/min, and the flow velocity of sulfuric acid solution is less than 5ml/min.
Further, the temperature of two phase reaction is 80~90 DEG C in step (1), and recycling the pH in flask is 7.0~1.0.
Further, the temperature of ageing process is room temperature in step (2), and the time of ageing process is 2h.
Further, it should be washed in step (3) to conductivity in 50 μ S/m hereinafter, dry temperature is 100~120 DEG C.
Further, dispersion membrane material is 316L in the film dispersion microreactor, and the aperture of dispersion membrane is 5~100 μm.
The invention has the benefit that the present invention is using barium carbonate and sulfuric acid as raw material, the generation of no coupling product, avoid because
By-product pollution on the environment, and reduce the cost of subsequent wastewater treatment；For the technique, equipment is dispersed micro- using film
Reactor, dispersed phase sulfuric acid is divided into uniform droplet after crossing film, and is uniformly dispersed in barium carbonate suspension, increases
The contact area of two-phase, enhances mass transport process, to obtain uniform particle diameter, the preferable nanoscale barium sulfate of dispersibility；And
And the various conditions in production can be accurately controlled using the technique, realize fine, quick, controllable production mode.
Detailed description of the invention
Barium sulfate material particle size in Fig. 1 embodiment one analyzes result table figure.
Barium sulfate material particle size in Fig. 2 embodiment one analyzes result chromatogram.
Barium sulfate material particle size in Fig. 3 embodiment two analyzes result table figure.
Barium sulfate material particle size in Fig. 4 embodiment two analyzes result chromatogram.
Barium sulfate material particle size in Fig. 5 embodiment three analyzes result table figure.
Barium sulfate material particle size in Fig. 6 embodiment three analyzes result chromatogram.
Barium sulfate material particle size in Fig. 7 example IV analyzes result table figure.
Barium sulfate material particle size in Fig. 8 example IV analyzes result chromatogram.
Specific embodiment
In order that the present invention can be more clearly and readily understood, below technical solution in the embodiment of the present invention into
Row clearly and completely describes.
Embodiment one
The technique that nano barium sulfate is prepared by microreactor as raw material using barium carbonate, comprising the following steps:
1) dilution heat of sulfuric acid that the barium carbonate suspension and concentration that compound concentration is 1.0mol/L are 0.5mol/L；
2) barium carbonate suspension is recycled as mobile phase by flask-microreactor-flask with the flow velocity of 250ml/min
Flowing, dilute sulfuric acid pass through the 316L film and carbonic acid in film dispersion microreactor as dispersed phase, with the flow velocity not higher than 5ml/min
The mixing of barium suspension, and precipitation reaction occurs at 80 DEG C, microreactor exports pH control 7.0~1.0.
3) the barium sulfate suspension after reacting is put in a stirring kettle, continues to stir aging 2h at normal temperature.
4) centrifugal filtration after aging, washing is to conductivity in 50 μ S/m hereinafter, being finally dried to obtain sulphur at 120 DEG C
Sour barium finished product.
According to above-mentioned processing step, barium sulfate material particle size analysis result as shown in Figure 1 and Figure 2 is obtained.
Embodiment two
The technique that nano barium sulfate is prepared by microreactor as raw material using barium carbonate, comprising the following steps:
1) dilution heat of sulfuric acid that the barium carbonate suspension and concentration that compound concentration is 1.0mol/L are 1.0mol/L；
2) barium carbonate suspension is recycled as mobile phase by flask-microreactor-flask with the flow velocity of 250ml/min
Flowing, dilute sulfuric acid pass through the 316L film and carbonic acid in film dispersion microreactor as dispersed phase, with the flow velocity not higher than 5ml/min
The mixing of barium suspension, and precipitation reaction occurs at 80 DEG C, microreactor exports pH control 7.0~1.0.
3) the barium sulfate suspension after reacting is put in a stirring kettle, continues to stir aging 2h at normal temperature.
4) centrifugal filtration after aging, washing is to conductivity in 50 μ S/m hereinafter, being finally dried to obtain sulphur at 120 DEG C
Sour barium finished product.
According to above-mentioned processing step, barium sulfate material particle size analysis result as shown in Figure 3, Figure 4 is obtained.
Embodiment three
A kind of microreactor prepares the new process of polymolecularity barium sulfate material, comprising the following steps:
1) dilution heat of sulfuric acid that the barium carbonate suspension and concentration that compound concentration is 1.0mol/L are 1.0mol/L；
2) barium carbonate suspension is recycled as mobile phase by flask-microreactor-flask with the flow velocity of 200ml/min
Flowing, dilute sulfuric acid pass through the 316L film and carbonic acid in film dispersion microreactor as dispersed phase, with the flow velocity not higher than 5ml/min
The mixing of barium suspension, and precipitation reaction occurs at 80 DEG C, microreactor exports pH control 7.0~1.0.
3) the barium sulfate suspension after reacting is put in a stirring kettle, continues to stir aging 2h at normal temperature.
4) centrifugal filtration after aging, washing is to conductivity in 50 μ S/m hereinafter, being finally dried to obtain sulphur at 120 DEG C
Sour barium finished product.
According to above-mentioned processing step, barium sulfate material particle size analysis result as shown in Figure 5, Figure 6 is obtained.
Example IV
A kind of microreactor prepares the new process of polymolecularity barium sulfate material, comprising the following steps:
1) dilution heat of sulfuric acid that the barium carbonate suspension and concentration that compound concentration is 0.5mol/L are 0.5mol/L；
2) barium carbonate suspension is recycled as mobile phase by flask-microreactor-flask with the flow velocity of 200ml/min
Flowing, dilute sulfuric acid pass through the 316L film and carbonic acid in film dispersion microreactor as dispersed phase, with the flow velocity not higher than 5ml/min
The mixing of barium suspension, and precipitation reaction occurs at 80 DEG C, microreactor exports pH control 7.0~1.0.
3) the barium sulfate suspension after reacting is put in a stirring kettle, continues to stir aging 2h at normal temperature.
4) centrifugal filtration after aging, washing is to conductivity in 50 μ S/m hereinafter, being finally dried to obtain sulphur at 120 DEG C
Sour barium finished product.
According to above-mentioned processing step, barium sulfate material particle size analysis result as shown in Figure 7, Figure 8 is obtained.
The present invention and its embodiments have been described above, this description is no restricted, only reality of the invention
One of mode is applied, actual embodiment is not limited thereto.All in all if those skilled in the art are opened by it
Show, without departing from the spirit of the invention, not inventively design embodiment similar with the technical solution,
It is within the scope of protection of the invention.
Claims (7)
1. the technique for preparing nano barium sulfate by microreactor as raw material using barium carbonate, it is characterised in that: the following steps are included:
(1) preparation of barium sulfate suspension: certain density barium carbonate suspension and aqueous sulfuric acid are prepared first, in barium carbonate
The catalyst of certain mass ratio is added in suspension, then barium carbonate suspension is mobile phase, and sulfuric acid solution is dispersed phase, is passed through
Film disperses microreactor and uniformly, quickly mixes, and reacts under certain temperature and pH, and barium sulfate suspension is prepared；
(2) aging of barium sulfate suspension: being put into the barium sulfate being prepared in step (1) is suspended in aging kettle, continues to exist
It is stirred at a temperature of certain, aging terminates after a certain period of time；
(3) finished product is made: the suspension after aging in step (2) being centrifugated, and with pure water, finally does
It is dry, obtain barium sulfate finished material.
2. the technique according to claim 1 for preparing nano barium sulfate by microreactor using barium carbonate as raw material, special
Sign is: the concentration of barium carbonate aqueous solution is 0.5~1.5mol/L in step (1), the concentration of sulfuric acid solution is 0.5~
1.5mol/L；Barium carbonate rate of circulating flow is 200~250ml/min, and the flow velocity of sulfuric acid solution is less than 5ml/min.
3. the technique according to claim 1 for preparing nano barium sulfate by microreactor using barium carbonate as raw material, special
Sign is: the temperature of two phase reaction is 80~90 DEG C in step (1), and recycling the pH in flask is 7.0~1.0.
4. the technique according to claim 1 for preparing nano barium sulfate by microreactor using barium carbonate as raw material, special
Sign is: the catalyst being added in step (1) is nitric acid, and additional proportion is the 5% of barium carbonate quality.
5. the technique according to claim 1 for preparing nano barium sulfate by microreactor using barium carbonate as raw material, special
Sign is: the temperature of ageing process is room temperature in step (2), and the time of ageing process is 2h.
6. the technique according to claim 1 for preparing nano barium sulfate by microreactor using barium carbonate as raw material, special
Sign is: should be washed in step (3) to conductivity in 50 μ S/m hereinafter, dry temperature is 100~120 DEG C.
7. the technique according to claim 1 for preparing nano barium sulfate by microreactor using barium carbonate as raw material, special
Sign is: the dispersion membrane material in the film dispersion microreactor is 316L, and the aperture of dispersion membrane is 5~100 μm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113683840A (en) * | 2021-08-19 | 2021-11-23 | 云浮鸿志新材料有限公司 | Novel modified plastic and preparation method thereof |
| CN114316655A (en) * | 2022-01-17 | 2022-04-12 | 山东金利特新材料有限责任公司 | Preparation process and application of graphene oxide/nano barium sulfate composite material |
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| CN113683840A (en) * | 2021-08-19 | 2021-11-23 | 云浮鸿志新材料有限公司 | Novel modified plastic and preparation method thereof |
| CN114316655A (en) * | 2022-01-17 | 2022-04-12 | 山东金利特新材料有限责任公司 | Preparation process and application of graphene oxide/nano barium sulfate composite material |
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Application publication date: 20191015 |