阅读说明：本技术 一种铁饼状微米碳酸钙的制备方法 (Preparation method of discus-shaped micron calcium carbonate ) 是由 曾一文 徐超 赵调彬 王农 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,具体涉及一种铁饼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)铁饼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铁饼状微米碳酸钙。本发明所述方法安全性能高,简单合理,能耗低,原料易得、价格低廉,所述铁饼状微米碳酸钙属于轻质碳酸钙,具有很好的粒度分布和稳定性,分散度良好,可用作橡胶、塑料、造纸、涂料和油墨等的填料。(The invention belongs to the field of calcium carbonate preparation, and particularly relates to a preparation method of discus-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) preparation of discus-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, performing centrifugal separation, and drying the obtained precipitate to obtain the discus-shaped micron calcium carbonate. The method has the advantages of high safety performance, simplicity, reasonableness, low energy consumption, easily obtained raw materials and low price, and the discus-shaped micron calcium carbonate belongs to light calcium carbonate, has good particle size distribution and stability and good dispersity and can be used as a filler for rubber, plastics, papermaking, paint, ink and the like.)

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

1) preparing reverse microemulsion: fully mixing water, oil, cosurfactant and surfactant according to a volume ratio to prepare clear reverse microemulsion; said aqueous phase is an aqueous calcium chloride solution, said oil phase is cyclohexane, said co-surfactant is n-octanol, said surfactant is OP-10;

2) preparation of discus-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, performing centrifugal separation, and drying the obtained precipitate to obtain the discus-shaped micron calcium carbonate.

2. The method of preparing discus-like micrometer calcium carbonate according to claim 1, wherein the volume ratio of water, oil, co-surfactant and surfactant is 4:50:15: 15.

3. The method for preparing discus-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) for reaction for 30 min.

4. The process for preparing discus-shaped monocalcium carbonate according to claim 1, wherein in step 2), the aging time is 24 hours.

5. The method for preparing discus-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 h.

6. The method of preparing discus-like micrometer calcium carbonate according to claim 1, wherein the aqueous calcium chloride 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.

[ 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 discus-shaped micron calcium carbonate.

[ background of the invention ]

Calcium carbonate is an important inorganic chemical product and is widely used in the industries of rubber, plastics, printing ink, coating, paper making and the like. In particular to micro-nano calcium carbonate which is used for rubber, paper making, plastics and the like and can ensure that products have bright surface, large tensile strength, high tensile strength, good bending resistance, good cracking resistance and the like. The ink has the characteristics of good gloss, transparency, stability, quick drying and the like in high-grade ink. In the paint industry, the paint is mainly used for synthetic resin paint, automobile paint and the like, improves the thixotropy of a system, can obviously improve the adhesive force, the washing resistance and the stain resistance of the paint, and has good anti-settling effect; the paint has many excellent functions such as strong adhesion, impact resistance, scratch resistance, firmness and durability when added into the automobile chassis paint. In the industry of sealing and bonding materials, the cross-linking reaction of the glue can be accelerated, the stability of the glue is enhanced, the mechanical property of the glue is improved, the dual functions of filling and reinforcing are achieved, and the surface of the glue material is bright and fine. In the production of micro-nano calcium carbonate, the size, the crystal shape, the particle size distribution and the dispersion performance of calcium carbonate crystal particles are important performance indexes. The product with small granularity, uniform distribution and good dispersion performance has higher economic utilization value and wider market prospect.

The reverse microemulsion method is a water-in-oil type dispersion system composed of an oil phase, a water phase, a surfactant and the like. As a novel preparation method, the method has simple equipment and process, can provide a nano-scale microreactor, can accurately control the size and the shape of particles, well avoids the phenomena of agglomeration, oxidation and the like of micro-nano particles possibly caused in the processes of other preparation methods, and the prepared nanoparticles have the advantages of small particle size, good dispersibility, no impurities and the like. Therefore, the microemulsion method is an effective method for preparing micro-nano particles developed in recent years. Is a very good chemical reaction medium, and the particle size and other properties of the product can be controlled by artificially controlling the size of the 'micro water pool'.

[ summary of the invention ]

The invention aims to provide a preparation method of discus-shaped micron calcium carbonate. The method has the advantages of high safety performance, simplicity, reasonableness, low energy consumption, easily obtained raw materials, low price, good particle size distribution and stability of the discus-shaped micron calcium carbonate, good dispersion degree and wide application prospect.

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

a preparation method of discus-shaped micron calcium carbonate 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; said aqueous phase is an aqueous calcium chloride solution, said oil phase is cyclohexane, said co-surfactant is n-octanol, said surfactant is OP-10;

2) preparation of discus-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, performing centrifugal separation, and drying the obtained precipitate to obtain the discus-shaped micron calcium carbonate.

Further, the volume ratio of the water, the oil, the cosurfactant and the surfactant is 4:50:15: 15.

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

the preparation method of the discus-shaped micron calcium carbonate has the advantages of high safety performance, simplicity, reasonability, low energy consumption, easily available raw materials and low price, and the discus-shaped micron calcium carbonate has good particle size distribution and stability, good dispersity and wide application prospect.

[ description of the drawings ]

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

FIG. 2: x-ray diffraction patterns of the discus-like micrometer 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.