CN112624173A - Preparation method of barium sulfate crystal with controllable shape - Google Patents
Preparation method of barium sulfate crystal with controllable shape Download PDFInfo
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- CN112624173A CN112624173A CN202011606298.2A CN202011606298A CN112624173A CN 112624173 A CN112624173 A CN 112624173A CN 202011606298 A CN202011606298 A CN 202011606298A CN 112624173 A CN112624173 A CN 112624173A
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- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 title claims abstract description 236
- 239000013078 crystal Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 102
- 239000000725 suspension Substances 0.000 claims abstract description 34
- 239000002245 particle Substances 0.000 claims abstract description 21
- 239000011259 mixed solution Substances 0.000 claims description 41
- 239000000243 solution Substances 0.000 claims description 37
- 159000000009 barium salts Chemical class 0.000 claims description 26
- 239000012266 salt solution Substances 0.000 claims description 25
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 21
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 238000005649 metathesis reaction Methods 0.000 claims description 7
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 6
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims description 6
- 229910001626 barium chloride Inorganic materials 0.000 claims description 6
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 6
- 235000011152 sodium sulphate Nutrition 0.000 claims description 6
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 3
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 claims description 3
- 239000000835 fiber Substances 0.000 claims description 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 3
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 230000006698 induction Effects 0.000 abstract description 5
- 230000001105 regulatory effect Effects 0.000 abstract description 5
- 238000000034 method Methods 0.000 description 14
- 238000000354 decomposition reaction Methods 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 229910017053 inorganic salt Inorganic materials 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 230000032683 aging Effects 0.000 description 4
- 230000033228 biological regulation Effects 0.000 description 4
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 4
- MXJDQIWBHIXNRE-UHFFFAOYSA-B C(CC(O)(C(=O)[O-])CC(=O)[O-])(=O)[O-].[C+4].C(CC(O)(C(=O)[O-])CC(=O)[O-])(=O)[O-].C(CC(O)(C(=O)[O-])CC(=O)[O-])(=O)[O-].C(CC(O)(C(=O)[O-])CC(=O)[O-])(=O)[O-].[C+4].[C+4] Chemical class C(CC(O)(C(=O)[O-])CC(=O)[O-])(=O)[O-].[C+4].C(CC(O)(C(=O)[O-])CC(=O)[O-])(=O)[O-].C(CC(O)(C(=O)[O-])CC(=O)[O-])(=O)[O-].C(CC(O)(C(=O)[O-])CC(=O)[O-])(=O)[O-].[C+4].[C+4] MXJDQIWBHIXNRE-UHFFFAOYSA-B 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 238000010907 mechanical stirring Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
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- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- NHYZIQDLKOJOSI-UHFFFAOYSA-N [C].OC(=O)CC(O)(C(O)=O)CC(O)=O Chemical class [C].OC(=O)CC(O)(C(O)=O)CC(O)=O NHYZIQDLKOJOSI-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 238000007602 hot air drying Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
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Images
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 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 relates to the technical field of barium sulfate crystal preparation, and provides a preparation method of a barium sulfate crystal with controllable morphology. According to the invention, the obtained amorphous barium sulfate suspension is mixed with the carbon quantum dots, and the strength of the barium sulfate precipitation induction effect is controlled by adjusting the using amount of the carbon quantum dots, so that the shape of the barium sulfate crystal can be regulated. Experimental results show that the morphology of the barium sulfate crystal obtained by the preparation method provided by the invention changes from rectangular sheet shape to elliptical shape, fleshy shape, dense fleshy shape and large particles without fixed shapes along with the change of the concentration of the carbon quantum dots in the amorphous barium sulfate suspension, so that the control of the morphology of the barium sulfate crystal is realized.
Description
Technical Field
The invention relates to the technical field of barium sulfate crystal preparation, in particular to a preparation method of a barium sulfate crystal with controllable morphology.
Background
The inorganic salt industry has promoted the development of modern industry and is widely applied to petrochemical industry, building materials, functional materials and environmental protection. With the continuous development of modern chemical industry, stricter requirements are put forward on the production process, product functionalization and product diversity of inorganic salt. The crystal morphology not only affects the physical properties such as mechanical strength and density of the crystal, but also affects the chemical properties such as thermal stability and water absorption of the material to a certain extent, and further affects other subsequent production processes. For example, crystals with larger particle diameter and uniform particle size distribution are easier to filter and dry than crystals with smaller particle diameter and wider particle size distribution range, and the product quality is better. In food processing, additives with different particle sizes and different crystal shapes also affect the eating mouthfeel.
The crystallization process of inorganic salts is also complex, and not only involves thermodynamic equilibrium of mass transfer and heat transfer, but also involves dynamic processes such as adsorption and diffusion. At present, the research on the morphology of inorganic salt crystals in China is still in the beginning stage, and the efficiency of regulating and controlling the morphology of inorganic salt is low. For example, chinese patent CN102381724A discloses a method for preparing monodisperse barium sulfate crystal particles with controllable morphology, which can regulate and control the morphology of barium sulfate crystals, but the technical scheme thereof requires to prepare an organic solution of a polymer first, and realizes the regulation and control of the morphology of barium sulfate crystals by adjusting the concentration and pH of the polymer solution, and this method requires the use of an organic reagent, which is not environment-friendly; and 5-120 h of aging time is needed, so that the efficiency is low. For another example, chinese patent CN103204532A discloses a method for preparing spinous spherical barium sulfate particles with aqueous hydrogen peroxide as a structure regulator, which regulates the morphology of barium sulfate particles through the regulation effect of hydrogen peroxide, but also requires 24-400 hours of aging time to realize the regulation process. Therefore, the defect of low efficiency in the prior art for regulating and controlling the crystal morphology of the inorganic salt exists.
Therefore, a method for preparing barium sulfate crystals with high efficiency and controllable morphology is needed.
Disclosure of Invention
The invention aims to provide a preparation method of a barium sulfate crystal with controllable morphology, which can regulate the morphology of the barium sulfate crystal, does not need long-time aging and has higher efficiency.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a barium sulfate crystal with controllable morphology, which comprises the following steps:
(1) mixing the barium salt solution and the sulfate solution, and carrying out double decomposition reaction to obtain amorphous barium sulfate suspension;
(2) mixing the amorphous barium sulfate suspension obtained in the step (1) with carbon quantum dots to obtain a mixed solution; the concentration of the carbon quantum dots in the mixed solution is 0-20 mg/L;
(3) and (3) drying the mixed solution obtained in the step (2) to obtain barium sulfate powder.
Preferably, the barium salt in the barium salt solution comprises one or more of barium chloride, barium nitrate and barium acetate.
Preferably, the concentration of the barium salt solution in the step (1) is 0.5-1 mol/L.
Preferably, the sulfate in the sulfate solution in step (1) includes one or more of sodium sulfate, aluminum sulfate and magnesium sulfate.
Preferably, the concentration of the sulfate solution in the step (1) is 0.2-0.5 mol/L.
Preferably, in the step (1), the mixed solution obtained by mixing the barium salt solution and the sulfate solution contains Ba2+With SO4 2-The ratio of the amounts of substances (1): 1-1: 2.
preferably, the time of the double decomposition reaction in the step (1) is 5-10 h.
Preferably, when the concentration of the carbon quantum dots in the mixed solution obtained in the step (2) is greater than or equal to 0mg/L and less than 4mg/L, the barium sulfate crystal is rectangular and flaky; when the concentration of the carbon quantum dots in the mixed solution is more than or equal to 4mg/L and less than 8mg/L, the barium sulfate crystal is elliptical in shape; when the concentration of the carbon quantum dots in the mixed solution is more than or equal to 8mg/L and less than or equal to 12mg/L, the barium sulfate crystal is fleshy; when the concentration of the carbon quantum dots in the mixed solution is more than 12mg/L and less than or equal to 16mg/L, the barium sulfate crystal is dense and fleshy; when the concentration of the carbon quantum dots in the mixed solution is more than 16mg/L and less than or equal to 20mg/L, the shape of the barium sulfate crystal is large particles without fixed shapes.
Preferably, the carbon quantum dots in step (2) include carbon quantum dots prepared from citric acid, carbon quantum dots prepared from pulp fibers, or carbon quantum dots prepared from plant ash.
Preferably, the drying temperature in the step (3) is 50-80 ℃, and the drying time is 4-8 h.
The invention provides a preparation method of a barium sulfate crystal with controllable morphology, which comprises the following steps: mixing the barium salt solution and the sulfate solution, and carrying out double decomposition reaction to obtain amorphous barium sulfate suspension; mixing the obtained amorphous barium sulfate suspension with carbon quantum dots to obtain a mixed solution; the concentration of the carbon quantum dots in the mixed solution is 0-20 mg/L; and drying the obtained mixed solution to obtain barium sulfate powder. Firstly synthesizing amorphous barium sulfate suspension, then adding carbon quantum dots into the suspension containing barium sulfate, and changing the morphology of barium sulfate crystals in the drying process by utilizing the induction effect of the carbon quantum dots on barium sulfate precipitation; the amorphous barium sulfate suspension obtained is mixed with the carbon quantum dots, and the dosage of the carbon quantum dots in the barium sulfate precipitation suspension is adjusted, so that the strength of the carbon quantum dots on the barium sulfate precipitation induction effect is adjusted, and the shape of barium sulfate crystals can be adjusted. Experimental results show that the morphology of the barium sulfate crystal obtained by the preparation method provided by the invention changes from rectangular sheet shape to elliptical shape, fleshy shape, dense fleshy shape and large particles without fixed shapes along with the change of the concentration of the carbon quantum dots in the amorphous barium sulfate suspension, so that the control of the morphology of the barium sulfate crystal is realized.
The preparation method of the barium sulfate crystal with controllable morphology, provided by the invention, is simple to operate, is efficient, and is suitable for large-scale production.
Drawings
FIG. 1 is a photograph of carbon quantum dots provided by the present invention at different concentrations;
FIG. 2 is an SEM photograph of barium sulfate powder prepared in example 1 of the present invention;
FIG. 3 is an SEM photograph of barium sulfate powder prepared in example 2 of the present invention;
FIG. 4 is an SEM photograph of barium sulfate powder prepared in example 3 of the present invention;
FIG. 5 is an SEM photograph of barium sulfate powder prepared in example 4 of the present invention;
FIG. 6 is an SEM photograph of barium sulfate powder prepared in example 5 of the present invention;
FIG. 7 is an SEM photograph of barium sulfate powder prepared in example 6 of the present invention.
Detailed Description
The invention provides a preparation method of a barium sulfate crystal with controllable morphology, which comprises the following steps:
(1) mixing the barium salt solution and the sulfate solution, and carrying out double decomposition reaction to obtain amorphous barium sulfate suspension;
(2) mixing the amorphous barium sulfate suspension obtained in the step (1) with carbon quantum dots to obtain a mixed solution; the concentration of the carbon quantum dots in the mixed solution is 0-20 mg/L;
(3) and (3) drying the mixed solution obtained in the step (2) to obtain barium sulfate powder.
The method mixes the barium salt solution and the sulfate solution to carry out double decomposition reaction, and obtains the amorphous barium sulfate suspension.
In the present invention, the barium salt in the barium salt solution preferably includes one or more of barium chloride, barium nitrate and barium acetate, and more preferably barium chloride. The source of the barium salt is not particularly limited in the present invention, and commercially available products well known to those skilled in the art may be used.
In the present invention, the concentration of the barium salt solution is preferably 0.5 to 1mol/L, and more preferably 0.6 to 0.8 mol/L. In the present invention, when the concentration of the barium salt solution is within the above range, the metathesis reaction is more advantageously carried out.
In the present invention, the sulfate in the sulfate solution preferably includes one or more of sodium sulfate, aluminum sulfate, and magnesium sulfate, and more preferably sodium sulfate. The source of the sulfate salt is not particularly limited in the present invention, and commercially available products known to those skilled in the art may be used.
In the invention, the concentration of the sulfate solution is preferably 0.2-0.5 mol/L, and more preferably 0.3-0.4 mol/L. In the present invention, when the concentration of the sulfate solution is within the above range, the metathesis reaction is more advantageously carried out.
In the invention, Ba in the mixed solution obtained by mixing the barium salt solution and the sulfate solution2+With SO4 2-The ratio of the amounts of substances (a) to (b) is preferably 1: 1-1: 2, more preferably 1: 1-1: 1.5. in the invention, Ba in the mixed solution obtained by mixing the barium salt solution and the sulfate solution2+With SO4 2-When the amount ratio of the substance(s) is in the above range, the metathesis reaction can be sufficiently carried out.
The operation mode of mixing the barium salt solution and the sulfate solution is not particularly limited in the invention, and the solution mixing mode known to those skilled in the art can be adopted. In the present invention, the mixing of the barium salt solution and the sulfate salt solution is preferably performed under mechanical stirring. The rotation speed of the mechanical stirring is not particularly limited, and the barium sulfate generated after the barium salt solution and the sulfate solution react can be dispersed. In the invention, the mechanical stirring can disperse the barium sulfate generated after the reaction, prevent the barium sulfate from precipitating and is beneficial to promoting the barium salt solution to fully react with the sulfate solution.
In the present invention, the time of the double decomposition reaction is preferably 5 to 10 hours, and more preferably 6 to 8 hours. In the present invention, when the time of the metathesis reaction is within the above range, Ba in the barium salt solution and the sulfate salt solution can be ensured2+With SO4 2-And (4) fully reacting.
In the present invention, the metathesis reaction is preferably carried out at room temperature, and more preferably at 20 to 30 ℃. In the present invention, Ba in the barium salt solution and the sulfate salt solution2+With SO4 2-Can generate double decomposition reaction at room temperatureA barium sulfate precipitate is formed.
After the amorphous barium sulfate suspension is obtained, the amorphous barium sulfate suspension is mixed with carbon quantum dots to obtain a mixed solution.
In the present invention, the carbon quantum dots preferably include carbon quantum dots prepared from citric acid, carbon quantum dots prepared from pulp fibers, or carbon quantum dots prepared from plant ash, and more preferably carbon quantum dots prepared from citric acid. The method for preparing the carbon quantum dots is not particularly limited in the present invention, and a method for preparing the carbon quantum dots, which is well known to those skilled in the art, may be used. In the invention, the method for preparing the carbon quantum dots by using the citric acid is preferably a high-temperature pyrolysis method.
In the invention, the concentration of the carbon quantum dots in the mixed solution is 0-20 mg/L, preferably 0-18 mg/L. In the invention, the carbon quantum dots can induce barium sulfate precipitation, and the shape of the barium sulfate crystal can be regulated and controlled in the subsequent drying process.
In the invention, when the concentration of the carbon quantum dots in the mixed solution is preferably more than or equal to 0mg/L and less than 4mg/L, the barium sulfate crystal is rectangular and flaky; when the concentration of the carbon quantum dots in the mixed solution is preferably more than or equal to 4mg/L and less than 8mg/L, the barium sulfate crystal is elliptical in shape; when the concentration of the carbon quantum dots in the mixed solution is preferably more than or equal to 8mg/L and less than or equal to 12mg/L, the barium sulfate crystal is fleshy; when the concentration of the carbon quantum dots in the mixed solution is preferably more than 12mg/L and less than or equal to 16mg/L, the barium sulfate crystal is dense and fleshy; when the concentration of the carbon quantum dots in the mixed solution is preferably more than 16mg/L and less than or equal to 20mg/L, the morphology of the barium sulfate crystal is large particles without fixed shapes. In the present invention, when the concentration of the carbon quantum dots in the mixed solution is in the above range, the morphology of the crystal of barium sulfate changes from a rectangular sheet to a large particle without a fixed shape as the concentration of the carbon quantum dots increases.
The operation mode of mixing the amorphous barium sulfate suspension and the carbon quantum dots is not particularly limited in the invention, and a solid-liquid mixing mode well known to those skilled in the art can be adopted.
In the present invention, the carbon quantum dots are preferably added in the form of a carbon quantum dot solution. The concentration of the carbon quantum dot solution is not particularly limited, and the concentration of the carbon quantum dots in the mixed solution obtained by mixing the amorphous barium sulfate suspension and the carbon quantum dot solution can be 0-20 mg/L. The method for preparing the carbon quantum dot solution is not particularly limited, and the preparation method known to those skilled in the art can be adopted. In the present invention, the preparation method of the carbon quantum dot solution is preferably to disperse the carbon quantum dots in water under ultrasound. The power of the ultrasound is not particularly limited, and the carbon quantum dots can be dispersed in water. In the present invention, the carbon quantum dots are mixed with the amorphous barium sulfate suspension as a carbon quantum dot solution, and the carbon quantum dots can be promoted to be more rapidly and uniformly dispersed in the mixed solution of the amorphous barium sulfate suspension and the carbon quantum dot solution.
In the present invention, the mixing of the amorphous barium sulfate suspension and the carbon quantum dots is preferably performed under stirring conditions. The stirring speed is not specially limited, and the carbon quantum dots and the barium sulfate can be uniformly dispersed in the mixed solution.
In the invention, the time for mixing the amorphous barium sulfate suspension and the carbon quantum dots is preferably 30-60 min, and more preferably 40-45 min. In the invention, when the mixing time is in the range, the carbon quantum dots and the barium sulfate can be fully mixed in the mixed solution, so that the carbon quantum dots and the barium sulfate are fully contacted and attached to the surface of the barium sulfate precipitate, thereby being beneficial to inducing the barium sulfate crystal in the subsequent drying process and changing the appearance of the barium sulfate crystal.
After the mixed solution is obtained, the mixed solution is dried to obtain barium sulfate powder.
In the invention, the drying temperature is preferably 50-80 ℃; more preferably 60-65 ℃; the drying time is preferably 4-7 hours, and more preferably 4.5-6 hours. In the invention, the drying can remove moisture on the surface of the barium sulfate precipitate on one hand; on the other hand, the shape of the barium sulfate crystal can be regulated and controlled by utilizing the induction effect of carbon quantum dots adsorbed on the surface of the barium sulfate precipitate on the barium sulfate crystal under the action of heat. In the present invention, when the drying temperature and time are within the above ranges, amorphous barium sulfate can be sufficiently converted into barium sulfate crystals. The drying apparatus of the present invention is not particularly limited, and a drying apparatus known to those skilled in the art may be used. In the present invention, the drying means is preferably an electric hot air drying oven.
In the present invention, it is preferable that the mixed solution is sequentially filtered and washed before drying. The operation manner of the filtration and washing is not particularly limited in the present invention, and the operation manner of the filtration and washing known to those skilled in the art may be adopted. In the present invention, the filtration is preferably suction filtration. In the present invention, the time for the suction filtration is preferably 1 hour. In the present invention, the washed solvent is preferably distilled water; the washing is preferably 3 times with distilled water. In the present invention, the filtration and washing can remove carbon quantum dots and solvent that are not attached to the surface of the barium sulfate precipitate.
The method firstly synthesizes amorphous barium sulfate suspension, then adds carbon quantum dots into the amorphous barium sulfate suspension, and changes the morphology of barium sulfate crystals in the drying process by utilizing the induction effect of the carbon quantum dots on barium sulfate precipitation.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Mixing and stirring 50mL of 0.7mol/L barium chloride solution and 50mL of 1.4mol/L sodium sulfate solution for 3h to obtain amorphous barium sulfate suspension; (Ba in barium chloride solution and sodium sulfate solution2+With SO4 2-The ratio of the amounts of substances (1): 2)
(2) and (2) mixing 10mL of the amorphous barium sulfate suspension obtained in the step (1) with 0g of carbon quantum dots to ensure that the concentration of the carbon quantum dots in the mixed system is 0g/mL, wherein the mixing time is 40min, filtering the obtained system, washing the filtered system with distilled water for 3 times, and drying the washed solid at 70 ℃ for 12h to obtain barium sulfate powder.
The carbon quantum dots adopted in the embodiment of the invention are citric acid carbon quantum dots obtained by a conventional method, and the photos of the carbon quantum dots at different concentrations are shown in fig. 1.
In FIG. 1, the concentrations of the carbon quantum dot solutions corresponding to a to e are 4g/mL, 8g/mL, 12g/mL, 14g/mL, and 16g/mL in this order. As can be seen from FIG. 1, the prepared carbon citrate quantum dots have good water solubility; and the color of the carbon quantum dot solution is gradually deepened along with the increase of the concentration of the carbon quantum dots.
The barium sulfate powder prepared in example 1 was tested using a scanning electron microscope, and the SEM image of the barium sulfate powder is shown in fig. 2.
As can be seen from fig. 2, the particles of barium sulfate powder appear to be uniform rectangular sheets without the addition of carbon quantum dots.
Example 2
The difference from example 1 is that 20mL of the amorphous barium sulfate suspension obtained in step (1) is mixed with 80g of carbon quantum dots in step (2) so that the concentration of the carbon quantum dots in the mixed system is 4g/mL, and the rest of the steps are the same as example 1.
The barium sulfate powder prepared in example 2 was tested using a scanning electron microscope, and the SEM image of the barium sulfate powder is shown in fig. 3.
As can be seen from fig. 3, when the concentration of the carbon quantum dots in the mixed system is 4g/mL, the barium sulfate powder particles have an oval shape with openings at both ends, which are about several tens of micrometers in length.
Example 3
The difference from example 1 is that 10mL of the amorphous barium sulfate suspension obtained in step (1) is mixed with 80g of carbon quantum dots in step (2) so that the concentration of the carbon quantum dots in the mixed system is 8g/mL, and the rest of the steps are the same as example 1.
The barium sulfate powder prepared in example 3 was tested using a scanning electron microscope, and the SEM image of the barium sulfate powder is shown in fig. 4.
As can be seen from fig. 4, at a carbon quantum dot concentration of 8g/mL in the mixed system, the particles of barium sulfate powder appeared to be fleshy with a size of about ten and several microns.
Example 4
The difference from example 1 is that 10mL of the amorphous barium sulfate suspension obtained in step (1) is mixed with 120g of carbon quantum dots in step (2) so that the concentration of the carbon quantum dots in the mixed system is 12g/mL, and the rest of the steps are the same as example 1.
The barium sulfate powder prepared in example 4 was tested using a scanning electron microscope, and the SEM image of the barium sulfate powder is shown in fig. 5.
As can be seen from fig. 5, when the concentration of the carbon quantum dots in the mixed system was 12g/mL, the barium sulfate powder particles were fleshy with a size of about ten and several micrometers, and the fleshy leaves increased and became thick.
Example 5
The difference from example 1 is that 10mL of the amorphous barium sulfate suspension obtained in step (1) is mixed with 160g of carbon quantum dots in step (2) so that the concentration of the carbon quantum dots in the mixed system is 16g/mL, and the rest of the steps are the same as example 1.
The barium sulfate powder prepared in example 5 was tested using a scanning electron microscope, and the SEM image of the barium sulfate powder is shown in fig. 6.
As can be seen from fig. 6, when the concentration of carbon quantum dots in the mixed system was 16g/mL, the barium sulfate powder particles were fleshy with a size of about ten and several micrometers, and the fleshy leaves increased and became thick.
Example 6
The difference from example 1 is that 10mL of the amorphous barium sulfate suspension obtained in step (1) is mixed with 200g of carbon quantum dots in step (2) so that the concentration of the carbon quantum dots in the mixed system is 20g/mL, and the rest of the steps are the same as example 1.
The barium sulfate powder prepared in example 6 was tested using a scanning electron microscope, and the SEM image of the barium sulfate powder is shown in fig. 7.
As can be seen from FIG. 7, when the concentration of the carbon quantum dots in the mixed system is 20g/mL, the particles of the barium sulfate powder have large particles without fixed morphology.
As can be seen from fig. 2 to 7, the morphology of the barium sulfate crystal can be changed by using the carbon quantum dots, and when the addition amount of the carbon citrate quantum dots is different, the morphology of the carbon citrate quantum dots is greatly changed, so that the morphology of the barium sulfate crystal can be controlled by controlling the amount of the carbon quantum dots in the barium sulfate precipitation suspension.
In addition, the preparation method provided by the invention is simple and efficient to operate, can realize the regulation and control of the barium sulfate crystal morphology without a long-time aging process, and is suitable for large-scale production.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
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| CN116023818A (en) * | 2022-12-30 | 2023-04-28 | 佛山安亿纳米材料有限公司 | Core-shell structured barium sulfate composite material and preparation method and application thereof |
| CN116179195A (en) * | 2023-02-09 | 2023-05-30 | 佛山安亿纳米材料有限公司 | Quantum dot composite material and preparation method and application thereof |
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