CN111484061B - Preparation method of cubic ultrafine calcium carbonate - Google Patents
Preparation method of cubic ultrafine calcium carbonate Download PDFInfo
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- CN111484061B CN111484061B CN202010433902.XA CN202010433902A CN111484061B CN 111484061 B CN111484061 B CN 111484061B CN 202010433902 A CN202010433902 A CN 202010433902A CN 111484061 B CN111484061 B CN 111484061B
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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
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
- C01F11/183—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds the additive being an organic compound
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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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/38—Particle morphology extending in three dimensions cube-like
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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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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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
Abstract
The invention discloses a preparation method of cubic ultrafine calcium carbonate, which comprises the following steps: a. uniformly mixing lauryl alcohol polyoxyethylene polyoxypropylene ether and alcohol, adding an oil phase, mixing, and adding a calcium salt solution to obtain a calcium salt microemulsion; b. uniformly mixing lauryl alcohol polyoxyethylene polyoxypropylene ether and alcohol, adding an oil phase, mixing, and adding a carbonate solution to obtain a carbonate microemulsion; c. and c, uniformly mixing the calcium salt microemulsion obtained in the step a and the carbonate microemulsion obtained in the step b, adding a crystal nucleus promoter and a dispersing agent, uniformly stirring, and performing aging, emulsion breaking, washing, centrifugal separation and drying treatment to obtain powdery cubic ultrafine calcium carbonate. The invention takes lauryl polyoxyethylene polyoxypropylene ether as a surfactant, and the cubic ultrafine calcium carbonate prepared by adopting a reverse microemulsion method has the characteristics of simple preparation process, good effect, environmental friendliness and the like.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the field of materials, and particularly relates to a preparation method of cubic calcium carbonate, which is simple in required equipment, simple and convenient to operate and environment-friendly.
[ background ] A method for producing a semiconductor device
The superfine calcium carbonate is a stable inorganic powder filling material, and can be applied to various fields, such as chemical industry, plastics, medicines and the like. Compared with other fillers, the cubic ultrafine calcium carbonate has the advantages of reinforcing effect and use cost, and also has great advantages in aspects of dispersibility, functionality and the like. At present, the cubic ultrafine calcium carbonate is prepared by a physical method and a chemical method, and the chemical method comprises a double decomposition method, a carbonation method and the like. The microemulsion method is a new method for preparing materials, and is concerned due to the simple reaction equipment and simple operation. The key of the microemulsion method is the preparation of microemulsion, so if the cubic ultrafine calcium carbonate can be prepared by one or more microemulsions, the preparation process of the cubic ultrafine calcium carbonate can be simplified, and the method has great application value.
[ summary of the invention ]
The invention aims to solve the problems and provides a method for preparing cubic ultrafine calcium carbonate with simple process and good effect.
The invention relates to a preparation method of cubic ultrafine calcium carbonate, which comprises the following steps:
a. preparation of calcium salt microemulsion: uniformly mixing lauryl polyoxyethylene polyoxypropylene ether and alcohol, adding an oil phase, mixing, and adding a calcium salt solution to obtain lauryl polyoxyethylene polyoxypropylene ether/alcohol/oil/calcium salt water reverse microemulsion;
b. preparation of carbonate microemulsion: uniformly mixing lauryl polyoxyethylene polyoxypropylene ether and alcohol, adding an oil phase, mixing, and adding a carbonate solution to obtain a lauryl polyoxyethylene polyoxypropylene ether/alcohol/oil/carbonate water reverse microemulsion;
c. preparation of cubic calcium carbonate: and (b) uniformly mixing the lauryl alcohol polyoxyethylene polyoxypropylene ether/alcohol/oil/calcium salt water reversed-phase microemulsion obtained in the step a and the lauryl alcohol polyoxyethylene polyoxypropylene ether/alcohol/oil/carbonate water reversed-phase microemulsion obtained in the step b, adding a crystal nucleus promoter and a dispersing agent, uniformly stirring, and performing aging, demulsification, washing, centrifugal separation and drying treatment to obtain powdery cubic ultrafine calcium carbonate.
In the step a, the weight ratio of the lauryl alcohol polyoxyethylene polyoxypropylene ether to the alcohol is 1: 1-3, wherein the alcohol is one of methanol, ethanol, propanol, butanol, pentanol and hexanol.
In the step a, the volume ratio of the laurinol polyoxyethylene polyoxypropylene ether to the oil phase is 2-4:8-6, and the oil phase is one of normal hexane, benzene, toluene and xylene.
In the step a, the calcium salt is soluble calcium salt, and the concentration of the soluble calcium salt is 0.1 mol/L-0.5 mol/L.
In the step a, the calcium salt is one of calcium chloride, calcium nitrate and calcium acetate.
In the step b, the weight ratio of the lauryl alcohol polyoxyethylene polyoxypropylene ether to the alcohol is 1: 1-3, wherein the alcohol is one of methanol, ethanol, propanol, butanol, pentanol and hexanol.
In the step b, the volume ratio of the laurinol polyoxyethylene polyoxypropylene ether to the oil phase is 2-4:8-6, and the oil phase is one of normal hexane, benzene, toluene and xylene.
In the step b, the carbonate is one of sodium carbonate, ammonium carbonate and potassium carbonate, and the concentration of the carbonate is 0.1-0.5 mol/L.
In the step c, the crystal nucleus accelerant and the dispersing agent are one of starch, sucrose and barium chloride, and the weight of the crystal nucleus accelerant and the dispersing agent is 0.1-1% of that of the cubic ultrafine calcium carbonate.
In the step c, the reaction temperature is 25-75 ℃, the stirring time is 10-60 minutes, the aging time is 24-48 hours, the drying temperature is 120-180 ℃, and the drying time is 24 hours.
The invention has the beneficial effects that: the invention takes environment-friendly nonionic surfactant lauryl polyoxyethylene polyoxypropylene ether as a surfactant and alcohol as a cosurfactant to form lauryl polyoxyethylene polyoxypropylene ether/alcohol/oil/calcium salt water reverse microemulsion and lauryl polyoxyethylene polyoxypropylene ether/alcohol/oil/carbonate water reverse microemulsion to prepare cubic ultrafine calcium carbonate, and the particle size of the obtained cubic ultrafine calcium carbonate is 0.2-20 microns. The invention has the characteristics of simple preparation process, good effect, energy saving, environmental protection and the like.
[ description of the drawings ]
FIG. 1 is an SEM photograph of calcium carbonate prepared in example 1 of the present invention.
Fig. 2 is an SEM image of calcium carbonate prepared in example 2 of the present invention.
Fig. 3 is an SEM image of calcium carbonate prepared in example 3 of the present invention.
[ detailed description ] embodiments
The present invention will be described in further detail with reference to specific examples, but the present invention is not limited thereto.
Example 1
Uniformly mixing laurinol polyoxyethylene polyoxypropylene ether and n-butanol according to a weight ratio of 1:1, then mixing the laurinol polyoxyethylene polyoxypropylene ether and the n-butanol with n-hexane according to a volume ratio of 2:8, and then adding 0.5mol/L calcium chloride solution to obtain transparent laurinol polyoxyethylene polyoxypropylene ether/alcohol/oil/calcium chloride water reverse microemulsion; the transparent reverse microemulsion of the lauryl polyoxyethylene polyoxypropylene ether/alcohol/oil/sodium carbonate is prepared by uniformly mixing the lauryl polyoxyethylene polyoxypropylene ether and n-butanol according to the weight ratio of 1:1, then mixing the mixture with n-hexane according to the volume ratio of 2:8, and then adding 0.5mol/L sodium carbonate solution. The lauryl polyoxyethylene polyoxypropylene ether/alcohol/oil/calcium chloride water reverse microemulsion and the lauryl polyoxyethylene polyoxypropylene ether/alcohol/oil/sodium carbonate water reverse microemulsion are uniformly mixed, 0.1 wt% of sucrose is added to serve as a crystal nucleus promoter and a dispersing agent, the mixture is stirred for 10 minutes at the temperature of 25 ℃, after aging is carried out for 24 hours, ethanol is added for ultrasonic demulsification, and after washing and centrifugal separation, the mixture is dried for 24 hours at the temperature of 120 ℃, cubic ultrafine calcium carbonate solid powder is obtained, wherein the structure of the cubic ultrafine calcium carbonate solid powder is shown in figure 1. As can be seen from FIG. 1, the cubic ultrafine calcium carbonate solid powder thus prepared was cubic, and had a particle size of about 11 μm.
Example 2
Uniformly mixing laurinol polyoxyethylene polyoxypropylene ether and n-hexanol according to a weight ratio of 1:2, then mixing the laurinol polyoxyethylene polyoxypropylene ether and n-hexanol with benzene according to a volume ratio of 3:7, and then adding 0.3mol/L calcium nitrate solution to obtain transparent laurinol polyoxyethylene polyoxypropylene ether/alcohol/oil/calcium nitrate water reverse microemulsion; the transparent polyoxyethylene lauryl polyoxypropylene ether/alcohol/oil/ammonium carbonate water reverse microemulsion is prepared by uniformly mixing the polyoxyethylene lauryl polyoxypropylene ether and n-hexanol according to the weight ratio of 1:2, then mixing the mixture with benzene according to the volume ratio of 3:7, and then adding 0.3mol/L ammonium carbonate solution. The lauryl polyoxyethylene polyoxypropylene ether/alcohol/oil/calcium nitrate water reverse microemulsion and the lauryl polyoxyethylene polyoxypropylene ether/alcohol/oil/ammonium carbonate water reverse microemulsion are uniformly mixed, starch with the weight content of 0.5% is added to serve as a crystal nucleus promoter and a dispersing agent, the mixture is stirred for 30 minutes at the temperature of 50 ℃, the mixture is aged for 36 hours, ethanol is added for ultrasonic demulsification, and after washing and centrifugal separation, the mixture is dried for 24 hours at the temperature of 150 ℃, and cubic ultrafine calcium carbonate solid powder is obtained, wherein the structure of the cubic ultrafine calcium carbonate solid powder is shown in figure 2. As can be seen from FIG. 2, the prepared cubic ultrafine calcium carbonate solid powder is cubic and has a particle size of about 0.2 to 3 μm.
Example 3
Uniformly mixing laurinol polyoxyethylene polyoxypropylene ether and ethanol according to a weight ratio of 1:3, then mixing the laurinol polyoxyethylene polyoxypropylene ether and the ethanol with xylene according to a volume ratio of 4:6, and then adding 0.1mol/L calcium acetate solution to obtain transparent laurinol polyoxyethylene polyoxypropylene ether/alcohol/oil/calcium acetate water reverse microemulsion; uniformly mixing laurinol polyoxyethylene polyoxypropylene ether and ethanol according to a weight ratio of 1:3, then mixing the laurinol polyoxyethylene polyoxypropylene ether and the ethanol with xylene according to a volume ratio of 4:6, and then adding a 0.1mol/L potassium carbonate solution to obtain the transparent laurinol polyoxyethylene polyoxypropylene ether/alcohol/oil/potassium carbonate water reverse microemulsion. The lauryl polyoxyethylene polyoxypropylene ether/alcohol/oil/calcium acetate water reversed-phase microemulsion and the lauryl polyoxyethylene polyoxypropylene ether/alcohol/oil/potassium carbonate water reversed-phase microemulsion are uniformly mixed, 1% by weight of barium chloride serving as a crystal nucleus promoter and a dispersing agent is added, the mixture is stirred for 60 minutes at the temperature of 75 ℃, after aging is carried out for 48 hours, ethanol is added for ultrasonic demulsification, and after washing and centrifugal separation, the mixture is dried for 24 hours at the temperature of 180 ℃, cubic ultrafine calcium carbonate solid powder is obtained, wherein the structure of the cubic ultrafine calcium carbonate solid powder is shown in figure 3. As can be seen from FIG. 3, the prepared cubic ultrafine calcium carbonate solid powder was cubic and had a particle size of about 1 μm.
From the examples 1 to 3, it can be seen that the cubic ultrafine calcium carbonate prepared by using the laurinol polyoxyethylene polyoxypropylene ether as the surfactant and adopting the reverse microemulsion method has the characteristics of simple preparation process, good effect, environmental friendliness and the like.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered in the protection scope of the present invention.
Claims (8)
1. The preparation method of the cubic ultrafine calcium carbonate is characterized by comprising the following steps:
a. preparation of calcium salt microemulsion: uniformly mixing lauryl polyoxyethylene polyoxypropylene ether and alcohol, adding an oil phase for mixing, and then adding a calcium salt solution to obtain lauryl polyoxyethylene polyoxypropylene ether/alcohol/oil/calcium salt water reverse microemulsion;
b. preparation of carbonate microemulsion: uniformly mixing lauryl polyoxyethylene polyoxypropylene ether and alcohol, adding an oil phase, mixing, and adding a carbonate solution to obtain a lauryl polyoxyethylene polyoxypropylene ether/alcohol/oil/carbonate water reverse microemulsion;
c. preparation of cubic calcium carbonate: uniformly mixing the lauryl alcohol polyoxyethylene polyoxypropylene ether/alcohol/oil/calcium salt water reversed-phase microemulsion obtained in the step a with the lauryl alcohol polyoxyethylene polyoxypropylene ether/alcohol/oil/carbonate water reversed-phase microemulsion obtained in the step b, adding a crystal nucleus promoter and a dispersing agent, uniformly stirring, and performing aging, demulsification, washing, centrifugal separation and drying treatment to obtain powdery cubic ultrafine calcium carbonate;
in the step a, the weight ratio of the laurinol polyoxyethylene polyoxypropylene ether to the alcohol is 1: 1-3, wherein the alcohol is one of methanol, ethanol, propanol, butanol, pentanol and hexanol;
in the step a, the volume ratio of the laurinol polyoxyethylene polyoxypropylene ether to the oil phase is 2-4:8-6, and the oil phase is one of normal hexane, benzene, toluene and xylene.
2. The method for preparing cubic ultrafine calcium carbonate according to claim 1, wherein in step a, the calcium salt is a soluble calcium salt and has a concentration of 0.1 to 0.5mol/L.
3. The method for preparing cubic ultrafine calcium carbonate according to claim 1, wherein in step a, the calcium salt is one of calcium chloride, calcium nitrate and calcium acetate.
4. The method for preparing cubic ultrafine calcium carbonate according to claim 1, wherein in step b, the weight ratio of laureth to alcohol is 1: 1-3, wherein the alcohol is one of methanol, ethanol, propanol, butanol, pentanol and hexanol.
5. The method for preparing cubic ultrafine calcium carbonate according to claim 1, wherein in step b, the volume ratio of the laureth-polyoxypropylene to the oil phase is 2-4:8-6, and the oil phase is one of n-hexane, benzene, toluene and xylene.
6. The method for preparing cubic ultrafine calcium carbonate according to claim 1, wherein in the step b, the carbonate is one of sodium carbonate, ammonium carbonate and potassium carbonate, and the concentration thereof is 0.1mol/L to 0.5mol/L.
7. The method for preparing cubic ultrafine calcium carbonate according to claim 1, wherein in step c, the nucleating agent and the dispersing agent are one of starch, sucrose and barium chloride, and the weight of the nucleating agent and the dispersing agent is 0.1 to 1 percent of the weight of the cubic ultrafine calcium carbonate.
8. The method for preparing cubic ultrafine calcium carbonate according to claim 1, wherein in step c, the reaction temperature is 25 to 75 ℃, the stirring time is 10 to 60 minutes, the aging time is 24 to 48 hours, the drying temperature is 120 to 180 ℃, and the drying time is 24 hours.
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| CN113120936A (en) * | 2021-04-21 | 2021-07-16 | 贺州学院 | Method for preparing superfine calcium carbonate by adopting N235 reversed-phase microemulsion method |
| CN112939048A (en) * | 2021-04-21 | 2021-06-11 | 贺州学院 | Method for preparing superfine calcium carbonate by adopting P507 reverse microemulsion method |
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