CN103058250B - Method for preparing nano calcium carbonate by gypsum - Google Patents
Method for preparing nano calcium carbonate by gypsum Download PDFInfo
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- CN103058250B CN103058250B CN201310001726.2A CN201310001726A CN103058250B CN 103058250 B CN103058250 B CN 103058250B CN 201310001726 A CN201310001726 A CN 201310001726A CN 103058250 B CN103058250 B CN 103058250B
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Abstract
The invention discloses a method for preparing nano calcium carbonate by gypsum. The method comprises the following steps: (1) grinding the desulfurization gypsum into solid powder of 50-1,000 meshes; (2) adding the ground desulfurization gypsum into a water solution of 8-12% of HCl or 20-40% of citric acid by weight, stirring for dissolving, and filtering to obtain filter liquor; and (3) spraying the filter liquor through a high-pressure spraying gun under the pressure of 0.1-2 MPa, and atomizing; meanwhile, inversely filling high-pressure carbon dioxide with the pressure of 0.15-4 MPa into atomized air flow; starting an enhanced microwave generator outside a container to emit enhanced microwaves of 0.1-10 W/cm<2> into the container; and collecting the generated solid powder to obtain nano calcium carbonate. Due to the adoption of the method, raw material sources are rich, the process is simpler, the prepared nano calcium carbonate is uniform in particle size, and the particle size can reach 0.05-0.08 mu m.
Description
Technical field
The present invention relates to a kind of method of producing calcium carbonate, especially relate to a kind of method that gypsum produces nano-calcium carbonate.
Background technology
Nano-calcium carbonate is also called super-refinement calcium carbonate, and its granularity is between 0.01-0.1 μm, and the most ripe industry of application is plastics industry, is mainly used on high-grade plastics, can improves the mobility of plastic matrix, improve its formability.Nano-calcium carbonate is used as plastic filler, has well toughened and reinforced effect, can improve flexural strength and the bending elastic modulus of plastics, heat-drawn wire and dimensional stability, also gives plastics stagnant hot simultaneously.Nano-calcium carbonate is used for ink filler, and have good stability, glossiness is high, does not affect the advantages such as the drying property of printing-ink, conformability.
The production method of nanometer grade calcium carbonate is a lot, can be divided into wet method and dry method substantially.
Chinese invention patent application 200710157482.1 discloses a kind of preparation method of nano-calcium carbonate, in water, add raw material unslaked lime or calcium hydroxide, be mixed with the suspension of 8-12%, carbonic acid gas is passed under whipped state, the pH of regulator solution, prepares the calcium carbonate of 20-80 nanometer finally by X-type nanometer ram machine.
Chinese invention patent application 201110390578.9 discloses a kind of preparation method of nano-calcium carbonate, and it provides a kind of under high-pressure carbon dioxide and ionic liquid participate in, and can carry out the preparation method of the nano-calcium carbonate of carburizing reagent in anhydrous conditions.
But above-mentioned two kinds of preparation process are all too complicated, repeatability is poor, is not suitable for suitability for industrialized production.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes the deficiencies in the prior art, provides a kind of abundant raw material source, and the better simply gypsum of technique produces the method for nano-calcium carbonate.
The technical scheme that the present invention solves the employing of its technical problem is:
Gypsum produces a method for nano-calcium carbonate, comprises the following steps:
(1) desulfurated plaster is ground into the pressed powder of 50-1000 order (preferred 500-800 order); Purity >=the 90wt% of described desulfurated plaster;
(2) desulfurated plaster after step (1) pulverizing is added 8-12wt%HCl or 20-40wt% lemon aqueous acid, filter after stirring and dissolving, obtain filtrate;
(3) by step (2) gained filtrate by high-pressure spray gun at the preferred 0.5-1.5 MPa of 0.1-2 MPa() pressure under spray, make it be atomized; Simultaneously to the reverse pressure that passes in the air-flow of atomization be the preferred 1-2 MPa of 0.15-4MPa() high-pressure carbon dioxide; And in container, launch 0.1-10 W/cm at the outside of container unlatching strengthening microwave generator
2(preferred 1-5 W/cm
2) strengthening microwave; Collect the pressed powder generated, obtain nanometer grade calcium carbonate.
Containing a large amount of calcium ion in mixing solutions after the present invention filters, under high-pressure spray gun effect, this solution is atomized, another mistake is to passing into high-pressure carbon dioxide gas, further refinement solution droplets on the one hand, promote that carbonic acid gas is dissolved in rapidly in solution on the other hand, generate carbonic acid, carbanion and calcium ion react, and generate calcium carbonate; Then, under the effect of periphery strengthening microwave, accelerate the motion of particle, water molecules energy is raised, accelerate the evaporation of moisture, drying calcium carbonate.
Adopt the gypsum of the present invention to produce the method for nano-calcium carbonate, abundant raw material source, technique is comparatively simple, and obtained nano-calcium carbonate, uniform particle size, particle diameter can reach 0.05-0.08 μm.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
The metering facility of Nano particles of calcium carbonate particle diameter in embodiment: the tester of nanometer particle size; Detection method standard is: ISO 13321 analysing particulates granulometry method.
Embodiment 1
The gypsum of the present embodiment produces the method for nano-calcium carbonate, comprises the following steps:
(1) desulfurated plaster is ground into 500 object pressed powders; The purity of described desulfurated plaster is 90wt%;
(2) desulfurated plaster after step (1) pulverizing is added 24wt% lemon aqueous acid, filter after stirring and dissolving, obtain filtrate;
(3) step (2) gained filtrate is sprayed by high-pressure spray gun under the pressure of 0.2 MPa, make it be atomized; Simultaneously reversely in the air-flow of atomization pass into the high-pressure carbon dioxide that pressure is 0.35MPa; And in container, launch 0.5W/cm at the outside of container unlatching strengthening microwave generator
2strengthening microwave; Collect the pressed powder generated, obtain nanometer grade calcium carbonate.
Adopt the gypsum of the present invention to produce the method for nano-calcium carbonate, abundant raw material source, technique is comparatively simple, and obtained nano-calcium carbonate, uniform particle size, median size reaches 0.07 μm.
Embodiment 2
The gypsum of the present embodiment produces the method for nano-calcium carbonate, comprises the following steps:
(1) desulfurated plaster is ground into 100 object pressed powders; The purity of described desulfurated plaster is 91wt%;
(2) desulfurated plaster after step (1) pulverizing is added 39wt% lemon aqueous acid, filter after stirring and dissolving, obtain filtrate;
(3) step (2) gained filtrate is sprayed by high-pressure spray gun under the pressure of 1.0 MPa, make it be atomized; Simultaneously reversely in the air-flow of atomization pass into the high-pressure carbon dioxide that pressure is 0.15MPa; And in container, launch 5W/cm at the outside of container unlatching strengthening microwave generator
2strengthening microwave; Collect the pressed powder generated, obtain nanometer grade calcium carbonate.
Adopt the gypsum of the present invention to produce the method for nano-calcium carbonate, abundant raw material source, technique is comparatively simple, and obtained nano-calcium carbonate, uniform particle size, median size reaches 0.06 μm.
Embodiment 3
The gypsum of the present embodiment produces the method for nano-calcium carbonate, comprises the following steps:
(1) desulfurated plaster is ground into 1000 object pressed powders; The purity of described desulfurated plaster is 92wt%;
(2) desulfurated plaster after step (1) pulverizing is added the aqueous solution of 10wt%HCl, filter after stirring and dissolving, obtain filtrate;
(3) step (2) gained filtrate is sprayed by high-pressure spray gun under the pressure of 2 MPa, make it be atomized; Simultaneously reversely in the air-flow of atomization pass into the high-pressure carbon dioxide that pressure is 4MPa; And in container, launch 10W/cm at the outside of container unlatching strengthening microwave generator
2strengthening microwave; Collect the pressed powder generated, obtain nanometer grade calcium carbonate.
Adopt the gypsum of the present invention to produce the method for nano-calcium carbonate, abundant raw material source, technique is comparatively simple, and obtained nano-calcium carbonate, uniform particle size, median size reaches 0.07 μm.
Claims (4)
1. gypsum produces a method for nano-calcium carbonate, it is characterized in that, comprises the following steps:
(1) desulfurated plaster is ground into 50-1000 object pressed powder; Purity >=the 90wt% of described desulfurated plaster;
(2) desulfurated plaster after step (1) pulverizing is added 20-40wt% aqueous citric acid solution, filter after stirring and dissolving, obtain filtrate;
(3) step (2) gained filtrate is sprayed by high-pressure spray gun under the pressure of 0.5-1.5 MPa, make it be atomized; Simultaneously reversely in the air-flow of atomization pass into the high-pressure carbon dioxide that pressure is 0.15-4MPa; And in container, launch 0.1-10 W/cm at the outside of container unlatching strengthening microwave generator
2strengthening microwave; Collect the pressed powder generated, obtain nanometer grade calcium carbonate.
2. gypsum according to claim 1 produces the method for nano-calcium carbonate, it is characterized in that, in step (1), desulfurated plaster is ground into 500-800 object pressed powder.
3. gypsum according to claim 1 and 2 produces the method for nano-calcium carbonate, it is characterized in that, in step (3), reversely in the air-flow of atomization passes into the high-pressure carbon dioxide that pressure is 1-2 MPa.
4. gypsum according to claim 1 and 2 produces the method for nano-calcium carbonate, it is characterized in that, in step (3), opens strengthening microwave generator and launch 1-5 W/cm in container
2strengthening microwave.
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Citations (3)
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|---|---|---|---|---|
| CN101045544A (en) * | 2007-04-26 | 2007-10-03 | 安徽工业大学 | Method for preparing superthin light calcium carbonate using plaster as raw material |
| CN102671523A (en) * | 2012-04-26 | 2012-09-19 | 上海第二工业大学 | Method for fixing light calcium carbonate as CO2 byproduct by using humate and desulfurization gypsum |
| EP2524898A1 (en) * | 2011-05-16 | 2012-11-21 | Omya Development AG | Precipitated calcium carbonate from pulp mill waste having an improved brightness, method for the production and use thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP5467276B2 (en) * | 2007-12-25 | 2014-04-09 | 学校法人日本大学 | Method for producing nano-sized calcium carbonate |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101045544A (en) * | 2007-04-26 | 2007-10-03 | 安徽工业大学 | Method for preparing superthin light calcium carbonate using plaster as raw material |
| EP2524898A1 (en) * | 2011-05-16 | 2012-11-21 | Omya Development AG | Precipitated calcium carbonate from pulp mill waste having an improved brightness, method for the production and use thereof |
| CN102671523A (en) * | 2012-04-26 | 2012-09-19 | 上海第二工业大学 | Method for fixing light calcium carbonate as CO2 byproduct by using humate and desulfurization gypsum |
Non-Patent Citations (4)
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| "氢氧化钙喷雾碳化生产超细碳酸钙";朱跃斌;《湖南化工》;19990228;第29卷(第1期);第39-40、42页 * |
| "水/乙二醇混合溶剂中微波辅助合成碳酸钙";孙新园等;《安庆师范学院学报( 自然科学版)》;20120630;第18卷(第2期);第77-80页 * |
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Effective date of registration: 20160825 Address after: An Industrial Park Economic Development Zone, Changde City, Hunan province Linli County 415200 Patentee after: Hunan Fu Xiang new type building material Co., Ltd. Address before: 410005, 12 floor, Haidong mansion, Furong Road, Changsha, Hunan Patentee before: Liu Liwen |