CN113860347A - Preparation method of stable and controllable vegetable pepper-shaped calcium carbonate particles with ultra-large particle size - Google Patents
Preparation method of stable and controllable vegetable pepper-shaped calcium carbonate particles with ultra-large particle size Download PDFInfo
- Publication number
- CN113860347A CN113860347A CN202111252458.2A CN202111252458A CN113860347A CN 113860347 A CN113860347 A CN 113860347A CN 202111252458 A CN202111252458 A CN 202111252458A CN 113860347 A CN113860347 A CN 113860347A
- Authority
- CN
- China
- Prior art keywords
- calcium carbonate
- suspension
- particle size
- carbonate particles
- stable
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparation method of stable and controllable vegetable pepper-shaped calcium carbonate particles with super large particle size, which comprises the following steps: preparing 8g/L calcium hydroxide suspension, adding a compound crystal form control agent into the suspension, and stirring and mixing uniformly; the crystal form control agent is ZnCl2And EDTA; adding a sodium carbonate solution with the concentration of 10.6g/L into the calcium hydroxide suspension by a peristaltic pump, controlling the temperature to be 60-80 ℃, stirring at the speed of 1000-1500rmb/min, and continuously stirring for 5-10min after the calcium hydroxide suspension is completely reacted to obtain a calcium carbonate suspension; filtering the calcium carbonate suspension, and drying the filter cake to obtain the vegetable pepper-shaped calcium carbonate particles. The invention provides the preparation of the vegetable pepper-shaped calcium carbonate particles with super large particle size, stability, controllability, narrow particle size distribution and stable product, provides a direction for producing calcium carbonate with different shapes, and is expected to widen the application of the calcium carbonate; and the preparation process is simple, the production efficiency is high, the raw material source is rich, the production cost is low, and the industrial production is easy to realize.
Description
Technical Field
The invention belongs to the technical field of inorganic material preparation, and particularly relates to a preparation method of stable and controllable vegetable pepper-shaped calcium carbonate particles with super large particle size.
Background
Calcium carbonate, a widely used industrial material, has the advantages of wide raw material sources, low price, no toxicity, no harm and excellent processability. In the preparation process of calcium carbonate, particles with different particle sizes and appearances can be obtained by adjusting reaction parameters such as temperature, reactants, additives and the like, and the appearances of the particles comprise cubic shapes, spindle shapes, needle shapes, spherical shapes, chain shapes, sheet shapes and the like. The specific morphology and size give the calcium carbonate particles a special functional application, as follows: the spindle calcium carbonate of micron or nanometer level may be used in papermaking, hard PVC stuffing, paint and other fields, and has certain amount of nanometer spindle calcium carbonate added into the paint to improve the product's glossiness, dryness, shading capacity, etc; spherical or hollow calcium carbonate is generally used in the biomedical field as a carrier for protein, DNA, bio-enzyme due to its excellent properties such as more pores in the particle structure, larger pore area, high solubility, good dispersibility, etc.; the nano-scale cubic calcium carbonate is applied to the fields of silicone adhesive, 107 adhesive, rubber and the like, and mainly plays roles in toughening, reinforcing and filling; micron-sized needle-shaped or rod-shaped calcium carbonate is applied to high-grade paper due to high dispersibility. Based on the above, the invention provides a preparation method of calcium carbonate particles with special shapes, which is expected to be applied in some special fields.
For example, patent CN104692437A relates to a method for preparing calcium carbonate with controllable morphology based on temperature control: introducing a solution containing carbonate or a gas capable of generating carbonate, such as CO2 or a gas mixture containing CO2, into a solution containing calcium ions at 10-100 ℃, initiating a precipitation reaction, harvesting a precipitation product after a few minutes, and drying at room temperature to obtain micron-sized calcium carbonate crystals with specific shapes (chain, chrysanthemum flower, ball and whisker). The calcium carbonate prepared by the method has good correspondence between the morphology and the reaction temperature, and is independent of the types of reactants; the prepared product has good dispersion and uniform size; and is efficient and stable in the aspect of crystal form control; in addition, the temperature control method is simple and feasible and can be synthesized in one step. Compared with the patent, the calcium carbonate particle does not show the vegetable pepper-shaped calcium carbonate particles, and the calcium source material is calcium chloride, so that the cost is lower than that of calcium hydroxide, and the industrialization is not facilitated.
For example, patent CN105271344A discloses a preparation method of pine cone-shaped calcite-type micron-sized calcium carbonate particles, which comprises dissolving 60 parts by weight of calcium oxide in water, preparing 5-15 wt% of ca (oh)2 suspension through conventional hydration reaction, adding a crystal growth composite control agent, introducing CO2 into a carbonization reaction kettle at 25-95 ℃ for primary carbonization reaction, stopping introducing CO2 when the pH = 8-9 of the reaction solution is subjected to secondary carbonization reaction until the pH = 7-7.5, continuing the carbonization reaction for 20min, filtering, washing and drying with hot air according to a conventional method to obtain pine cone-shaped calcite-type micron-sized calcium carbonate particles. The invention obtains the pinecone-shaped calcium carbonate product by changing the crystal growth control agent and carrying out secondary carbonization reaction, the product has lower oil absorption value and larger surface area, improves the application effect of the calcium carbonate, and has the advantages of simple reaction condition, easy operation, lower production cost, and better economic benefit, social benefit and ecological benefit.
For example, patent CN105417564A, the present invention relates to a method for continuously preparing petal-shaped flaky calcium carbonate crystals under the condition of a high gravity field. The concrete implementation steps are as follows: and (3) dropwise adding a certain amount of ammonia water into the aqueous solution with the preparation concentration of 0.005-0.02 mol/LCaCl2 to adjust the pH value, sealing and stirring, and transferring to a supergravity reactor. Controlling the carbonization temperature to be 15-50 ℃, and rotating CaCl in a high-speed manner in a hypergravity reactor2The mixed solution is in countercurrent contact with CO2 with the flow rate of 30-500L/h to carry out carbonization reaction. And stopping ventilation when the pH of the slurry is = 6.5-7.0, and finishing the carbonization reaction. And centrifuging the slurry after complete carbonization, drying for 5 hours at 70 ℃, and crushing to obtain the petal-shaped flaky calcium carbonate product with the average particle size of 330-640 nm. Compared with other carbonization methods, the concentration of the CaCl2 aqueous solution is regulated to be 0.005-0.02 mol/L, no crystal form control agent is required to be added, the petal-shaped flaky calcium carbonate product prepared by the supergravity carbonization method has the advantages of narrow particle size distribution, uniform appearance and good dispersibility, and the carbonization time is greatly shortened.
For example, patent CN107601540A, a method for preparing calcium carbonate with different morphologies by using a single control agent, comprises the following steps: 1) preparing a sodium carbonate aqueous solution and a calcium chloride aqueous solution; 2) adding tetrasodium ethylene diamine tetraacetate into a sodium carbonate aqueous solution, and stirring and dissolving completely; 3) slowly dripping the calcium chloride aqueous solution into the solution obtained in the step 2) under the condition of stirring at constant temperature, and continuing stirring after the reaction is completed; 4) filtering the product obtained in the step 3), washing the product with ethanol, and drying the washed product to obtain calcium carbonate powder. The method can realize the preparation of the micron calcium carbonate with different shapes (spherical shape and spindle shape), can realize batch production and has good particle dispersibility. The preparation method provided by the invention has the advantages of simple process flow, high solution concentration, short production period, good safety, recoverable solvent and the like.
For example, patent CN108163879A discloses a method for preparing calcium carbonate with different morphologies and phase structures, which comprises preparing calcium carbonate particles with different morphologies such as spherical, ellipsoidal, petal-shaped, rod-shaped, spindle-shaped, cubic, and lamellar shapes by simple precipitation reaction of calcium acetate and sodium bicarbonate in a system of a mixed solvent of water and ethylene glycol, and studying the influence of the concentration of calcium acetate and sodium bicarbonate, the volume ratio of water and ethylene glycol, and the reaction temperature on the phase structure and morphology of the product.
For example, patent CN109809458A discloses an olivary calcium carbonate and its preparation process, the preparation method comprises: adding a crystal form directing 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 8, and dehydrating, drying, crushing and screening to obtain the rugby-shaped calcium carbonate. The rugby-shaped 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.
For example, patent CN109824076A, the invention discloses a process for preparing calcium carbonate by a bubble membrane method and application thereof, belonging to the technical field of preparation of inorganic non-metallic material calcium carbonate powder. The process for preparing calcium carbonate by the bubble membrane method comprises carbonization and surface treatment, wherein the refined calcium hydroxide slurry is subjected to rapid carbonization reaction in a bubble membrane rapid carbonization reactor, the slurry obtained by the reaction is subjected to appropriate surface treatment as required, and calcium carbonate powder with uniform particle size can be obtained by filtering, drying, crushing and screening. The process for preparing calcium carbonate by the bubble membrane method does not need to add a crystal form control agent, has controllable crystal morphology, uniform and controllable product particle size, good dispersibility, simple and feasible process and low production cost, and the prepared calcium carbonate powder is suitable for industries including plastics, rubber, papermaking, food, medicine and cosmetics and has good economic benefit and social benefit.
For example, patent CN109824077A discloses a spherical calcium carbonate and a preparation method thereof, which comprises the following steps: slaking and aging quicklime and water according to a certain proportion, sieving to remove impurities, adding an ethanol solvent into the raw slurry, and refining and adjusting to obtain calcium hydroxide slurry; transferring the prepared slurry into a supergravity reactor, adding a crystal form control agent, and controlling the carbonization temperature, the CO2 gas flow and the supergravity level to enable the calcium hydroxide slurry to be in countercurrent contact with carbon dioxide gas for carbonization reaction; and (3) centrifuging the slurry after carbonization to obtain precipitate, drying and crushing to obtain the spherical calcium carbonate.
In summary, although the shapes of the calcium carbonate prepared at present are chain, spherical, rod-shaped, petal-shaped and the like, the preparation of the capsicum-like calcium carbonate particles is not found.
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 vegetable pepper-shaped calcium carbonate particles with super-large particle size, stability, controllability, narrow particle size distribution and stable products, provides more shapes for the calcium carbonate particles, and is expected to widen the application of the calcium carbonate.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a preparation method of stable and controllable vegetable pepper-shaped calcium carbonate particles with super-large particle size comprises the following steps:
(1) preparing 8g/L calcium hydroxide suspension, adding a compound crystal form control agent into the suspension, and stirring and mixing uniformly; the crystal form control agent is ZnCl2And EDTA;
(2) adding a sodium carbonate solution with the concentration of 10.6g/L into the calcium hydroxide suspension by a peristaltic pump, controlling the temperature to be 60-80 ℃, stirring at the speed of 1000-1500rmb/min, and continuously stirring for 5-10min after the calcium hydroxide suspension is completely reacted to obtain a calcium carbonate suspension;
(3) filtering the calcium carbonate suspension, and drying the filter cake to obtain the vegetable pepper-shaped calcium carbonate particles.
Further, ZnCl in the crystal form control agent2And EDTA in a mass ratio of 1: 1.
Further, the addition amount of the crystal form control agent is 1-5% of the mass of the calcium hydroxide.
Further, the addition rate of the sodium carbonate solution is 4-8 ml/min.
Further, the drying is vacuum microwave drying.
Further, the drying is drying at a temperature of 80-100 ℃.
Compared with the prior art, the invention has the advantages and beneficial effects that:
the method provides vegetable pepper-shaped calcium carbonate particles with super-large particle size, stability, controllability, narrow particle size distribution and stable product, provides a direction for producing calcium carbonate with different shapes, and is expected to widen the application of the calcium carbonate; and the preparation process is simple, the production efficiency is high, the raw material source is rich, the production cost is low, and the industrial production is easy to realize.
Drawings
FIG. 1 is an electron micrograph of a calcium carbonate product according to example 1 of the present invention;
FIG. 2 is an electron micrograph of a calcium carbonate product according to example 2 of the present invention;
FIG. 3 is an electron micrograph of a calcium carbonate product according to example 3 of the present invention;
FIG. 4 is an electron micrograph of a comparative calcium carbonate product according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of stable and controllable vegetable pepper-shaped calcium carbonate particles with super-large particle size comprises the following steps:
(1) preparing 8g/L calcium hydroxide suspension, adding a compound crystal form control agent accounting for 1% of the mass of the calcium hydroxide into the suspension, and stirring and mixing uniformly; the crystal form control agent is prepared from ZnCl with the mass ratio of 1:12And EDTA;
(2) adding 10.6g/L sodium carbonate solution into the calcium hydroxide suspension at the speed of 8ml/min by a peristaltic pump, controlling the temperature at 60 ℃, stirring at the speed of 1000rmb/min, and continuously stirring for 10min after the calcium hydroxide suspension completely reacts to obtain calcium carbonate suspension;
(3) filtering the calcium carbonate suspension, and drying the filter cake in a vacuum microwave dryer at 80 ℃ to obtain the vegetable pepper-shaped calcium carbonate particles.
The calcium carbonate prepared in the embodiment is detected by a scanning electron microscope, and the detection result is shown in fig. 1, from which the calcium carbonate prepared by the invention has a vegetable pepper-shaped appearance, large and uniform particles, and has particle sizes larger than 7 μm and similar particle sizes.
Example 2
A preparation method of stable and controllable vegetable pepper-shaped calcium carbonate particles with super-large particle size comprises the following steps:
(1) preparing 8g/L calcium hydroxide suspension, adding a compound crystal form control agent accounting for 3% of the mass of the calcium hydroxide into the suspension, and stirring and mixing uniformly; the crystal form control agent is prepared from ZnCl with the mass ratio of 1:12And EDTA;
(2) adding 10.6g/L sodium carbonate solution into the calcium hydroxide suspension at the speed of 5ml/min by a peristaltic pump, controlling the temperature at 60 ℃, stirring at 1200rmb/min, and continuously stirring for 10min after the calcium hydroxide suspension completely reacts to obtain calcium carbonate suspension;
(3) filtering the calcium carbonate suspension, and drying the filter cake in a vacuum microwave dryer at 100 ℃ to obtain the vegetable pepper-shaped calcium carbonate particles.
The calcium carbonate prepared in the embodiment is detected by a scanning electron microscope, and the detection result is shown in fig. 2, and the calcium carbonate prepared by the method has a vegetable pepper-shaped particle shape, large and uniform particles, and has particle sizes larger than 5 μm and similar particle sizes.
Example 3
A preparation method of stable and controllable vegetable pepper-shaped calcium carbonate particles with super-large particle size comprises the following steps:
(1) preparing 8g/L calcium hydroxide suspension, adding a compound crystal form control agent accounting for 5% of the mass of the calcium hydroxide into the suspension, and stirring and mixing uniformly; the crystal form control agent is prepared from ZnCl with the mass ratio of 1:12And EDTA;
(2) adding 10.6g/L sodium carbonate solution into the calcium hydroxide suspension at a speed of 4ml/min by a peristaltic pump, controlling the temperature at 80 ℃, stirring at 1500rmb/min, and continuously stirring for 5min after the calcium hydroxide suspension completely reacts to obtain calcium carbonate suspension;
(3) filtering the calcium carbonate suspension, and drying the filter cake in a vacuum microwave dryer at 100 ℃ to obtain the vegetable pepper-shaped calcium carbonate particles.
The calcium carbonate prepared in the embodiment is detected by a scanning electron microscope, and the detection result is shown in fig. 3, and the calcium carbonate particles prepared by the method are vegetable pepper-shaped, large in size, uniform in distribution, larger than 5 μm in particle size and similar in particle size.
Comparative example 1
(1) Preparing 5g/L calcium hydroxide suspension, adding a compound crystal form control agent accounting for 5% of the mass of the calcium hydroxide into the suspension, and stirring and mixing uniformly; the crystal form control agent consists of ZnCl2 and EDTA in a mass ratio of 1: 1;
(2) adding 10.6g/L sodium carbonate solution into the calcium hydroxide suspension at a speed of 4ml/min by a peristaltic pump, controlling the temperature at 80 ℃, stirring at 1500rmb/min, and continuously stirring for 5min after the calcium hydroxide suspension completely reacts to obtain calcium carbonate suspension;
(3) filtering the calcium carbonate suspension, and drying the filter cake in a vacuum microwave dryer at 100 ℃ to obtain calcium carbonate particles.
The calcium carbonate prepared by the comparative example is detected by a scanning electron microscope, the detection result is shown in fig. 4, and the clustered short rod-shaped morphology of the calcium carbonate product can be seen from the figure; thus, the concentration of the sodium carbonate solution and the calcium hydroxide suspension has a great influence on the morphology of the calcium carbonate.
Comparative example 2
(1) Preparing 8g/L calcium hydroxide suspension, adding a compound crystal form control agent accounting for 5% of the mass of the calcium hydroxide into the suspension, and stirring and mixing uniformly; the crystal form control agent consists of ZnCl2 and EDTA in a mass ratio of 1: 1;
(2) adding 4g/L sodium carbonate solution into the calcium hydroxide suspension at a speed of 4ml/min by a peristaltic pump, controlling the temperature to be 80 ℃, stirring at a speed of 1500rmb/min, and continuously stirring for 5min after the calcium hydroxide suspension completely reacts to obtain calcium carbonate suspension;
(3) filtering the calcium carbonate suspension, and drying the filter cake in a vacuum microwave dryer at 100 ℃ to obtain calcium carbonate particles.
Comparative example 3
(1) Preparing a suspension of calcium hydroxide 8g/L, adding into the suspension5 percent of compound crystal form control agent of the mass of the calcium hydroxide is stirred and mixed evenly; the crystal form control agent is prepared from ZnCl with the mass ratio of 1:12And EDTA;
(2) adding 10.6g/L sodium carbonate solution into the calcium hydroxide suspension at a speed of 15ml/min by a peristaltic pump, controlling the temperature at 80 ℃, stirring at 1500rmb/min, and continuously stirring for 5min after the calcium hydroxide suspension completely reacts to obtain calcium carbonate suspension;
(3) filtering the calcium carbonate suspension, and drying the filter cake in a vacuum microwave dryer at 100 ℃ to obtain calcium carbonate particles.
Comparative example 4
(1) Preparing 8g/L calcium hydroxide suspension, adding a compound crystal form control agent accounting for 5% of the mass of the calcium hydroxide into the suspension, and stirring and mixing uniformly; the crystal form control agent consists of ZnCl2 and EDTA in a mass ratio of 1: 1;
(2) adding 10.6g/L sodium carbonate solution into the calcium hydroxide suspension at the speed of 1ml/min by a peristaltic pump, controlling the temperature at 80 ℃, stirring at the speed of 1500rmb/min, and continuously stirring for 5min after the calcium hydroxide suspension completely reacts to obtain calcium carbonate suspension;
(3) filtering the calcium carbonate suspension, and drying the filter cake in a vacuum microwave dryer at 100 ℃ to obtain calcium carbonate particles.
The calcium carbonates obtained in examples 1 to 3 of the present invention and comparative examples 1 to 4 were measured for their particle size distribution and specific surface area according to a conventional method, and the results of the measurements are shown in Table 1.
| Sample numbering | D50 (μm) | D97 (μm) | BET (m2/g) |
| Example 1 | 9.25 | 11.50 | 1.22 |
| Example 1 | 10.76 | 12.44 | 0.98 |
| Example 1 | 8.43 | 11.32 | 1.50 |
| Comparative example 1 | 4.20 | 8.52 | 6.54 |
| Comparative example 2 | 6.27 | 14.26 | 5.31 |
| Comparative example 3 | 2.17 | 8.95 | 4.69 |
| Comparative example 4 | 8.62 | 16.22 | 8.34 |
From the test results, it was found that the concentration of the calcium carbonate solution or the calcium hydroxide suspension had a great influence on the particle size of the calcium carbonate particles, and that the particle size distribution of the calcium carbonate particles was smaller and the specific surface area was larger under the conditions of 10.6g/L of the sodium carbonate solution and 8g/L of the calcium hydroxide suspension. The adding speed of the sodium carbonate solution also has great influence on the particle size distribution and the specific surface area of the calcium carbonate particles, and the calcium carbonate particles prepared at the adding speed of 4-8ml/min have narrower distribution and smaller 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 (6)
1. A preparation method of stable and controllable vegetable pepper-shaped calcium carbonate particles with super large particle size is characterized by comprising the following steps:
(1) preparing 8g/L calcium hydroxide suspension, adding a compound crystal form control agent into the suspension, and stirring and mixing uniformly; the crystal form control agent is ZnCl2And EDTA;
(2) adding a sodium carbonate solution with the concentration of 10.6g/L into the calcium hydroxide suspension by a peristaltic pump, controlling the temperature to be 60-80 ℃, stirring at the speed of 1000-1500rmb/min, and continuously stirring for 5-10min after the calcium hydroxide suspension is completely reacted to obtain a calcium carbonate suspension;
(3) filtering the calcium carbonate suspension, and drying the filter cake to obtain the vegetable pepper-shaped calcium carbonate particles.
2. The method for preparing the cabbageworm calcium carbonate particles with ultra-large particle size and stable and controllable sizes as claimed in claim 1, which is characterized in that: ZnCl in the crystal form control agent2And EDTA in a mass ratio of 1: 1.
3. The method for preparing the cabbageworm calcium carbonate particles with ultra-large particle size and stable and controllable sizes as claimed in claim 2, which is characterized in that: the addition amount of the crystal form control agent is 1-5% of the mass of the calcium hydroxide.
4. The method for preparing the cabbageworm calcium carbonate particles with ultra-large particle size and stable and controllable sizes as claimed in claim 1, which is characterized in that: the addition rate of the sodium carbonate solution is 4-8 ml/min.
5. The method for preparing the cabbageworm calcium carbonate particles with ultra-large particle size and stable and controllable sizes as claimed in claim 1, which is characterized in that: the drying is vacuum microwave drying.
6. The method for preparing the cabbageworm calcium carbonate particles with ultra-large particle size and stable and controllable sizes as claimed in claim 5, which is characterized in that: the drying is carried out at a temperature of 80-100 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111252458.2A CN113860347B (en) | 2021-10-27 | 2021-10-27 | Preparation method of super-large-particle-size stable and controllable cayenne pepper-shaped calcium carbonate particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111252458.2A CN113860347B (en) | 2021-10-27 | 2021-10-27 | Preparation method of super-large-particle-size stable and controllable cayenne pepper-shaped calcium carbonate particles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113860347A true CN113860347A (en) | 2021-12-31 |
| CN113860347B CN113860347B (en) | 2023-09-08 |
Family
ID=78998298
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111252458.2A Active CN113860347B (en) | 2021-10-27 | 2021-10-27 | Preparation method of super-large-particle-size stable and controllable cayenne pepper-shaped calcium carbonate particles |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113860347B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1179401A (en) * | 1996-10-16 | 1998-04-22 | 长春市迪瑞检验制品有限责任公司 | Method for producing crystalline form nm-class calcium carbonate |
| CN1309089A (en) * | 2001-02-16 | 2001-08-22 | 清华大学 | Process for preparing nm-class calcium carbonate |
| JP2007070164A (en) * | 2005-09-07 | 2007-03-22 | Nittetsu Mining Co Ltd | Silica-calcium carbonate composite particle, its producing method and pigment, filler or paper containing it |
| CN101234776A (en) * | 2007-10-31 | 2008-08-06 | 汤建新 | Process for preparing nano calcium carbonate |
-
2021
- 2021-10-27 CN CN202111252458.2A patent/CN113860347B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1179401A (en) * | 1996-10-16 | 1998-04-22 | 长春市迪瑞检验制品有限责任公司 | Method for producing crystalline form nm-class calcium carbonate |
| CN1309089A (en) * | 2001-02-16 | 2001-08-22 | 清华大学 | Process for preparing nm-class calcium carbonate |
| JP2007070164A (en) * | 2005-09-07 | 2007-03-22 | Nittetsu Mining Co Ltd | Silica-calcium carbonate composite particle, its producing method and pigment, filler or paper containing it |
| CN101234776A (en) * | 2007-10-31 | 2008-08-06 | 汤建新 | Process for preparing nano calcium carbonate |
Non-Patent Citations (1)
| Title |
|---|
| YUQIAN YE ET AL.: "The Role Of Crystal Control Agent in the Formation Of Needlelike Calcium Carbonate Nano Particles", 《ADVANCED MATERIALS RESEARCH》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113860347B (en) | 2023-09-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109809457B (en) | Regular spherical calcium carbonate and preparation process thereof | |
| CN108821322B (en) | Preparation method of microsphere precipitated calcium carbonate with layered structure | |
| CN112723402B (en) | Preparation method of monodisperse spindle-shaped precipitated calcium carbonate | |
| CN106517285A (en) | Method for preparing bar-shaped nanometer calcium carbonate | |
| CN101570344A (en) | Preparation method of aragonite crystal form calcium carbonate | |
| CN108975372A (en) | A kind of preparation method of spindle winnofil | |
| CN106542557B (en) | A kind of preparation technology of nano-calcium carbonate | |
| CN108217707A (en) | A kind of calcium carbonate tiny balloon and preparation method thereof | |
| CN109809458B (en) | Rugby-shaped calcium carbonate and preparation process thereof | |
| CN101318685A (en) | Method for preparing ultra-fine active nano-calcium carbonate with low-ore grade limestone activation of activation tank | |
| CN101318682A (en) | Stephanoporate calcium carbonate, preparing method and application thereof | |
| CN114291835B (en) | Preparation method of large-small cubic dispersion precipitated calcium carbonate | |
| CN114408959A (en) | Preparation method of monodisperse calcium carbonate with regular appearance and narrow particle size distribution | |
| CN110451545B (en) | Preparation method of rod-like calcium carbonate for PE (polyethylene) breathable film | |
| CN107792872B (en) | A kind of preparation process of spindle nanometer calcium carbonate | |
| CN110128851B (en) | Preparation method of hydrophobic nano calcium carbonate | |
| CN112811456A (en) | Nano calcium carbonate with high specific surface area and preparation method thereof | |
| CN108793217A (en) | The preparation method of one bulb tufted shape precipitated calcium carbonate | |
| CN108190935A (en) | A kind of preparation method of strip of sheet calcium carbonate superfine particle | |
| CN113860347A (en) | Preparation method of stable and controllable vegetable pepper-shaped calcium carbonate particles with ultra-large particle size | |
| CN105271344B (en) | A kind of preparation method of strobile pattern calcite type micron order calcium carbonate granule | |
| CN115321572B (en) | Efficient preparation method of environment-friendly spherical nano calcium carbonate | |
| CN115043421B (en) | Cuju spherical precipitated calcium carbonate and preparation method thereof | |
| CN114408958B (en) | Device and method for preparing hollow spherical calcium carbonate and hollow spherical calcium carbonate prepared by using device | |
| CN112441605B (en) | Preparation method of vermicular precipitated calcium carbonate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |