阅读说明：本技术 一种菊花状微米碳酸钙的制备方法 (Preparation method of chrysanthemum-shaped micron calcium carbonate ) 是由 王农 赵调彬 曾一文 于 2020-05-11 设计创作，主要内容包括：本发明属于碳酸钙制备领域,具体涉及一种菊花状微米碳酸钙的制备方法。所述方法包括以下步骤：1)反相微乳液的制备：将水、油、助表面活性剂和表面活性剂按体积比充分混合配制成澄清的反相微乳液；2)菊花状微米碳酸钙的制备：在搅拌状态下,将二氧化碳通入步骤1)的反相微乳液中反应一定时间,直至不再产生沉淀,然后停止通入二氧化碳气体,结束搅拌,在室温下静置、陈化后离心分离,将所得沉淀进行烘干即得所述菊花状微米碳酸钙。本发明制备的菊花状微米碳酸钙表面具有多层褶皱,形似一朵绽放的菊花,且形貌均一,分散度良好,具有广阔的应用前景。(The invention belongs to the field of calcium carbonate preparation, and particularly relates to a preparation method of chrysanthemum-shaped micron calcium carbonate. The method comprises the following steps: 1) preparing reverse microemulsion: fully mixing water, oil, cosurfactant and surfactant according to a volume ratio to prepare clear reverse microemulsion; 2) preparing chrysanthemum-shaped micron calcium carbonate: and (2) introducing carbon dioxide into the reversed-phase microemulsion obtained in the step 1) under the stirring state for reacting for a certain time until no precipitate is generated, stopping introducing carbon dioxide gas, ending stirring, standing at room temperature, aging, then performing centrifugal separation, and drying the obtained precipitate to obtain the chrysanthemum-shaped micron calcium carbonate. The chrysanthemum-shaped micron calcium carbonate prepared by the method has the advantages of multilayer folds on the surface, uniform appearance, good dispersion degree and wide application prospect, and is similar to a blooming chrysanthemum.)

1. A preparation method of chrysanthemum-shaped micron calcium carbonate is characterized by comprising the following steps:

1) preparing reverse microemulsion: fully mixing water, oil, cosurfactant and surfactant to prepare clear reverse microemulsion; the water phase is calcium chloride water solution, the oil phase is cyclohexane, the cosurfactant is n-butanol, and the surfactant is cetyl trimethyl ammonium bromide;

2) preparing chrysanthemum-shaped micron calcium carbonate: and (2) introducing carbon dioxide into the reversed-phase microemulsion obtained in the step 1) under the stirring state for reacting for a certain time until no precipitate is generated, stopping introducing carbon dioxide gas, ending stirring, standing at room temperature, aging, then performing centrifugal separation, and drying the obtained precipitate to obtain the chrysanthemum-shaped micron calcium carbonate.

2. The method for preparing chrysanthemum-shaped micron calcium carbonate according to claim 1, wherein the dosage ratio of the water, the oil, the cosurfactant and the surfactant is 4ml:100ml:30ml:16 g.

3. The method for preparing chrysanthemum-shaped micron calcium carbonate according to claim 1, wherein in the step 2), carbon dioxide is introduced into the reverse microemulsion of the step 1) to react for 30 min.

4. The method for preparing chrysanthemum-like micron calcium carbonate according to claim 1, wherein in the step 2), the aging time is 24 hours.

5. The method for preparing chrysanthemum-shaped micron calcium carbonate according to claim 1, wherein in the step 2), the drying treatment is drying in an oven at 80 ℃ for 24 hours.

6. The method for preparing chrysanthemum-like micron calcium carbonate according to claim 1, wherein the calcium chloride aqueous solution is prepared by the following method: weighing calcium chloride, dissolving with 25% ammonia water and a small amount of water, and adding water to obtain 0.5mol/L solution after completely dissolving.

7. The method for preparing chrysanthemum-like micron calcium carbonate according to claim 1, wherein the carbon dioxide is prepared by the following method: weighing a certain amount of concentrated hydrochloric acid, placing in a conical flask, weighing equimolar marble, and placing in the conical flask for reaction to obtain the product.

[ technical field ] A method for producing a semiconductor device

The invention belongs to the field of calcium carbonate preparation, and particularly relates to a preparation method of chrysanthemum-shaped micron calcium carbonate.

[ background of the invention ]

The reverse microemulsion is a water-in-oil type dispersion system composed of oil phase, water phase and surfactant. The preparation method is a novel preparation method, equipment and process are simple, a micro-reactor is provided for a water tank in the micro-emulsion, the morphology of particles can be controlled, the instability (agglomeration, oxidation and the like) of the particles possibly caused by other preparation methods can be avoided, and the preparation method has the advantages of small particle size, good dispersibility, no impurities and the like. Therefore, the microemulsion method is an effective method for preparing nanoparticles, which has been developed in recent years. The nanometer water pool is a very good chemical reaction medium, and the particle size and other properties of the product are controlled by artificially controlling the size of the nanometer water pool.

The micron-sized light calcium carbonate is an important inorganic chemical product serving as a filling agent and a reinforcing agent, is widely used in the production and processing of rubber, plastics, building materials for papermaking, coatings, printing ink, food, feeds, toothpaste, cosmetics and the like, and common micron-sized calcium carbonate particles are spindle-shaped, rod-shaped or cubic and the like, have the average particle size of 0.5-5 microns and the relative density of 2.4-2.7, are slightly alkaline, are insoluble in water and are stable in chemical properties of easy moisture absorption. If the rubber is added into tires, rubber tubes of conveyer belts, rubberized fabrics and medical rubber products, the rubber consumption can be reduced, and the cost can be reduced, and the rubber can also play a role in reinforcement and semi-reinforcement. When the organic light-emitting material is applied to plastics, the consumption of organic raw materials can be reduced, the cost is reduced, the stability, the hardness and the rigidity of the plastics are improved, the processability of the plastics is improved, the heat resistance is improved, the light scattering property of the plastics is improved, and the like. The practical application of calcium carbonate is related to the properties of the shape, the granularity, the specific surface area, the oil absorption value and the like of the particles of the calcium carbonate, so that the research and development of the controllable preparation method of the calcium carbonate with specific shape and high dispersity is of great significance. There are many existing CaCO₃Research reports on optimizing corresponding properties of micro-nano materials by controlling the shapes and sizes of the micro-nano materials in the preparation process, researchers have adopted various preparation methods to synthesize CaCO₃Nano-wire, hollow ball, rugby, octahedron, etc. However, few reports have been made on micro-nano chrysanthemum-like calcium carbonate crystals.

[ summary of the invention ]

The invention aims to provide a preparation method of chrysanthemum-shaped micron calcium carbonate. The chrysanthemum-shaped micron calcium carbonate particles prepared by the method are simple in preparation method and easy to obtain raw materials, the surfaces of the chrysanthemum-shaped micron calcium carbonate particles have multiple layers of folds, the chrysanthemum-shaped micron calcium carbonate particles are similar to a blooming chrysanthemum flower, the appearance is uniform, the dispersity is good, and the chrysanthemum-shaped micron calcium carbonate particles have a wide application prospect.

In order to achieve the purpose, the technical scheme adopted by the invention is as follows:

a preparation method of chrysanthemum-shaped micron calcium carbonate comprises the following steps:

1) preparing reverse microemulsion: fully mixing water, oil, cosurfactant and surfactant to prepare clear reverse microemulsion; the water phase is calcium chloride water solution, the oil phase is cyclohexane, the cosurfactant is n-butanol, and the surfactant is cetyl trimethyl ammonium bromide;

2) preparing chrysanthemum-shaped micron calcium carbonate: and (2) introducing carbon dioxide into the reversed-phase microemulsion obtained in the step 1) under the stirring state for reacting for a certain time until no precipitate is generated, stopping introducing carbon dioxide gas, ending stirring, standing at room temperature, aging, then performing centrifugal separation, and drying the obtained precipitate to obtain the chrysanthemum-shaped micron calcium carbonate.

Further, the dosage ratio of the water, the oil, the cosurfactant and the surfactant is 4ml to 100ml to 30ml to 16 g.

Further, in the step 2), carbon dioxide is introduced into the reversed-phase microemulsion of the step 1) to react for 30 min.

Further, in the step 2), the aging time is 24 hours.

Further, in the step 2), the drying treatment is drying in an oven at 80 ℃ for 24 hours.

In the invention, the calcium chloride aqueous solution is prepared by the following method: weighing calcium chloride, dissolving with 25% ammonia water and a small amount of water, and adding water to obtain 0.5mol/L solution after completely dissolving.

In the invention, the carbon dioxide is prepared by the following method: weighing a certain amount of concentrated hydrochloric acid, placing in a conical flask, weighing equimolar marble, and placing in the conical flask for reaction to obtain the product.

In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:

(1) the preparation method is simple, the raw materials are easy to obtain, and the chrysanthemum-shaped micron calcium carbonate prepared by the method has uniform appearance and particle size.

(2) The chrysanthemum-shaped micron calcium carbonate prepared by the invention has multilayer folds on the surface, is similar to a blooming chrysanthemum, has uniform appearance, good dispersity and higher specific surface area and settling volume, can be used for papermaking filling, can effectively improve indexes such as bulk, opacity, whiteness and the like of paper sheets, and has wide application prospect.

[ description of the drawings ]

FIG. 1: scanning electron micrographs of the chrysanthemum-like micron calcium carbonate prepared in the examples;

FIG. 2: x-ray diffraction patterns of the daisy-like micron calcium carbonate prepared in the examples;

FIG. 3: scanning electron micrographs of the micron calcium carbonate prepared in the comparative example;

FIG. 4: the X-ray diffraction pattern of the micron calcium carbonate prepared in the comparative example;

FIG. 5: the main characteristic peaks in the standard X-ray diffraction patterns of vaterite and calcite.

[ detailed description ] embodiments

The specific embodiments and effects of the present invention will be illustrated by the following examples, but the scope of the present invention is not limited thereto.