CN112441605A - Preparation method of vermicular precipitated calcium carbonate - Google Patents
Preparation method of vermicular precipitated calcium carbonate Download PDFInfo
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Abstract
The invention discloses a preparation method of vermicular precipitated calcium carbonate, which comprises the steps of carrying out digestion reaction on quick lime, and adjusting specific gravity to obtain a calcium hydroxide suspension; adding salt of magnesium, strontium or barium element or compound thereof serving as a crystal form control agent into the suspension, stirring and mixing uniformly, adding into a carbonization tower, introducing mixed gas containing carbon dioxide to perform calcium carbonate reaction until the pH value is reduced to 9.0, and stopping carbonation to obtain PCC suspension; slowly adding phosphoric acid solution into the PCC suspension until the pH value is reduced to 7.0, stopping the reaction, standing, and then carrying out filter pressing, drying, crushing and grading on the suspension according to a conventional method to obtain the vermicular precipitated calcium carbonate powder. The method controls the final end point of the reaction by adding the salt of magnesium, strontium or barium or the compound thereof as a crystal form control agent, and adjusts the final pH value by using phosphoric acid, so that the obtained vermicular precipitated calcium carbonate has the advantages of high purity, high whiteness, high specific surface area and the like.
Description
Technical Field
The invention belongs to the technical field of inorganic materials, and particularly relates to a preparation method of vermicular precipitated calcium carbonate.
Background
Calcium carbonate is used as an environment-friendly inorganic material and has wide application. Because the calcium carbonate raw material is low in acquisition cost, the production cost is mature compared with the related technology, and the calcium carbonate is used as the filler, so that the mechanical property, the appearance effect and the structure adjustment of the product can be improved, the cost of the product is greatly reduced, and the like, and the calcium carbonate can be applied to the fields of rubber, plastics, papermaking, printing ink, plastics and the like. The calcium carbonate is applied to coatings, sealants and the like, and calcium carbonate particles with good dispersion can form a good space site structure, so that the anti-sagging performance and the mechanical property of products are improved, and the calcium carbonate has important significance in automotive coatings, building adhesives and the like. The calcium carbonate is applied to paper making, plastics and the like, not only can the mechanical property of products be improved, but also the advantages of the calcium carbonate in whiteness can be fully shown, and the products can be conveniently colored; and part of special shapes, such as spherical calcium carbonate, can be applied to printing ink, lubricating oil and the like because of better wear resistance. At present, the shapes of precipitated calcium carbonate on the market mainly include cubic, spherical, spindle-shaped, chain-shaped, needle-shaped and sheet-shaped shapes, and the preparation methods or processes of precipitated calcium carbonate with different shapes can be different. The application fields of calcium carbonate with different morphologies are gradually explored, and the research and preparation of calcium carbonate with various morphologies have important significance. At present, precipitated calcium carbonate of various morphologies has been studied and is being applied to industrial production in a mature manner.
Patent CN107555459A discloses a preparation method of nano spindle precipitated calcium carbonate, which is characterized in that limestone is calcined, digested and refined, then a mixture of a composite crystal form control agent sodium bis (2-ethylhexyl) succinate sulfonate and zinc sulfate with the mass ratio of 1-3:1 is added, CO is introduced2Adding sodium polyacrylate, sodium polymethacrylate, maleic acid-acrylic acid copolymer sodium salt and other dispersing agents when the mixture is carbonated to the conductivity of 1.0-2.0 mS/cm to obtain the nano spindle precipitated calcium carbonate. The sodium sulfosuccinate is added in the method, so that more bubbles are generated during carbonation, the materials in the carbonation tower overflow during carbonation, and accidents are easily caused during pilot plant test or industrial production. In addition, the method is complicated in adding a crystal form control agent, a dispersing agent and the like, and is not favorable for the stability of the product. The morphology of the calcium carbonate prepared by the method is not vermicular calcium carbonate.
Patent CN111153424A discloses a method for preparing pinecone-shaped calcium carbonate, which comprises dissolving a certain amount of anhydrous calcium chloride in deionized water to prepare solutions with different concentrations, and then adding 2% of crystal form control agent to form a solution A; dissolving a certain amount of anhydrous sodium carbonate in deionized water to prepare solutions with different concentrations, and adding a certain amount of anhydrous ethanol solution to form a solution B; and (3) placing the solution A and the solution B in a constant-temperature water bath at 45 ℃, stirring for 0.5h, quickly pouring the constant-temperature solution B into the solution A, stirring strongly for 2h, and performing centrifugal separation, suction filtration, washing, drying and grinding to obtain the pinecone-shaped calcium carbonate powder. The method uses double decomposition method to prepare the pinecone-shaped calcium carbonate, the preparation conditions are harsh, the industrial production is difficult, and the prepared calcium carbonate is non-worm-shaped.
The patent CN110366539A provides a calcium carbonate with small particle size and easy dispersion in polymer and a preparation method thereof, wherein the content of calcium carbonate and magnesium carbonate is 12000-120000 ppm, and the specific surface area is 60-120 m2The crystallite size of the (104) surface is 20-50 nm, and the particles are connected into a chain shape. The method is an invention of Japan industrial company, adds a proper amount of magnesium hydroxide before carbonating to prepare chain calcium carbonate, and dehydrates and dries after surface treatment to obtain the chain calcium carbonate which has good dispersion and good elongation when being applied to rubber. However, the morphology prepared by the method is calcite chain-shaped and is not vermicular calcium carbonate.
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 vermicular precipitated calcium carbonate. The method controls the final end point of the reaction by adding the salt of magnesium, strontium or barium or the compound thereof as a crystal form control agent, and adjusts the final pH value by using phosphoric acid, so that the obtained vermicular precipitated calcium carbonate has the advantages of high purity, high whiteness, high specific surface area and the like.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a method for preparing vermicular precipitated calcium carbonate, comprising the following steps:
(1) slaking and reacting quicklime to obtain lime milk, and adjusting the specific gravity of the lime milk to 1.045-1.065 to obtain a calcium hydroxide suspension;
(2) adding salt of magnesium, strontium or barium element or compound thereof serving as a crystal form control agent into the calcium hydroxide suspension, stirring and mixing uniformly, adding into a carbonization tower, introducing mixed gas containing carbon dioxide for carbonation reaction, and stopping carbonation until the pH value is reduced to 9.0 to obtain PCC suspension;
(3) slowly adding phosphoric acid solution into the PCC suspension until the pH value is reduced to 7.0, stopping the reaction, standing for 10-30min, and then carrying out filter pressing, drying, crushing and grading on the suspension according to a conventional method to obtain vermicular precipitated calcium carbonate powder.
Further, the crystal form control agent is one or a combination of more of magnesium chloride, magnesium oxide, magnesium hydroxide, calcium magnesium hydroxide, strontium chloride, strontium oxide, strontium nitrate, strontium cyanide, barium chloride, barium oxide, barium nitrate and barium acetate.
Furthermore, the dosage of the crystal form control agent is 0.2-0.5mol per 15kg of calcium hydroxide suspension, and the crystal form control agent is prepared into the calcium hydroxide suspension with water to have the concentration of 1-8 mol/L. Preferably, the crystal form control agent consists of 0.1mol of magnesium chloride and 0.2mol of strontium chloride; or 0.4mol of magnesium bicarbonate and 0.1mol of barium chloride; or 0.5mol of strontium nitrate and 0.3mol of strontium cyanide.
Further, the mass concentration of the phosphoric acid is 5%.
Further, the adding speed of the phosphoric acid is 200-300 ml/min.
Further, the initial carbonization temperature of the calcium hydroxide suspension in the carbonation reaction process is 20.0-24.0 ℃, the concentration of the carbon dioxide mixed gas is 30-33%, and the gas inlet flow is 2.0-2.4m3The stirring frequency was 20 Hz.
Compared with the prior art, the invention has the advantages and beneficial effects that:
1. according to the method, the salt of magnesium, strontium or barium or the compound thereof is used as a crystal form control agent to form carbonate, the application effect of calcium carbonate is not influenced, phosphoric acid is added in the later stage of reaction to control PH, the accurate control means of the carbonation end point is realized, the liquid phase residual substance is treated in the later stage, the product is more stable, calcium phosphate with smaller particles can be formed, the defect of the surface of calcium carbonate is favorably filled, the obtained calcium carbonate is vermiform in appearance, high in purity, high in whiteness and high in specific surface area, and the obtained calcium carbonate has potential application prospects in the fields of papermaking, plastics, rubber, medical treatment, biological pharmacy, daily chemicals and the like.
2. The method adopts the traditional bubbling carbonation process, has simple process and mature technology, and is beneficial to the industrialized application of the vermicular calcium carbonate; the adopted crystal form control agent is easy to obtain and low in price, and the use of the crystal form control agent does not have any pollution, environmental protection and safety problems.
Drawings
FIG. 1 is a 150000 SEM image of the vermicular precipitated calcium carbonate product obtained in example 1.
FIG. 2 is a 100000 SEM image of the vermicular precipitated calcium carbonate product made in example 1.
FIG. 3 is a 10000-fold SEM image of the vermicular precipitated calcium carbonate product made in example 1.
FIG. 4 is a 150000 SEM image of the vermicular precipitated calcium carbonate product obtained in example 2.
Figure 5 is a 100000 SEM image of the vermicular precipitated calcium carbonate product made in example 2.
Figure 6 is a 100000 SEM image of the vermicular precipitated calcium carbonate product made in example 3.
Figure 7 is a 100000 SEM image of the vermicular precipitated calcium carbonate product made in example 4.
FIG. 8 is a 100000 SEM image of the vermicular precipitated calcium carbonate product of example 5.
Figure 9 is a 100000 SEM image of the non-vermicular precipitated calcium carbonate product made in 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 method for preparing vermicular precipitated calcium carbonate, comprising the following steps:
(1) slaking and reacting quicklime to obtain lime milk, and regulating the specific gravity of the lime milk to 1.050 to obtain calcium hydroxide suspension;
(2) taking 15kg of calcium hydroxide suspension, adding 0.1mol of magnesium chloride and 0.2mol of strontium chloride into the suspension to prepare a solution with a cation molar concentration of 1mol/L as a crystal form control agent, uniformly stirring and mixing the solution, adding the solution into a carbonization tower, controlling the stirring speed to be 20Hz and the carbonization starting temperature to be 21.0 ℃, introducing carbon dioxide mixed gas with the concentration of 30 percent into the suspension, wherein the flow rate is 2.0m3Stopping carbonation until the pH drops to 9.0 to obtain a PCC suspension;
(3) adding a phosphoric acid solution with the mass concentration of 5% into the PCC suspension at the speed of 220ml/min until the pH value is reduced to 7.0, stopping the reaction, standing for 10min, and then carrying out filter pressing, drying, crushing and grading on the suspension according to a conventional method to obtain the vermicular precipitated calcium carbonate powder.
The precipitated calcium carbonate powder prepared in this example is detected by scanning electron microscopy under different multiples, and the detection results are shown in fig. 1, fig. 2, and fig. 3, and it can be seen from the figures that the prepared calcium carbonate powder is vermiform, and has the characteristics of regular morphology, uniform particle size distribution, and good dispersibility.
Example 2
A method for preparing vermicular precipitated calcium carbonate, comprising the following steps:
(1) slaking and reacting quicklime to obtain lime milk, and regulating the specific gravity of the lime milk to 1.060 to obtain calcium hydroxide suspension;
(2) taking 15kg of calcium hydroxide suspension, adding 0.3mol of magnesium oxide into the suspension to prepare a solution with the concentration of 3mol/L as a crystal form control agent, uniformly stirring and mixing the solution, adding the solution into a carbonization tower, and controlling the stirring speedThe rate is 20Hz, the carbonization starting temperature is 23.0 ℃, and carbon dioxide mixed gas with the concentration of 31 percent is introduced into the suspension, and the flow rate is 2.0m3Stopping carbonation until the pH drops to 9.0 to obtain a PCC suspension;
(3) adding 5% phosphoric acid solution into the PCC suspension at a rate of 250ml/min until the pH value is reduced to 7.0, stopping the reaction, standing for 20min, and performing filter pressing, drying, crushing and grading on the suspension according to a conventional method to obtain the vermicular precipitated calcium carbonate powder.
The precipitated calcium carbonate powder prepared in this example is detected by scanning electron microscopy under different multiples, and the detection result is shown in fig. 4 and 5, and it can be seen from the figure that the prepared calcium carbonate powder is vermiform, and has the characteristics of regular morphology, uniform particle size distribution, and good dispersibility.
Example 3
A method for preparing vermicular precipitated calcium carbonate, comprising the following steps:
(1) slaking and reacting quicklime to obtain lime milk, and adjusting the specific gravity of the lime milk to 1.065 to obtain calcium hydroxide suspension;
(2) taking 15kg of calcium hydroxide suspension, adding 0.4mol of magnesium bicarbonate and 0.1mol of barium chloride into the suspension to prepare a solution with a cation concentration of 5mol/L as a crystal form control agent, uniformly stirring and mixing the solution, adding the solution into a carbonization tower, controlling the stirring rate to be 20Hz and the carbonization starting temperature to be 24 ℃, introducing a carbon dioxide mixed gas with the concentration of 33 percent into the suspension, wherein the flow rate is 2.2m3Stopping carbonation until the pH drops to 9.0 to obtain a PCC suspension;
(3) adding phosphoric acid solution with mass concentration of 5% into the PCC suspension at the speed of 280ml/min until the pH value is reduced to 7.0, stopping the reaction, standing for 30min, and then carrying out filter pressing, drying, crushing and grading on the suspension according to a conventional method to obtain the vermicular precipitated calcium carbonate powder.
The precipitated calcium carbonate powder prepared in the embodiment is detected by a scanning electron microscope, and the detection result is shown in fig. 6, and it can be seen from the figure that the prepared calcium carbonate powder is vermiform, regular in morphology, uniform in particle size distribution and good in dispersibility.
Example 4
A method for preparing vermicular precipitated calcium carbonate, comprising the following steps:
(1) slaking and reacting quicklime to obtain lime milk, and regulating the specific gravity of the lime milk to 1.060 to obtain calcium hydroxide suspension;
(2) taking 15kg of calcium hydroxide suspension, adding 0.5mol of strontium nitrate and 0.3mol of strontium cyanide into the suspension to prepare a solution with a cation concentration of 8mol/L as a crystal form control agent, uniformly stirring and mixing the solution, adding the solution into a carbonization tower, controlling the stirring rate to be 20Hz and the carbonization starting temperature to be 20 ℃, introducing 32 percent carbon dioxide mixed gas into the suspension, wherein the flow rate is 2.0m3Stopping carbonation until the pH drops to 9.0 to obtain a PCC suspension;
(3) adding phosphoric acid solution with mass concentration of 5% into the PCC suspension at a speed of 240ml/min until the pH value is reduced to 7.0, stopping the reaction, standing for 10min, and then carrying out filter pressing, drying, crushing and grading on the suspension according to a conventional method to obtain the vermicular precipitated calcium carbonate powder.
The precipitated calcium carbonate powder prepared in this example is detected by a scanning electron microscope, and the detection result is shown in fig. 7, and it can be seen from the figure that the prepared calcium carbonate powder is vermiform, regular in morphology, uniform in particle size distribution, and good in dispersibility.
Example 5
A method for preparing vermicular precipitated calcium carbonate, comprising the following steps:
(1) slaking and reacting quicklime to obtain lime milk, and regulating the specific gravity of the obtained lime milk to 1.055 to obtain calcium hydroxide suspension;
(2) taking 15kg of calcium hydroxide suspension, adding 0.3mol of barium nitrate and 0.3mol of barium acetate into the suspension to prepare a solution with the cation concentration of 6mol/L as a crystal form control agent, uniformly stirring and mixing the solution, adding the solution into a carbonization tower, controlling the stirring rate to be 20Hz and the carbonization starting temperature to be 20 ℃, introducing 32 percent carbon dioxide mixed gas into the suspension, wherein the flow rate is 2.3m3Stopping carbonation until the pH drops to 9.0 to obtain a PCC suspension;
(3) adding phosphoric acid solution with mass concentration of 5% into the PCC suspension at a speed of 240ml/min until the pH value is reduced to 7.0, stopping the reaction, standing for 10min, and then carrying out filter pressing, drying, crushing and grading on the suspension according to a conventional method to obtain the vermicular precipitated calcium carbonate powder.
The precipitated calcium carbonate powder prepared in this example is detected by a scanning electron microscope, and the detection result is shown in fig. 8, and it can be seen from the figure that the prepared calcium carbonate powder is vermiform, regular in morphology, uniform in particle size distribution, and good in dispersibility.
Comparative example 1
(1) Slaking quicklime to prepare lime milk, and preparing the lime milk with the specific gravity of 1.060;
(2) taking 15kg of the calcium hydroxide suspension prepared in the S1; adding into a carbonization tower, stirring well at a stirring rate of 20Hz, controlling the carbonization starting temperature to be 21.0 ℃, introducing carbon dioxide gas mixture with the concentration of 30% into the suspension, and the flow rate is 2m3Stopping carbonation until the pH drops to 7.0 to obtain a PCC suspension;
(3) and then carrying out filter pressing, drying, crushing and grading on the suspension to obtain precipitated calcium carbonate powder.
The precipitated calcium carbonate powder prepared by the example is detected by a scanning electron microscope, and the detection result is shown in fig. 9, wherein the precipitated calcium carbonate prepared by the conventional method is not vermiform and has irregular appearance.
TABLE 1 detection data of vermicular precipitated calcium carbonate
| Sample (I) | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 |
| CaCO3Ingredients (a) of | 98.3 | 98.5 | 97.4 | 96.8 | 98.2 | 95.4 |
| Whiteness degree% | 96.8 | 96.2 | 95.4 | 96.3 | 95.6 | 94.1 |
| BET, m2/g | 32.44 | 29.31 | 27.20 | 30.02 | 30.51 | 23.63 |
The detection results of the vermicular precipitated calcium carbonate prepared in this example are shown in table 1, and it can be seen from the detection results that the obtained precipitated calcium carbonate has high purity, whiteness and specific surface area.
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 method for preparing vermicular precipitated calcium carbonate, which is characterized by comprising the following steps: the method comprises the following steps:
(1) slaking and reacting quicklime to obtain lime milk, and adjusting the specific gravity of the lime milk to 1.045-1.065 to obtain a calcium hydroxide suspension;
(2) adding salt of magnesium, strontium or barium element or compound thereof serving as a crystal form control agent into the calcium hydroxide suspension, stirring and mixing uniformly, adding into a carbonization tower, introducing mixed gas containing carbon dioxide for carbonation reaction, and stopping carbonation until the pH value is reduced to 9.0 to obtain PCC suspension;
(3) slowly adding phosphoric acid solution into the PCC suspension until the pH value is reduced to 7.0, stopping the reaction, standing for 10-30min, and then carrying out filter pressing, drying, crushing and grading on the suspension according to a conventional method to obtain vermicular precipitated calcium carbonate powder.
2. The process for the preparation of vermicular precipitated calcium carbonate according to claim 1, characterized in that: the crystal form control agent is one or a combination of more of magnesium chloride, magnesium oxide, magnesium hydroxide, calcium magnesium hydroxide, strontium chloride, strontium oxide, strontium nitrate, strontium cyanide, barium chloride, barium oxide, barium nitrate and barium acetate.
3. The process for the preparation of vermicular precipitated calcium carbonate according to claim 2, characterized in that: the dosage of the crystal form control agent is 0.1-0.8mol added into every 15kg of calcium hydroxide suspension, and the concentration of the crystal form control agent is 1-8mol/L prepared by water.
4. A process for the preparation of vermicular precipitated calcium carbonate according to claim 3, characterized in that: the crystal form control agent consists of 0.1mol of magnesium chloride and 0.2mol of strontium chloride; or 0.4mol of magnesium bicarbonate and 0.1mol of barium chloride; or 0.5mol of strontium nitrate and 0.3mol of strontium cyanide.
5. The process for the preparation of vermicular precipitated calcium carbonate according to claim 1, characterized in that: the mass concentration of the phosphoric acid is 5%.
6. The process for the preparation of vermicular precipitated calcium carbonate according to claim 5, characterized in that: the addition rate of the phosphoric acid is 200-300 ml/min.
7. The process for the preparation of vermicular precipitated calcium carbonate according to claim 1, characterized in that: the initial carbonization temperature of the calcium hydroxide suspension in the carbonation reaction process is 20.0-24.0 ℃, the concentration of the carbon dioxide mixed gas is 30-33%, and the gas inlet flow is 2.0-2.4m3The stirring frequency was 20 Hz.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114853049A (en) * | 2022-05-30 | 2022-08-05 | 广西华纳新材料股份有限公司 | Preparation method of high-stability nano calcium carbonate |
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