CN108975372B - Preparation method of spindle-shaped precipitated calcium carbonate - Google Patents
Preparation method of spindle-shaped precipitated calcium carbonate Download PDFInfo
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- 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
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- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- 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
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- 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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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Abstract
The invention discloses a preparation method of spindle-shaped precipitated calcium carbonate, which comprises the steps of taking lime and water for a digestion reaction to obtain lime slurry, standing, sieving by a 100-mesh sieve for deslagging and refining, adjusting the solid content to 8-12%, and aging for 24 hours to obtain refined lime slurry for later use; conveying the mixture into a reaction kettle, adding a crystal form control agent, controlling the temperature of lime slurry to be 26-50 ℃, introducing mixed gas containing carbon dioxide to perform carbonation reaction, adding a composite organic metal scale inhibitor after calcium carbonate reaction is performed for 5-10min, continuing carbonation reaction after uniform stirring, adding a cellulose-based surfactant to continue carbonation when the conductivity of the system has a drop inflection point, and stopping introducing gas to terminate carbonation reaction after the conductivity is reduced to 0.5ms/cm and carbonizing for 3-5min to obtain calcium carbonate slurry; the spindle-shaped precipitated calcium carbonate product can be obtained by carrying out filter pressing, drying, crushing and sieving on the calcium carbonate slurry. The calcium carbonate prepared by the invention has a spindle-shaped structure, narrow particle size distribution, uniform appearance, good dispersibility and good market application prospect.
Description
Technical Field
The invention belongs to the technical field of inorganic materials, and particularly relates to a preparation method of spindle-shaped precipitated calcium carbonate.
Background
Calcium carbonate is an important chemical material and is widely applied to industries such as papermaking, plastics, coatings, rubber, medicines and the like. According to the production method, the calcium carbonate can be divided into heavy calcium carbonate and light calcium carbonate (precipitated calcium carbonate). The heavy calcium carbonate is prepared by directly and mechanically crushing, grinding and grading ores; and precipitated calcium carbonate is prepared by chemical precipitation. The heavy calcium carbonate obtained by mechanically grinding natural ore has irregular particle shape and unstable product quality, and is difficult to meet the requirement of the market on high-quality products. Precipitated calcium carbonate with different particle sizes, specific surface areas, morphologies, and other physicochemical properties can be prepared by a chemical precipitation method.
The preparation method of the precipitated calcium carbonate mainly comprises an intermittent bubbling carbonization method, a spray carbonization method, a supergravity carbonization method and the like. The intermittent bubbling carbonization method is the most widely applied method in industry at present, and the method has the advantages of simple operation, low production cost, low production efficiency, large product agglomeration and wide particle size distribution. The spray carbonization method has the advantage of high utilization rate of carbon dioxide, but the equipment maintenance is complicated, and the product instability is caused due to poor production operability. The hypergravity carbonization method has the advantage of narrow product particle size distribution, but the high equipment investment limits the application of the hypergravity carbonization method in industry. In general, the production of precipitated calcium carbonate is mainly faced with the problems of difficult control of crystal form, wide particle size distribution of the product and different particle sizes, which greatly affects the later application stability of the precipitated calcium carbonate. For example, in the plastic industry, the mechanical properties of plastic products are seriously reduced due to poor dispersibility of calcium carbonate products, and in the coating industry, the coating performance is influenced due to poor dispersibility of the coating caused by wide particle size distribution of the calcium carbonate products. Therefore, how to prepare precipitated calcium carbonate with narrow particle size distribution, good uniformity and good dispersibility becomes the key point of research.
Chinese patent CN102583483A discloses a method for preparing micron spindle composite nano calcium carbonate, which comprises aging the micron spindle calcium carbonate for a long time at the final stage of reaction, adding a small amount of raw slurry for carbon supplement, and continuously growing small particle crystals on the original spindle.
Chinese patent CN107792872A discloses a process for preparing spindle-shaped nano calcium carbonate, which comprises using high-activity lime and carbon dioxide as raw materials, carbonizing the raw materials in a first-stage carbonization tower until the pH value is 9, aging the slurry for 72h, and feeding the slurry into a second-stage carbonization tower to continue carbonizing until the carbon is cooked to obtain the product. The product has the characteristics of regular appearance, uniform particle size and good particle size dispersion, but the production period of the method is too long, and the equipment utilization rate is extremely low.
Chinese patent CN107555459A discloses a method for preparing precipitated calcium carbonate of nano spindle, which comprises grinding lime slurry, adding crystal control agent of sodium bis (2-ethylhexyl) succinate sulfonate and zinc sulfate, carbonating, and adding sodium polyacrylate dispersant to obtain final product. The product of the invention has good appearance of the spindle body, but poor dispersibility and a plurality of clusters.
The above background disclosure is only for the purpose of assisting understanding of the inventive concept and technical solutions of the present invention, and does not necessarily belong to the prior art of the present patent application, and should not be used for evaluating the novelty and inventive step of the present application in the case that there is no clear evidence that the above content is disclosed at the filing date of the present patent application.
Disclosure of Invention
The invention aims to provide a preparation method of spindle-shaped precipitated calcium carbonate with narrow particle size distribution, uniform appearance, uniform particle size and good dispersibility.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a preparation method of spindle-shaped precipitated calcium carbonate comprises the following steps:
(1) taking active lime with the activity degree of 200-400 and water for a digestion reaction, stirring for 15-30min by a high-speed stirrer to obtain lime slurry, standing, sieving by a 100-mesh sieve for deslagging and refining, adjusting the solid content to 8-12%, and aging for 24h to obtain refined lime slurry for later use;
(2) conveying the refined lime slurry into a reaction kettle, adding a crystal form control agent accounting for 0.1-1% of the dry basis weight of calcium carbonate, starting stirring, starting jacket circulating water for controlling the temperature, controlling the temperature of the lime slurry to be 26-50 ℃, closing the circulating water, introducing mixed gas containing carbon dioxide for carbonation reaction, adding a composite organic metal scale inhibitor accounting for 0.1-1% of the dry basis weight of calcium carbonate after the calcium carbonate reaction is carried out for 5-10min, continuing the carbonation reaction after the lime slurry is uniformly stirred, adding a cellulose-based surfactant accounting for 0.3-3% of the dry basis weight of calcium carbonate for continuing the carbonation when the electrical conductivity of the system has a drop inflection point, and then carbonizing for 3-5min after the electrical conductivity is reduced to 0.5ms/cm, stopping introducing air and terminating the carbonation reaction to obtain calcium;
(3) the spindle-shaped precipitated calcium carbonate product can be obtained by carrying out filter pressing, drying, crushing and sieving on the calcium carbonate slurry.
Further, the mass ratio of the slaked reaction lime to the water is 1: 5-8.
Further, the digestion reaction is controlled at 30-60 ℃ and at a rotation speed of 150-300 r/min.
Further, the crystal form control agent is tartaric acid and/or succinic acid.
Further, the composite organic metal scale inhibitor comprises any one or a mixture of a plurality of polyacrylic acid, polymaleic anhydride and polyaspartic acid in any proportion.
Further, the cellulose-based surfactant is one or more of hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, sodium lignosulfonate and calcium lignosulfonate.
Further, the concentration of carbon dioxide in the mixed gas at the early stage of the carbonation reaction for 5-10min is 5-20%, and the gas flow is 0.5-1m3H, then adjusting the concentration of carbon dioxide in the mixed gas to be 30-50%, and the flow rate to be 1-4m3H until the reaction is complete.
Further, the stirring speed of the carbonation reaction kettle is 500-800 r/min.
Further, the stirring paddle used by the carbonation reaction kettle is a straight blade turbine type stirring paddle.
Further, the drying temperature is 100-120 ℃, and the drying time is 6-8 h.
Compared with the prior art, the invention has the advantages and beneficial effects that:
1. the method controls the growth rate of crystals and prevents particles from coagulating by adding the crystal form control agent and the composite organic metal scale inhibitor in the initial reaction stage and regulating and controlling the initial reaction temperature and gas concentration, and further prevents agglomeration by adding the surfactant in the later reaction stage, so that the nano-scale and micron-scale spindle-shaped calcium carbonate with narrow particle size distribution and excellent dispersibility is successfully prepared.
2. The calcium carbonate prepared by the invention has a spindle-shaped structure, narrow particle size distribution, uniform appearance, uniform particle size and good dispersibility, and is easy to realize industrial production.
3. The method has the advantages of simple and feasible process, low production cost, high production efficiency and better economic and social benefits.
Drawings
FIG. 1 is a 50000 SEM photograph of calcium carbonate of example 1;
FIG. 2 is a 500-magnification SEM photograph of calcium carbonate of example 1;
FIG. 3 is an SEM photograph of calcium carbonate of example 2 at 20000 magnification;
FIG. 4 is a 500 SEM photograph of the calcium carbonate of example 2;
FIG. 5 is a 20000 SEM photograph of the product of comparative example 1;
FIG. 6 is a 500-magnification SEM photograph of the product of comparative example 1.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments. It should be emphasized that the following description is merely exemplary in nature and is not intended to limit the scope of the invention or its application.
Example 1
A preparation method of spindle-shaped precipitated calcium carbonate comprises the following steps:
(1) taking active lime with activity degree and water with temperature of 30 ℃ to carry out digestion reaction according to the mass ratio of 2:11, stirring for 15min by a high-speed stirrer to obtain lime slurry, standing, sieving by a 100-mesh sieve to remove slag and refine, adjusting the solid content to 10%, and aging for 24h to obtain refined lime slurry for later use;
(2) conveying the refined lime slurry into a reaction kettle, adding a succinic acid crystal form control agent with the mass of 0.5 percent of the dry basis mass of calcium carbonate, starting stirring, starting jacket circulating water for controlling the temperature, controlling the temperature of the lime slurry to be 26 ℃, closing the circulating water, regulating the rotating speed to be 600r/min, introducing carbon dioxide with the concentration of 10 percent and the concentration of 1m3The mixed gas with flow rate per hour is subjected to carbonation reaction, and the calcium carbonate reaction is carried out to 5Adding polyaspartic acid accounting for 0.3 percent of the dry basis weight of calcium carbonate in min, stirring uniformly, continuing carbonization reaction, adjusting the concentration of carbon dioxide in the mixed gas to be 33 percent, continuing carbonization when the conductivity of the system is lowered to an inflection point, adding sodium lignosulfonate accounting for 1 percent of the dry basis weight of calcium carbonate in the mixed gas, continuing carbonization for 5min when the conductivity is lowered to 0.5ms/cm, stopping ventilation, and terminating the carbonization reaction to obtain calcium carbonate slurry;
(3) and (3) carrying out filter pressing on the calcium carbonate slurry, drying for 6h at 110 ℃, crushing, and sieving to obtain the spindle-shaped precipitated calcium carbonate product.
The 50000 times SEM pictures and 500 times SEM pictures of the calcium carbonate product of the embodiment are respectively shown in figures 1 and 2, and it can be seen from the figures that the calcium carbonate prepared by the invention has a spindle-shaped structure, narrow particle size distribution and uniform appearance.
Example 2
A preparation method of spindle-shaped precipitated calcium carbonate comprises the following steps:
(1) taking active lime with activity degree and water with temperature of 50 ℃ to carry out digestion reaction according to the mass ratio of 1:7, stirring for 20min by a high-speed stirrer to obtain lime slurry, standing, sieving by a 100-mesh sieve to remove slag and refine, adjusting the solid content to 8%, and aging for 24h to obtain refined lime slurry for later use;
(2) conveying the refined lime slurry into a reaction kettle, adding a tartaric acid crystal form control agent accounting for 0.2 percent of the dry basis weight of calcium carbonate, starting stirring, starting jacket circulating water for controlling the temperature, controlling the temperature of the lime slurry to be 40 ℃, closing the circulating water, regulating the rotating speed to be 600r/min, introducing carbon dioxide with the concentration of 10 percent and the concentration of 0.5m3Performing carbonation reaction on the mixed gas with flow rate/h, adding 0.2% polyacrylic acid and 0.1% polymaleic anhydride into calcium carbonate reaction for 5min, stirring uniformly, continuing the carbonation reaction, and simultaneously adjusting the concentration of carbon dioxide in the mixed gas to 33% and the flow rate to 2m3Continuing carbonization for every hour, adding hydroxymethyl cellulose with the mass being 1 percent of the dry basis mass of calcium carbonate when the conductivity of the system is lowered to an inflection point, continuing carbonization, and stopping ventilation to terminate the carbonation reaction after the conductivity is lowered to 0.5ms/cm for 5min to obtain calcium carbonate slurry;
(3) and (3) carrying out filter pressing on the calcium carbonate slurry, drying for 8h at 100 ℃, crushing, and sieving to obtain the spindle-shaped precipitated calcium carbonate product.
The 20000-fold SEM photograph and 500-fold SEM photograph of the calcium carbonate product of this example are shown in fig. 3 and 4, respectively, and it can be seen from the drawings that the calcium carbonate prepared by the present invention has a spindle-shaped structure, narrow particle size distribution and uniform morphology.
Example 3
A preparation method of spindle-shaped precipitated calcium carbonate comprises the following steps:
(1) taking active lime with activity degree and water with temperature of 40 ℃ to carry out digestion reaction according to the mass ratio of 1:8, stirring for 30min by a high-speed stirrer to obtain lime slurry, standing, sieving by a 100-mesh sieve to remove slag and refine, adjusting the solid content to 11.5%, and aging for 24h to obtain refined lime slurry for later use;
(2) conveying the refined lime slurry into a reaction kettle, adding a tartaric acid crystal type control agent accounting for 1 percent of the dry basis weight of calcium carbonate, starting stirring, starting jacket circulating water for controlling the temperature, controlling the temperature of the lime slurry to be 35 ℃, closing the circulating water, regulating the rotating speed to be 800r/min, introducing carbon dioxide with the concentration of 8 percent and the concentration of 1m3Carbonating the mixed gas with flow rate of/h for 10min, adding 0.8% polyacrylic acid, stirring, continuing carbonation reaction, and regulating carbon dioxide concentration to 40% and flow rate to 1m3Continuing carbonization for hours, adding calcium lignosulphonate with the mass of 2 percent of the dry basis mass of calcium carbonate to continue carbonization when the conductivity of the system is lowered to an inflection point, and then carbonizing for 3min after the conductivity is lowered to 0.5ms/cm, stopping ventilation to terminate the carbonation reaction to obtain calcium carbonate slurry;
(3) and (3) carrying out filter pressing on the calcium carbonate slurry, drying for 8h at 100 ℃, crushing, and sieving to obtain the spindle-shaped precipitated calcium carbonate product.
Example 4
A preparation method of spindle-shaped precipitated calcium carbonate comprises the following steps:
(1) taking active lime with activity degree and water with temperature of 50 ℃ to carry out digestion reaction according to the mass ratio of 1:6, stirring for 30min by a high-speed stirrer to obtain lime slurry, standing, sieving by a 100-mesh sieve to remove slag and refine, adjusting the solid content to 13.5%, and aging for 24h to obtain refined lime slurry for later use;
(2) conveying the refined lime slurry into a reaction kettle, adding tartaric acid accounting for 0.2 percent of the dry basis weight of calcium carbonate and a succinic acid crystal form control agent accounting for 0.3 percent of the dry basis weight of calcium carbonate, starting stirring, starting jacket circulating water to control the temperature, controlling the temperature of the lime slurry to be 45 ℃, closing the circulating water, regulating the rotating speed to be 500r/min, introducing carbon dioxide with the concentration of 20 percent and the concentration of 0.5m3Performing carbonation reaction on the mixed gas with flow rate/h, performing calcium carbonate reaction for 8min, adding 0.5% polyacrylic acid and 0.3% polyaspartic acid, stirring well, continuing carbonation reaction, and simultaneously adjusting the concentration of carbon dioxide in the mixed gas to 33% and the flow rate to 3m3Continuously carbonizing for one hour, adding sodium lignosulfonate accounting for 1 percent of the dry basis weight of calcium carbonate and 1 percent of hydroxyethyl cellulose to continuously carbonize when the conductivity of the system is lowered to an inflection point, carbonizing for 5min after the conductivity is lowered to 0.5ms/cm, stopping introducing air to terminate the carbonation reaction, and obtaining calcium carbonate slurry;
(3) and (3) carrying out filter pressing on the calcium carbonate slurry, drying for 6h at 120 ℃, crushing, and sieving to obtain the spindle-shaped precipitated calcium carbonate product.
Comparative example
Mixing active lime with activity degree of 200 with water at 30 ℃ according to a mass ratio of 2:11, stirring for 15min by a high-speed stirrer to obtain lime raw slurry, standing for 30min, sieving by a 100-mesh sieve for deslagging and refining, adjusting solid content to 10%, aging for 24h, and aging for 24h to obtain refined lime slurry to obtain refined lime for later use; starting circulating hot water until the temperature of lime slurry in the reaction kettle rises to 26 ℃, closing the circulating water, adjusting the stirring speed to 600r/min, introducing carbon dioxide with the concentration of 33% and the flow of 2m3The mixed gas/h is subjected to carbonation reaction. And (3) reducing the electric conductivity to 0.5ms/cm, starting timing, stopping ventilation after 5min to terminate the reaction to obtain calcium carbonate suspension slurry, dehydrating, drying at 110 ℃ for 6h, and crushing to obtain the calcium carbonate product. The electron micrographs of the resulting product are shown in FIGS. 5 and 6.
The calcium carbonate products prepared in examples 1 to 4 of the present invention were measured for particle size and specific surface area according to a conventional method, and the measurement results are shown in table 1.
Table 1: the calcium carbonate product prepared by the invention has the performance test result
From the above test results, it can be seen that the precipitated calcium carbonate in spindle form prepared by the method of the present invention has the advantages of adjustable specific surface area and small D97, indicating that the precipitated calcium carbonate in spindle form prepared by the method of the present invention has excellent dispersibility.
The foregoing is a more detailed description of the invention in connection with specific/preferred embodiments and is not intended to limit the practice of the invention to those descriptions. It will be apparent to those skilled in the art that various substitutions and modifications can be made to the described embodiments without departing from the spirit of the invention, and such substitutions and modifications are to be considered as within the scope of the invention.
Claims (7)
1. A preparation method of spindle-shaped precipitated calcium carbonate is characterized by comprising the following steps: the method comprises the following steps:
(1) taking active lime with the activity degree of 200-400 and water for a digestion reaction, stirring for 15-30min by a high-speed stirrer to obtain lime slurry, standing, sieving by a 100-mesh sieve for deslagging and refining, adjusting the solid content to 8-12%, and aging for 24h to obtain refined lime slurry for later use;
(2) conveying the refined lime slurry into a reaction kettle, adding a crystal form control agent accounting for 0.1-1% of the dry basis weight of calcium carbonate, starting stirring, starting jacket circulating water for controlling the temperature, controlling the temperature of the lime slurry to be 26-50 ℃, closing the circulating water, introducing mixed gas containing carbon dioxide for carbonation reaction, adding a composite organic metal scale inhibitor accounting for 0.1-1% of the dry basis weight of calcium carbonate after the calcium carbonate reaction is carried out for 5-10min, continuing the carbonation reaction after the lime slurry is uniformly stirred, adding a cellulose-based surfactant accounting for 0.3-3% of the dry basis weight of calcium carbonate for continuing the carbonation when the electrical conductivity of the system has a drop inflection point, and then carbonizing for 3-5min after the electrical conductivity is reduced to 0.5ms/cm, stopping introducing air and terminating the carbonation reaction to obtain calcium;
(3) the calcium carbonate slurry is subjected to filter pressing, drying, crushing and sieving to obtain a spindle-shaped precipitated calcium carbonate product;
the crystal form control agent is tartaric acid and/or succinic acid;
the composite organic metal scale inhibitor comprises one or a mixture of a plurality of polyacrylic acid, polymaleic anhydride and polyaspartic acid in any proportion;
the cellulose-based surfactant is one or a combination of more of hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, sodium lignosulfonate and calcium lignosulfonate.
2. The process for the preparation of spindle-shaped precipitated calcium carbonate according to claim 1, characterized in that: the mass ratio of the slaked reaction lime to the water is 1: 5-8.
3. The process for the preparation of spindle-shaped precipitated calcium carbonate according to claim 1, characterized in that: the digestion reaction is controlled at 30-60 ℃ and at a rotation speed of 150-300 r/min.
4. The process for the preparation of spindle-shaped precipitated calcium carbonate according to claim 1, characterized in that: the concentration of carbon dioxide in the mixed gas at the early stage of carbonation reaction for 5-10min is 5-20%, and the gas flow is 0.5-1m3H, then adjusting the concentration of carbon dioxide in the mixed gas to be 30-50%, and the flow rate to be 1-4m3H until the reaction is complete.
5. The process for the preparation of spindle-shaped precipitated calcium carbonate according to claim 4, characterized in that: the stirring speed of the carbonation reaction kettle is 500-800 r/min.
6. The process for the preparation of spindle-shaped precipitated calcium carbonate according to claim 5, characterized in that: the stirring paddle used by the carbonation reaction kettle is a straight-blade turbine type stirring paddle.
7. The process for the preparation of spindle-shaped precipitated calcium carbonate according to claim 1, characterized in that: the drying temperature is 100-120 ℃, and the drying time is 6-8 h.
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| CN109775742A (en) * | 2019-01-03 | 2019-05-21 | 浙江理工大学 | One kind preparing aragonite CaCO by lignin monomer model compound cinnamic acid regulation3Method |
| CN109650431A (en) * | 2019-01-07 | 2019-04-19 | 卢氏国嵩莱纳米科技有限公司 | A kind of preparation method of MS glue nanometer calcium carbonate |
| CN109574057B (en) * | 2019-01-14 | 2020-12-25 | 江油市万山矿业有限公司 | Preparation method of calcium carbonate |
| CN110372024A (en) * | 2019-08-28 | 2019-10-25 | 广西合山市华纳新材料科技有限公司 | A kind of preparation method of plastics submicron order rice particle shape calcium carbonate |
| CN112209417B (en) * | 2019-08-28 | 2022-04-19 | 浙江天石纳米科技股份有限公司 | Preparation method of light calcium carbonate powder for papermaking coating |
| CN110817923A (en) * | 2019-12-13 | 2020-02-21 | 贺州学院 | Preparation method of fusiform vaterite calcium carbonate |
| CN113087004A (en) * | 2021-04-14 | 2021-07-09 | 上海抚翌科技有限公司 | Production method of calcium carbonate in cigarette paper |
| CN114349036B (en) * | 2021-11-01 | 2023-11-24 | 山东宇信纳米科技有限公司 | Preparation method of nano calcium carbonate for MS glue |
| CN116375071A (en) * | 2023-03-30 | 2023-07-04 | 苏州盛耀塑胶新材料有限公司 | Production process of superfine calcium carbonate |
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| CN1112320C (en) * | 2000-01-18 | 2003-06-25 | 北京化工大学 | Process for preparing calcium carbonate deposit by continuous method |
| CN1429772B (en) * | 2001-12-31 | 2010-12-08 | 纳米材料科技有限公司 | Method for preparing calcium carbonate with actual forms |
| CN101538059B (en) * | 2009-04-17 | 2011-06-15 | 北京工业大学 | Preparation method of superstructure aragonite calcium carbonate crystal |
| CN103539186A (en) * | 2013-09-28 | 2014-01-29 | 昆山市周市溴化锂溶液厂 | Preparation method of fusiform light calcium carbonate |
| CN106082295B (en) * | 2016-06-08 | 2017-05-31 | 江西广源化工有限责任公司 | A kind of individual layer pyrophillite modified superfine powdered whiting and preparation method thereof |
| CN106832660A (en) * | 2017-01-09 | 2017-06-13 | 广西华纳新材料科技有限公司 | A kind of method that rod-like precipitates calcium carbonate improves hard PVC section bar performance |
| CN107555459A (en) * | 2017-09-13 | 2018-01-09 | 泰兴市诚盛化工有限公司 | A kind of preparation method of nanometer of spindle winnofil |
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