CN111153424A - Preparation method of pinecone-shaped calcium carbonate - Google Patents
Preparation method of pinecone-shaped calcium carbonate Download PDFInfo
- Publication number
- CN111153424A CN111153424A CN202010029926.9A CN202010029926A CN111153424A CN 111153424 A CN111153424 A CN 111153424A CN 202010029926 A CN202010029926 A CN 202010029926A CN 111153424 A CN111153424 A CN 111153424A
- Authority
- CN
- China
- Prior art keywords
- solution
- calcium carbonate
- pinecone
- anhydrous
- preparation
- 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.)
- Pending
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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- 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
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)
- Medicinal Preparation (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a preparation method of pinecone-shaped calcium carbonate, which comprises the following steps: (1) dissolving a certain amount of anhydrous calcium chloride in deionized water to prepare solutions with different concentrations, and then adding 2% of a crystal form control agent to form a solution A; (2) 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; (3) 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 raw materials are cheap and easy to obtain, the process is simple, the particle size control, the shape control and the surface modification are synchronously completed, the method is a more advanced surface treatment technology, and the prepared pinecone-shaped calcium carbonate has the advantages of special appearance, controllable size, high whiteness, good dispersibility and good application prospect.
Description
Technical Field
The invention relates to the technical field of chemical engineering and material engineering, in particular to a preparation method of pinecone-shaped calcium carbonate.
Background
Calcium carbonate is an excellent inorganic filler, has low price, high whiteness, no toxicity, no odor and excellent reinforcing property, and is widely applied to various industries such as plastics, rubber, papermaking, coating, food, cosmetics and the likeThe field of the technology. The calcium carbonate has different functional requirements in different fields, the function depends on parameters such as crystal form, appearance, particle size and the like of calcium carbonate particles, and the calcium carbonate particles with different forms and structures have different functions and application fields. By means of the regulation and control function of various inorganic ions or organic additives, the size, morphology, crystal form and the like of calcium carbonate can be modified by controlling the dosage of the calcium carbonate in the process of synthesizing calcium carbonate particles, so that the calcium carbonate synthesized by modification and having special morphology has higher service performance and added value, which is still an important research topic in the field at home and abroad. The calcium carbonate can be divided into micron-sized, submicron-sized, nanometer-sized and the like according to the particle size, and CaCO is used simultaneously3The calcium carbonate has various shapes, such as cubic shape, spindle shape, needle shape, chain shape, rod shape, spherical shape and the like, and the calcium carbonate with different shapes has different functions and purposes. The preparation method of calcium carbonate mainly comprises three methods: precipitation, carbonization and hypergravity. The morphology and the crystal form of the calcium carbonate prepared by the carbonization method are not easy to control, the steps are complicated, and a serious agglomeration phenomenon exists; the reaction conditions of the hypergravity method are harsh. The precipitation method overcomes the defects of the two calcium carbonate preparation methods, so the precipitation method is favored in the aspects of preparing calcium carbonate and researching the controllability of the shape of the calcium carbonate. However, the calcium carbonate prepared by the existing precipitation method has a single appearance, and the crystal form control is performed by adding the crystal form control agent after the calcium carbonate is prepared, so that the preparation method is complicated, and the organic matter is not beneficial to fully exerting the control effect on the crystal growth.
Disclosure of Invention
The invention aims to provide a preparation method of pinecone-shaped calcium carbonate, which has special appearance and is rarely pinecone-shaped, and synchronously completes particle size control, shape control and surface modification.
The technical scheme of the invention is as follows:
a preparation method of pinecone-shaped calcium carbonate comprises the following steps:
(1) preparation of solution A: dissolving a certain amount of anhydrous calcium chloride in deionized water to prepare solutions with different concentrations, and then adding a crystal form control agent to form a solution A;
(2) preparation of solution B: dissolving a certain amount of anhydrous sodium carbonate in deionized water to prepare solutions with different concentrations, and adding an anhydrous ethanol solution to form a solution B;
(3) and (3) placing the solution A obtained in the step (1) and the solution B obtained in the step (2) in a constant-temperature water bath at 45 ℃, stirring for 0.5h, quickly pouring the solution B subjected to constant temperature into the solution A, strongly stirring for 2h, and performing suction filtration, washing, drying and grinding to obtain the pinecone-shaped calcium carbonate powder.
In the solution A, the concentration of the anhydrous calcium chloride solution is 0.05-0.3 mol/L.
In the step (1), the crystal form control agent is a double-chain surfactant, namely dicetyl dimethyl ammonium bromide.
In the step (1), the mass of the dicetyl dimethyl ammonium bromide accounts for 2% of the theoretical mass of the calcium carbonate.
In the solution B, the concentration of the sodium carbonate solution is 0.05-0.3 mol/L.
The mass ratio of the anhydrous calcium chloride solution to the sodium carbonate solution was 1: 1.
The invention has the beneficial effects that:
1. the dicetyl dimethyl ammonium bromide is used as a crystal form control agent, is a double-chain surfactant and a phase transfer catalyst, is widely used as a cracking reagent in pharmacy and clinical diagnosis kits, and is also used as an emulsifier, a bactericide, a disinfectant, an antistatic agent and the like in the fields of biological engineering and electronics.
2. The precipitation method adopted by the invention has the advantages of cheap and easily available raw materials, simple process, easy operation, short reaction time, high speed, small energy consumption in the reaction process, environmental protection, safety, no pollution and the like.
3. The invention synchronously completes the control of particle size, shape and surface modification, and is a more advanced surface treatment technology. The structure and the appearance of the calcium carbonate are controlled through the interaction of organic molecules and inorganic ions at an interface, so that the exquisite material with preferred growth orientation is formed. Meanwhile, the prepared pinecone-shaped calcium carbonate has special appearance, controllable size, high whiteness, good dispersibility and good application prospect.
4. The invention adopts a liquid phase precipitation method, takes anhydrous calcium chloride and sodium carbonate as raw materials, takes dicetyl dimethyl ammonium bromide as a crystal form control agent to prepare the pinecone-shaped calcium carbonate particles with novel appearance, and researches the appearance change of the calcium carbonate particles under the condition of adding the dicetyl dimethyl ammonium bromide into reaction systems with different concentrations. The product is characterized by a Scanning Electron Microscope (SEM), an X-ray diffractometer (XRD), a whiteness meter and the like, and a new thought and way is provided for the preparation of the calcium carbonate with special morphology.
Drawings
Fig. 1 is a Scanning Electron Microscope (SEM) photograph of a pinecone-like calcium carbonate prepared by the method provided in example 4 of the present invention.
Fig. 2 is an X-ray diffraction (XRD) spectrum of the pinecone-like calcium carbonate prepared by the method provided in example 4 of the present invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and specific examples so that those skilled in the art may better understand the present invention, but the embodiments of the present invention are not limited thereto.
Example 1
(1) Preparation of solution A: dissolving 0.56g of anhydrous calcium chloride in 100ml of deionized water to prepare a 0.05mol/L solution, and then adding 0.3g of a crystal form control agent (dicetyl dimethyl ammonium bromide accounts for 2% of the theoretical mass of calcium carbonate) to form a solution A;
(2) preparation of solution B: dissolving 0.53g of anhydrous sodium carbonate in 100ml of deionized water to prepare a solution of 0.05mol/L, and adding 2ml of anhydrous ethanol solution to form a solution B; the absolute ethyl alcohol solution is used for promoting the crystal form control agent to better play the roles of dissolution and regulation.
(3) And (3) placing the solution A obtained in the step (1) and the solution B obtained in the step (2) in a constant-temperature water bath at 45 ℃, stirring for 0.5h, quickly pouring the solution B subjected to constant temperature into the solution A, strongly stirring for 2h, and performing suction filtration, washing, drying and grinding to obtain the pinecone-shaped calcium carbonate powder.
Example 2
(1) Preparation of solution A: dissolving 1.11g of anhydrous calcium chloride in 100ml of deionized water to prepare a 0.1mol/L solution, and then adding 0.3g of a crystal form control agent (dicetyl dimethyl ammonium bromide accounts for 2% of the theoretical mass of calcium carbonate) to form a solution A;
(2) preparation of solution B: dissolving 1.06g of anhydrous sodium carbonate in 100ml of deionized water to prepare a solution of 0.1mol/L, and adding 5ml of anhydrous ethanol solution to form a solution B;
(3) and (3) placing the solution A obtained in the step (1) and the solution B obtained in the step (2) in a constant-temperature water bath at 45 ℃, stirring for 0.5h, quickly pouring the solution B subjected to constant temperature into the solution A, strongly stirring for 2h, and performing suction filtration, washing, drying and grinding to obtain the pinecone-shaped calcium carbonate powder.
Example 3
(1) Preparation of solution A: dissolving 2.22g of anhydrous calcium chloride in 100ml of deionized water to prepare a 0.2mol/L solution, and then adding 0.3g of a crystal form control agent (dicetyl dimethyl ammonium bromide accounts for 2% of the theoretical mass of calcium carbonate) to form a solution A;
(2) preparation of solution B: dissolving 2.12g of anhydrous sodium carbonate in 100ml of deionized water to prepare a solution of 0.2mol/L, and adding 2ml of anhydrous ethanol solution to form a solution B;
(3) and (3) placing the solution A obtained in the step (1) and the solution B obtained in the step (2) in a constant-temperature water bath at 45 ℃, stirring for 0.5h, quickly pouring the solution B subjected to constant temperature into the solution A, strongly stirring for 2h, and performing suction filtration, washing, drying and grinding to obtain the pinecone-shaped calcium carbonate powder.
Example 4
(1) Preparation of solution A: dissolving 3.33g of anhydrous calcium chloride in 100ml of deionized water to prepare a 0.3mol/L solution, and then adding 0.3g of a crystal form control agent (dicetyl dimethyl ammonium bromide accounts for 2% of the theoretical mass of calcium carbonate) to form a solution A;
(2) preparation of solution B: dissolving 3.18g of anhydrous sodium carbonate in 100ml of deionized water to prepare a solution of 0.3mol/L, and adding 5ml of anhydrous ethanol solution to form a solution B;
(3) and (3) placing the solution A obtained in the step (1) and the solution B obtained in the step (2) in a constant-temperature water bath at 45 ℃, stirring for 0.5h, quickly pouring the solution B subjected to constant temperature into the solution A, strongly stirring for 2h, and performing suction filtration, washing, drying and grinding to obtain the pinecone-shaped calcium carbonate powder.
(4) And (4) placing the sample vessel on a whiteness tester test bench, and measuring the whiteness value. The average was measured three times and the average was taken. The results show that the modified pinecone CaCO3Having a significantly higher whiteness value than the unmodified CaCO3And has better use value in production.
TABLE 1 CaCO3Measurement of whiteness value
Claims (6)
1. A preparation method of pinecone-shaped calcium carbonate is characterized by comprising the following steps: the method comprises the following steps:
(1) preparation of solution A: dissolving a certain amount of anhydrous calcium chloride in deionized water to prepare solutions with different concentrations, and then adding a crystal form control agent to form a solution A;
(2) preparation of solution B: dissolving a certain amount of anhydrous sodium carbonate in deionized water to prepare solutions with different concentrations, and adding an anhydrous ethanol solution to form a solution B;
(3) and (3) placing the solution A obtained in the step (1) and the solution B obtained in the step (2) in a constant-temperature water bath at 45 ℃, stirring for 0.5h, quickly pouring the solution B subjected to constant temperature into the solution A, strongly stirring for 2h, and performing suction filtration, washing, drying and grinding to obtain the pinecone-shaped calcium carbonate powder.
2. The method of preparing pineal calcium carbonate according to claim 1, wherein: in the solution A, the concentration of the anhydrous calcium chloride solution is 0.05-0.3 mol/L.
3. The method of preparing pineal calcium carbonate according to claim 1, wherein: in the step (1), the crystal form control agent is a double-chain surfactant, namely dicetyl dimethyl ammonium bromide.
4. The method of preparing pineal calcium carbonate according to claim 1, wherein: in the step (1), the mass of the dicetyl dimethyl ammonium bromide accounts for 2% of the theoretical mass of the calcium carbonate.
5. The method of preparing pineal calcium carbonate according to claim 1, wherein: in the solution B, the concentration of the sodium carbonate solution is 0.05-0.3 mol/L.
6. The method of preparing pineal calcium carbonate according to claim 1, wherein: the mass ratio of the anhydrous calcium chloride solution to the sodium carbonate solution was 1: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010029926.9A CN111153424A (en) | 2020-01-10 | 2020-01-10 | Preparation method of pinecone-shaped calcium carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010029926.9A CN111153424A (en) | 2020-01-10 | 2020-01-10 | Preparation method of pinecone-shaped calcium carbonate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111153424A true CN111153424A (en) | 2020-05-15 |
Family
ID=70562502
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010029926.9A Pending CN111153424A (en) | 2020-01-10 | 2020-01-10 | Preparation method of pinecone-shaped calcium carbonate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111153424A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040234443A1 (en) * | 2001-12-31 | 2004-11-25 | Jianfeng Chen | Calcium carbonate of different shapes and the preparation process thereof |
| CN101935866A (en) * | 2010-09-16 | 2011-01-05 | 河南城建学院 | Method for preparing flaky calcite calcium carbonate crystal |
| CN102424415A (en) * | 2011-09-14 | 2012-04-25 | 陕西科技大学 | Preparation method for needle cluster-like micrometer-scale calcium carbonate |
| CN102557099A (en) * | 2011-12-16 | 2012-07-11 | 杭州师范大学 | Method for preparing calcite phase and/or vaterite phase calcium carbonate |
| CN103663530A (en) * | 2013-12-04 | 2014-03-26 | 中国中材国际工程股份有限公司 | Method for preparing calcium carbonate powder |
| CN107986313A (en) * | 2017-12-25 | 2018-05-04 | 广西大学 | A kind of preparation method of spherical calcium carbonate |
-
2020
- 2020-01-10 CN CN202010029926.9A patent/CN111153424A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040234443A1 (en) * | 2001-12-31 | 2004-11-25 | Jianfeng Chen | Calcium carbonate of different shapes and the preparation process thereof |
| CN101935866A (en) * | 2010-09-16 | 2011-01-05 | 河南城建学院 | Method for preparing flaky calcite calcium carbonate crystal |
| CN102424415A (en) * | 2011-09-14 | 2012-04-25 | 陕西科技大学 | Preparation method for needle cluster-like micrometer-scale calcium carbonate |
| CN102557099A (en) * | 2011-12-16 | 2012-07-11 | 杭州师范大学 | Method for preparing calcite phase and/or vaterite phase calcium carbonate |
| CN103663530A (en) * | 2013-12-04 | 2014-03-26 | 中国中材国际工程股份有限公司 | Method for preparing calcium carbonate powder |
| CN107986313A (en) * | 2017-12-25 | 2018-05-04 | 广西大学 | A kind of preparation method of spherical calcium carbonate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Shirsath et al. | Continuous precipitation of calcium carbonate using sonochemical reactor | |
| CN103273083A (en) | Method for preparing gold nanoparticles | |
| CN111592025B (en) | Preparation method of chrysanthemum-shaped micron calcium carbonate | |
| CN101704536A (en) | Novel Prussian blue mesocrystals and preparation method thereof | |
| CN104790024A (en) | Preparation method for aragonite calcium carbonate whisker with high length-diameter ratio | |
| CN109867986A (en) | A kind of macromolecule modified nanometer calcium carbonate new product family | |
| CN107930591A (en) | A kind of gravity Method metal-organic solution deposition doping amino acid composite material and preparation method thereof | |
| CN101935866B (en) | Method for preparing flaky calcite calcium carbonate crystal | |
| CN1128199C (en) | Preparation process of magnesium hydroxide fire-retarding nanomaterial | |
| CN102649590A (en) | Method for preparing mesoporous material NiAl2O4 without specific surface active agent | |
| CN101177291B (en) | Method for preparing special-shaped AlOOH nano material | |
| CN113548682A (en) | Method for preparing hexagonal flaky flame-retardant magnesium hydroxide from natural hydromagnesite | |
| CN106220889B (en) | A kind of phenyl-phosphonic acid zinc nucleator, preparation method, morphological control method and application | |
| CN105727922B (en) | A kind of Li adulterates SrTiO3The preparation method and product of ten octahedron nanometer particles | |
| CN102424415B (en) | Preparation method for needle cluster-like micrometer-scale calcium carbonate | |
| CN110449597A (en) | A kind of chain Fe nanowire and preparation method thereof | |
| CN103131210A (en) | Preparation method of composite calcium carbonate | |
| CN109133137B (en) | Ellipsoidal micro-nano calcium carbonate and preparation method thereof | |
| CN110407212B (en) | High-dispersity nano carbonate gel as well as preparation method and application thereof | |
| CN102134746B (en) | Preparation method of alkali type magnesium chloride whisker | |
| CN100420629C (en) | 4A zeolite molecular sieve and its preparation method | |
| CN108083334A (en) | A kind of preparation method of monodisperse spherical nano zirconium dioxide powder body material | |
| CN111153424A (en) | Preparation method of pinecone-shaped calcium carbonate | |
| CN111620381A (en) | beta-FeOOH nano rod and preparation method thereof | |
| CN114408958B (en) | Device and method for preparing hollow spherical calcium carbonate and hollow spherical calcium carbonate prepared by using device |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200515 |
|
| RJ01 | Rejection of invention patent application after publication |