CN109809457B - Regular spherical calcium carbonate and preparation process thereof - Google Patents
Regular spherical calcium carbonate and preparation process thereof Download PDFInfo
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Abstract
The invention discloses regular spherical calcium carbonate and a preparation process thereof, wherein the preparation method comprises the following steps: adding a composite crystal form control agent into the refined and prepared calcium hydroxide slurry, uniformly stirring, regulating and controlling the initial carbonization temperature, introducing carbon dioxide gas for carbonization until the pH value is lower than 7, dehydrating, drying, crushing and screening to obtain the regular spherical calcium carbonate. The regular spherical calcium carbonate obtained by the invention does not need surface treatment, has good dispersibility, simple process, short carbonization time and low production cost, can be adjusted and controlled in the range of the particle size of 300-plus-900 nm, has good processing fluidity as a downstream product filler, has higher added value as a template material of hollow particles, and is suitable for the light industry of food, medicine and cosmetics, as well as the industries of plastics, rubber, coating, printing ink, paper making, new materials and chemical industry.
Description
Technical Field
The invention belongs to the technical field of preparation of inorganic non-metallic material calcium carbonate powder, and particularly relates to calcium carbonate with regular spherical vaterite crystal form crystal morphology prepared from calcium hydroxide and a process thereof.
Background
Calcium carbonate products with different forms have different application fields and functions. The function of the calcium carbonate is good or bad and mainly depends on the parameters of the calcium carbonate product such as chemical composition, morphological characteristics, particle size and the like, wherein the most important is the crystal form and the particle size distribution of calcium carbonate particles. At present, the special crystal form nanometer calcium carbonate product is prepared by artificially controlling the crystallization of calcium carbonate, so that the higher application performance and the added value of the product are still hot spots for the development of the calcium carbonate industry. Among various nano calcium carbonate products with special crystal forms, spherical calcium carbonate has a simpler structure, smaller stacking volume, lower oil absorption value, good opacity (coverage degree) and good ink absorption performance, so the nano calcium carbonate is mainly used in industries such as papermaking and the like. In addition, the spherical calcium carbonate has the characteristics of good smoothness, flowability and the like, and is widely applied to industries such as rubber, paint, high-grade ink and the like.
In recent years, researches show that the hollow particles are a novel material with a special cavity structure, due to the special geometric structure and the physical and chemical properties such as high internal space, low density, large specific surface area, good stability, strong surface permeability and the like, the hollow particles have attracted attention in the field of scientific research, and have good application prospects in the fields of medicine, catalysis, materials and the like. Different templates have different advantages and disadvantages, the calcium carbonate raw material is cheap and easy to obtain, the preparation method is simple, and the calcium carbonate is easy to remove, so that the spherical calcium carbonate is considered as a template material with great potential.
The preparation research of the domestic spherical calcium carbonate has made some progress, the CaCO is prepared3The conventional methods for particles are mainly a double decomposition method and a carbonization method. The double decomposition method has the advantages of simple preparation method and easy control of CaCO3The crystal form, the morphology and the particle size of the particles, but the defects are that the production cost is higher, the production efficiency is lower, and the large-scale industrial production cannot be realized at present. The carbonization method is used for preparing CaCO with specific appearance in the current industrial production3The main method of the product. The method is divided into an intermittent bubbling carbonization method and an intermittent stirring carbonization method according to different contact modes in the carbonization process, wherein the intermittent bubbling carbonization method is simple to operate but has high energy consumption and poor particle size uniformity, and the intermittent stirring carbonization method has the characteristics of low production cost, uniform particle size distribution, short carbonization time and the like, and has high equipment investment although the operation is relatively complicated and the particle size uniformity of products is relatively high. The existing spherical calcium carbonate product is basically used in industries such as papermaking, rubber, coating, high-grade ink and the like, the price of the product is about thousand yuan per ton, and the product cannot be used as a template material for preparing hollow particles due to large particle size. As the submicron (500-800nm) spherical calcium carbonate particles serving as template materials for preparing hollow particles are easy to remove, the price reaches 400 yuan/kg at present, and the industrialization of such high-added-value refined calcium carbonate products is almost in a blank state, therefore, a carbonization method is developed to prepare submicron spherical calcium carbonate serving as a template agent, and spherical calcium carbonate products which have stable performance and meet different requirements are prepared by improving a carbonization process so as to meet the continuously increasing market requirements, and the method has positive significance for improving the added value of the calcium carbonate products.
Disclosure of Invention
The invention provides regular spherical calcium carbonate and a preparation process thereof, which solves the technical problem of the preparation process for submicron (500-800nm) spherical calcium carbonate particles serving as template materials of hollow particles.
In order to solve the technical problems, the invention adopts the following technical scheme:
a regular spherical calcium carbonate belongs to the preparation of spherical calcium carbonate by calcium hydroxide carbonization, which comprises the steps of firstly preparing calcium hydroxide slurry, then adding a composite crystal form control agent into the calcium hydride slurry, fully stirring and mixing, adjusting the initial carbonization temperature, then introducing carbon dioxide gas for carbonization, dehydrating, drying, crushing and screening the obtained calcium carbonate slurry to obtain the regular spherical calcium carbonate, wherein the preparation method comprises the following steps:
1) slaking lime, refining and preparing into calcium hydroxide slurry;
2) adding a composite crystal form control agent into the prepared calcium hydroxide slurry;
3) adjusting the initial carbonization temperature of the calcium hydroxide slurry, introducing carbon dioxide gas for carbonization reaction, judging that the reaction is finished when the pH is lower than 7, and stopping introducing the carbon dioxide gas;
4) and after the carbonization reaction is finished, dehydrating, drying, crushing and screening to obtain the regular spherical calcium carbonate.
Furthermore, the regular spherical calcium carbonate crystal form is a mixed crystal form of a vaterite crystal form and a calcite crystal form, the crystal morphology is regular spheres, the vaterite crystal form in the mixed crystal form is a high-content main constituent part, the calcite crystal form is a low-content secondary constituent part, the regular spherical calcium carbonate has the particle size of 300-900 nm, the particle size is uniform, and the particle size is controllable.
Further, the regular spherical calcium carbonate can be uniform, regular and complete spherical calcium carbonate or regular spherical calcium carbonate containing partial crushed ball calcium, which is formed unevenly due to the fact that reaction conditions and process parameters are not controlled.
Further, lime in the step 1) can be directly digested by water, or can be digested by mixing water with methanol or ethanol according to a certain proportion, or can be digested by mixing water, methanol and ethanol according to a certain proportion, or can be digested by preparing and dehydrating clear liquid for digestion by regular ball calcium carbonate; after lime slaking and refining, the content of calcium hydroxide in the prepared calcium hydroxide slurry is 4-16%, and the content of methanol or ethanol or the mixture of the methanol and the ethanol in the calcium hydroxide slurry is 25-80% of the mass of the calcium hydroxide slurry; in order to reduce the volatilization loss of methanol and ethanol caused by the heat release of digestion, the methanol and the ethanol are preferably digested with water and refined, and then the methanol or the ethanol or the mixture of the methanol and the ethanol is proportionally added to adjust the required concentration ratio.
Further, in the step 2), a composite crystal form control agent is added into the prepared calcium hydroxide slurry, wherein the composite crystal form control agent is divided into two components, one component is a calcium carbonate crystal form directing agent, and the other component is a calcium carbonate morphology control agent; the crystal form directing agent is used as a coagulant for coagulating the vaterite crystal into balls, and the morphology control agent is used as a spherical calcium carbonate morphology regulator for regulating the morphology of calcium carbonate particles to tend to be complete spheres; the crystal form directing agent is one or a plurality of compounds of soluble starch slurry, polyvinylpyrrolidone, sodium polyvinylbenzene sulfonate and polyethyleneimine which are heated and cured; the crystal form regulating agent is one or more compounds of sodium polyacrylate, polysorbate, sodium polyaspartate and sorbitan fatty acid ester; the amount of the crystal form directing agent added is 0.5-8% of the solid content of calcium hydroxide, and the amount of the crystal form controlling agent added is 0.6-10% of the solid content of calcium hydroxide.
Furthermore, it is desirable to add the crystal form directing agent in an amount of 1-6% based on the total preparation cost and preparation efficiency, and exceeding the above range will have an effect on the preparation cost and efficiency and still fall within the scope of the claims.
Further, in the stirring carbonization device in the step 3), adding the composite crystal form control agent into the calcium hydroxide slurry, uniformly stirring, adjusting the initial carbonization temperature to 3-40 ℃, introducing gas with the carbon dioxide gas concentration of 20-100% under the stirring state, carrying out carbonization reaction until the pH value is lower than 7, and stopping introducing the gas to finish carbonization.
Further, stopping introducing gas in the step 3), stopping stirring after carbonization is finished, waiting for the slurry to form gel, and waiting for the gel to melt after the gel is formed or accelerating the gel to melt by appropriate heating. The pH value of the slurry is lower than 7, the slurry is subjected to carbonization to form calcium carbonate and calcium bicarbonate mixed slurry, and after the gas introduction is stopped, the calcium bicarbonate is decomposed to form calcium carbonate and carbon dioxide gas which are released to form bubbles in the sol gelling process.
Furthermore, after the gel is dissolved, calcium carbonate filter cakes can be obtained by filtering or centrifugal dehydration, and the regular spherical calcium carbonate can be obtained by drying, crushing and screening the filter cakes.
Further, filtrate obtained by dehydrating the calcium carbonate slurry in the step 4) can be recycled after precipitation, filtration and clarification.
The invention has the following beneficial effects:
1. the lime reacts with water to effectively convert the quick lime into slaked lime calcium hydride slurry, and the cost for preparing the calcium hydroxide slurry is greatly reduced in the processes of lime slaking and calcium hydroxide slurry screening, impurity removal and refining by taking water as a solvent to dissolve calcium oxide.
2. The refined calcium hydroxide slurry is added with methanol or ethanol or a mixture of the methanol and the ethanol, so that the dissolution of carbon dioxide in the calcium hydroxide slurry can be effectively accelerated, the carbonation reaction can be effectively promoted, and the formation of the vaterite crystal form calcium carbonate can be promoted.
3. The vaterite crystal form calcium carbonate has better stability in methanol and ethanol solution, and the regular spherical calcium carbonate is more favorably formed under the action of the composite crystal form control agent under the condition that the vaterite is not converted into the calcite crystal form.
4. The method has the characteristics of simple process design, easy implementation of mass production, low process cost, short carbonization reaction time and easy operation and control, and the regular spherical calcium carbonate produced by the method has uniform grain diameter and stable product quality.
5. The regular spherical calcium carbonate prepared by the method has controllable particle size, has good processing fluidity as a downstream product filler, has higher added value as a template material of hollow particles, and is suitable for the light industry of food, medicine and cosmetics, and also suitable for the industries of plastics, rubber, coating, printing ink, papermaking, new materials and chemical industry.
Drawings
FIG. 1 is a scanning electron microscope analysis chart of the regular spherical calcium carbonate product prepared in example 1;
FIG. 2 is a scanning electron microscope analysis chart of the regular spherical calcium carbonate product prepared in example 2.
Detailed Description
In order to facilitate a better understanding of the invention, the following examples are given to illustrate, but not to limit the scope of the invention.
Example 1
A regular spherical calcium carbonate belongs to a spherical calcium carbonate prepared by a calcium hydroxide carbonization method, and the preparation method comprises the following steps:
(1) lime slaking and calcium hydroxide slurry preparation: fully stirring and digesting lime and water at a mass ratio of 1:4 at room temperature, properly aging and cooling, filtering the obtained lime slurry to remove large particles of insoluble matters and impurities to obtain refined calcium hydroxide slurry, adding methanol to regulate the content of calcium hydroxide to 10% after the calcium hydroxide slurry is cooled to room temperature, wherein the adding amount of the methanol is 50% of the mass of the regulated calcium hydroxide slurry;
(2) adding a crystal form control agent: pumping the debugged calcium hydroxide slurry into an intermittent bubbling carbonization tower with a stirring device by using a pump, adding a heated and cured soluble starch solution with the mass of 3.8 percent of the mass of the calcium hydroxide as a crystal form directing agent, adding polyoxyethylene (20) sorbitan monolaurate with the mass of 3.0 percent of the mass of the calcium hydroxide as a shape control agent, and uniformly stirring;
(3) carbonizing: adjusting the initial carbonization temperature of the calcium hydroxide slurry to 10 ℃, opening a gas valve, introducing pure carbon dioxide-containing gas for carbonization reaction, closing the gas valve when the pH of the reaction solution is 6.9 after carbonization, stopping the reaction, and stopping stirring;
(4) and (3) dehydrating and drying: after the calcium carbonate slurry is gelled and dissolved, the regular spherical calcium carbonate with the average grain diameter of 758 nanometers is obtained after the procedures of dehydration, drying, crushing, sieving and the like.
Example 2
A regular spherical calcium carbonate belongs to a method for preparing spherical calcium carbonate by a calcium hydroxide solution carbonization method, and the preparation method comprises the following steps:
(1) lime slaking and calcium hydroxide slurry preparation: fully stirring and digesting lime and water at a mass ratio of 1:3 at room temperature, properly aging and cooling, filtering the obtained lime slurry to remove large particles of insoluble matters and impurities to obtain refined calcium hydroxide slurry, adding methanol to regulate the content of calcium hydroxide to 12% after the calcium hydroxide slurry is cooled to room temperature, wherein the adding amount of the methanol is 60% of the mass of the regulated calcium hydroxide slurry;
(2) adding a crystal form control agent: pumping the debugged calcium hydroxide slurry into an intermittent bubble carbonization tower with a stirring device by using a pump, adding polyethyleneimine of which the mass is 2.6 percent of that of the calcium hydroxide as a crystal form guiding agent and sodium polyaspartate of which the mass is 3.8 percent of that of the calcium hydroxide as a morphology control agent, and uniformly stirring;
(3) carbonizing: adjusting the initial carbonization temperature of the calcium hydroxide slurry to 20 ℃, opening an air valve, and introducing CO2Carrying out carbonization reaction on gas with the volume concentration of 33%, closing a gas valve when the reaction solution is carbonized until the pH value is 6.8, stopping the reaction, and stopping stirring;
(4) and (3) dehydrating and drying: after the calcium carbonate slurry is gelled and dissolved, the regular spherical calcium carbonate with the average grain diameter of 646 nanometers is obtained through the working procedures of dehydration, drying, crushing, sieving and the like.
Example 3
A regular spherical calcium carbonate belongs to a method for preparing spherical calcium carbonate by a calcium hydroxide solution carbonization method, and the preparation method comprises the following steps:
(1) lime slaking and calcium hydroxide slurry preparation: fully stirring and digesting the lime and the water at the temperature mass ratio of 1:3, properly aging and cooling, and filtering the obtained lime slurry to remove large particles of insoluble matters and impurities to obtain the refined calcium hydroxide slurry. After the calcium hydroxide slurry is cooled to room temperature, adding ethanol and water to adjust the content of the calcium hydroxide to 10 percent, wherein the adding amount of the ethanol is 60 percent of the mass of the adjusted calcium hydroxide slurry;
(2) adding a crystal form control agent: pumping the debugged calcium hydroxide slurry into an intermittent bubble carbonization tower with a stirring device by using a pump, adding polyvinylpyrrolidone with the mass of 2.8 percent of the mass of the calcium hydroxide as a crystal form control agent, adding sorbitan monostearate with the mass of 2.8 percent of the mass of the calcium hydroxide as a morphology control agent, and uniformly stirring;
(3) carbonizing: adjusting the initial carbonization temperature of the calcium hydroxide slurry to 5 ℃, opening an air valve, and introducing CO2Carrying out carbonization reaction on gas with the volume concentration of 36%, closing a gas valve when the reaction solution is carbonized until the pH value is 6.9, stopping the reaction, and stopping stirring;
(4) and (3) dehydrating and drying: after the calcium carbonate slurry is gelled and dissolved, the regular spherical calcium carbonate with the average grain diameter of 710 nanometers is obtained through the working procedures of dehydration, drying, crushing, sieving and the like.
Example 4
A regular spherical calcium carbonate belongs to a method for preparing spherical calcium carbonate by a calcium hydroxide solution carbonization method, and the preparation method comprises the following steps:
(1) lime slaking and calcium hydroxide slurry preparation: sufficiently stirring and digesting lime and prepared regular spherical calcium carbonate dehydration filtrate (mixture of methanol and water) at room temperature according to the mass ratio of 1:8, properly aging and cooling, and filtering the obtained lime slurry to remove large particles of insoluble matters and impurities to obtain refined calcium hydroxide slurry; after the calcium hydroxide slurry is cooled to room temperature, adding methanol to regulate the content of the calcium hydroxide to be 8 percent, wherein the adding amount of the methanol is 60 percent of the mass of the regulated calcium hydroxide slurry;
(2) adding a crystal form control agent: pumping the debugged calcium hydroxide slurry into an intermittent bubble carbonization tower with a stirring device by using a pump, adding sodium polyvinylbenzene sulfonate with the mass of 3.8 percent of the mass of the calcium hydroxide as a crystal form directing agent, adding sodium polyaspartate with the mass of 3.2 percent of the mass of the calcium hydroxide as a morphology control agent, and uniformly stirring;
(3) carbonizing: adjusting the initial carbonization temperature of the calcium hydroxide slurry to 15 ℃, opening an air valve, and introducing CO2Carrying out carbonization reaction on gas with the volume concentration of 40%, closing a gas valve when the reaction solution is carbonized until the pH value is 6.9, stopping the reaction, and stopping stirring;
(4) and (3) dehydrating and drying: after the calcium carbonate slurry is gelled and dissolved, the regular spherical calcium carbonate with the average grain diameter of 532 nanometers is obtained through the working procedures of dehydration, drying, crushing, sieving and the like.
Example 5
A regular spherical calcium carbonate belongs to a method for preparing spherical calcium carbonate by a calcium hydroxide solution carbonization method, and the preparation method comprises the following steps:
(1) lime slaking and calcium hydroxide slurry preparation: sufficiently stirring and digesting lime and prepared regular spherical calcium carbonate dehydration filtrate (mixture of ethanol and water) in a mass ratio of 1:7 at room temperature, properly aging and cooling, filtering the obtained lime slurry to remove large particles of insoluble matters and impurities to obtain refined calcium hydroxide slurry, adding ethanol after the calcium hydroxide slurry is cooled to room temperature to regulate the content of calcium hydroxide to 9%, wherein the adding amount of the ethanol is 50% of the mass of the regulated calcium hydroxide slurry;
(2) adding a crystal form control agent: pumping the adjusted calcium hydroxide slurry into an intermittent bubbling carbonization tower with a stirring device by using a pump, adding a heated and cured soluble starch solution with the mass of 4.2 percent of the mass of the calcium hydroxide as a crystal form control agent, adding sodium polyacrylate with the mass of 3.5 percent of the mass of the calcium hydroxide as a morphology control agent, and uniformly stirring;
(3) carbonizing: adjusting the initial carbonization temperature of the calcium hydroxide slurry to 16 ℃, opening an air valve, and introducing CO2Carrying out carbonization reaction on gas with the volume concentration of 36%, closing a gas valve when the reaction solution is carbonized until the pH value is 6.9, stopping the reaction, and stopping stirring;
(4) and (3) dehydrating and drying: after the calcium carbonate slurry is gelled and dissolved, the regular spherical calcium carbonate with the average grain diameter of 682 nanometers is obtained through the procedures of dehydration, drying, crushing, sieving and the like.
Example 6
A regular spherical calcium carbonate belongs to a method for preparing spherical calcium carbonate by a calcium hydroxide solution carbonization method, and the preparation method comprises the following steps:
(1) lime slaking and calcium hydroxide slurry preparation: fully stirring and digesting lime and water at a mass ratio of 1:4 at room temperature, properly aging and cooling, filtering the obtained lime slurry to remove large particles of insoluble matters and impurities to obtain refined calcium hydroxide slurry, adding a solution of which the mass ratio of methanol to ethanol is 1:1 after the calcium hydroxide slurry is cooled to room temperature to regulate the content of calcium hydroxide to be 10%, and adding methanol and ethanol to the solution to be 50% of the mass of the regulated calcium hydroxide slurry;
(2) adding a crystal form control agent: pumping the debugged calcium hydroxide slurry into an intermittent bubble carbonization tower with a stirring device by using a pump, adding polyethyleneimine of which the mass is 2.2% of that of the calcium hydroxide as a crystal form guiding agent, adding sodium polyacrylate of which the mass is 3.1% of that of the calcium hydroxide as a morphology control agent, and uniformly stirring;
(3) carbonizing: adjusting the initial carbonization temperature of the calcium hydroxide slurry to 12 ℃, opening an air valve, and introducing CO2Carbonizing gas with volume concentration of 28%Reacting, namely closing the air valve when the pH value of the reaction liquid is 6.9 after carbonization, stopping the reaction and stopping stirring;
(4) and (3) dehydrating and drying: after the calcium carbonate slurry is gelled and dissolved, the regular spherical calcium carbonate with the average grain diameter of 638 nanometers is obtained after the procedures of dehydration, drying, crushing, sieving and the like.
Claims (2)
1. A method for preparing regular spherical calcium carbonate is characterized by comprising the following steps: the preparation method comprises the following steps of firstly preparing calcium hydroxide slurry, then adding a composite crystal form control agent into the calcium hydroxide slurry, fully stirring and mixing, adjusting the initial carbonization temperature, introducing carbon dioxide gas for carbonization, dehydrating, drying, crushing and screening the obtained calcium carbonate slurry to obtain regular spherical calcium carbonate, wherein the crystal form of the regular spherical calcium carbonate is a mixed crystal form of a vaterite crystal form and a calcite crystal form, the content of the vaterite crystal form is more than 50%, the content of the calcite crystal form is less than 50%, and the particle size of the regular spherical calcium carbonate is 300-plus 900 nm:
1) slaking lime, refining and preparing into calcium hydroxide slurry;
2) adding a composite crystal form control agent into the prepared calcium hydroxide slurry in a stirring carbonization device, and uniformly stirring;
3) adjusting the initial carbonization temperature of the calcium hydroxide slurry, introducing carbon dioxide gas for carbonization reaction, judging that the reaction is finished when the pH is lower than 7, and stopping introducing the carbon dioxide gas;
4) after the carbonization reaction is finished, dehydrating, drying, crushing and screening to obtain regular spherical calcium carbonate;
in the step 1), lime is directly digested by water, or water is mixed with methanol or ethanol and then digested, or water, methanol and ethanol are mixed and then digested, or clear liquid obtained by dehydration in the preparation process of regular spherical calcium carbonate is used for digestion; after lime is digested and refined, methanol and/or ethanol are added to regulate the content of calcium hydroxide in the calcium hydroxide slurry to be 4-16%, and the adding amount of methanol or ethanol or the mixture of the methanol and the ethanol in the calcium hydroxide slurry is 25-80% of the mass of the calcium hydroxide slurry;
adding a composite crystal form control agent into the prepared calcium hydroxide slurry in the step 2), wherein the composite crystal form control agent is divided into two components, one component is a calcium carbonate crystal form directing agent, and the other component is a morphology control agent; the crystal form directing agent is used as a coagulant for coagulating the vaterite crystal into balls, and the morphology control agent is used as a spherical calcium carbonate morphology regulator for regulating the morphology of calcium carbonate particles to tend to be complete spheres; the crystal form directing agent is one or a compound of more of soluble starch slurry, polyvinylpyrrolidone, sodium polyvinylbenzene sulfonate and polyethyleneimine which are heated and cured, and the amount of the added crystal form directing agent is 1-6% of the solid content of calcium hydroxide; the morphology control agent is one or more compounds of sodium polyacrylate, polysorbate, sodium polyaspartate and sorbitan fatty acid ester; the amount of the added morphology control agent is 0.6-10% of the solid content of the calcium hydroxide;
adjusting the initial carbonization temperature to 3-40 ℃ in the step 3), introducing gas containing 20-100% of carbon dioxide volume concentration under the state of starting stirring for carbonization reaction until the pH value is lower than 7, and stopping introducing the gas to finish carbonization;
stopping introducing carbon dioxide gas in the step 3), stopping stirring after carbonization is finished, waiting for the slurry to form gel, and waiting for the gel to melt after the gel is formed or heating the gel properly to accelerate the gel to melt; the pH value of the slurry is lower than 7, the slurry is over-carbonized to form calcium carbonate and calcium bicarbonate mixed slurry, and after gas introduction is stopped, the calcium bicarbonate is decomposed to form calcium carbonate and carbon dioxide gas which are released to form bubbles in the gel melting process;
and filtering or centrifugally dewatering the dissolved gel to obtain a calcium carbonate filter cake, and drying, crushing and screening the filter cake to obtain the regular spherical calcium carbonate.
2. The process for preparing regular spherical calcium carbonate according to claim 1, characterized in that: and 4) carrying out precipitation, filtration and clarification on filtrate obtained by dehydrating the calcium carbonate slurry in the step 4), and then recycling.
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| CN111036342B (en) * | 2019-12-05 | 2021-01-15 | 四川大学 | Preparation device and preparation process of polymer-based spherical powder |
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| CN114314628A (en) * | 2020-09-29 | 2022-04-12 | 王权广 | Process for preparing regular spherical calcium carbonate by double decomposition method |
| CN115448346B (en) * | 2022-08-11 | 2024-03-12 | 中南大学 | Preparation method of superfine light calcium carbonate |
| CN115321572B (en) * | 2022-08-19 | 2024-02-06 | 中国科学院兰州化学物理研究所 | Efficient preparation method of environment-friendly spherical nano calcium carbonate |
| CN115520888B (en) * | 2022-10-18 | 2023-08-29 | 四川大学 | Application of carbon dioxide adduct of polyethyleneimine in preparation of calcium carbonate |
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