CN107892318A - A kind of preparation method of active nano-calcium carbonate - Google Patents
A kind of preparation method of active nano-calcium carbonate Download PDFInfo
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- CN107892318A CN107892318A CN201711189298.5A CN201711189298A CN107892318A CN 107892318 A CN107892318 A CN 107892318A CN 201711189298 A CN201711189298 A CN 201711189298A CN 107892318 A CN107892318 A CN 107892318A
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- Prior art keywords
- calcium carbonate
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- active nano
- slurries
- crystal formation
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- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
-
- 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
- C01F11/185—After-treatment, e.g. grinding, purification, conversion of crystal morphology
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- 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
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- 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
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Nanotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of preparation method of active nano-calcium carbonate, it is characterised in that comprises the following steps：(1) chemical additives are added into calcium hydroxide emulsion, carburizing reagent is carried out, obtains cubic calcium carbonate slurries；(2) random calcium carbonate serosity is added in the cubic calcium carbonate slurries that step (1) is prepared, and adds crystal formation dispersant, react 13 hours in dynamic mixer, then insulation reaction 30 50 hours at 50 80 DEG C, you can；The crystal formation for the active nano-calcium carbonate that the method for the present invention is prepared is controllable, has good dispersed and excellent glossiness.The BET of the nano-calcium carbonate of the present invention is 25 ± 2 ㎡/g, DOP oil factors：45ml/100g.
Description
Technical field
The invention belongs to the preparing technical field of calcium carbonate, more particularly to a kind of preparation method of active nano-calcium carbonate.
Background technology
Nano-calcium carbonate refers to that particle diameter is less than 100 nanometers of superfine powder, and nm-class active calcium carbonate refers to that calcium carbonate passes through
Oil loving chemical products are become by hydrophily after the organic process of surface, product can be widely applied to vehicle paint base, rubber, plastics
Etc. industry.Fine, particle diameter distribution are narrow, crystal morphology is stable and product quality reappearance height is one of the product and substantially
Ask.
The preparation method of nano-calcium carbonate has multilevel spray carbonization, gravity Method, low-temperature carbonization precipitation method etc. at present.Spraying carbon
How the design that change method is related to nozzle during amplification ensures that being uniformly distributed for droplet, the accurate control of degree of carbonisation etc. is asked
Topic, realize that industrialized normal production requirement condition is higher, still there is imperfection part；Gravity Method be related to equipment amplification after how
Influenceed to the factor such as original force distribution during holding lab scale, higher is required to the operating condition of industrialized production；It is and low
The temperature carbonization precipitation method have cube, spindle and bar-shaped shape, especially particle diameter distribution because the shape of particle of synthesis is irregular
It is wide.Particularly nano-calcium carbonate is in surface treatment, due to the agglomeration of particle, not in the case of monodispersity during processing
Carry out, so treatment effect is not ideal enough, have impact on the excellent application performance of the product.Patent CN1162568A is added by adding
Agent is added to obtain the colloidal calcium carbonate that average diameter is 0.07 μm, average length is 0.5 μm, the product is not cube, it is impossible to full
Requirement of some materials of foot to shape and appearance of calcium carbonate.
The content of the invention
The problem of existing for prior art, it is an object of the invention to provide a kind of preparation of active nano-calcium carbonate
Method.
To achieve these goals, the present invention uses following technical scheme：
A kind of preparation method of active nano-calcium carbonate, comprises the following steps：
(1) chemical additives are added into calcium hydroxide emulsion, carburizing reagent is carried out, obtains cubic calcium carbonate slurries；
(2) random calcium carbonate serosity is added in the cubic calcium carbonate slurries that step (1) is prepared, added brilliant
Type dispersant, 1-3 hours are reacted in dynamic mixer, then at 50-80 DEG C after insulation reaction 30-50 hours, press filtration, done
Dry, crushing, sieving, you can.
Preferably, the concentration of the calcium hydroxide emulsion is 5-15%, and temperature is 15-35 DEG C.
Preferably, the addition of the chemical additives is the 0.2-3% of calcium hydroxide weight in calcium hydroxide emulsion.
Preferably, the chemical additives are acid and polysaccharide is 1-3 by weight:1-3 mixture.Before use, will
Acid and polysaccharide are proportionally added into a certain amount of water after dissolving, in the calcium hydroxide emulsion of addition.
It is further preferred that the acid is selected from least one of hydrochloric acid, sulfuric acid, acetic acid, citric acid；The polysaccharide is shallow lake
At least one of powder, cellulose and pectin.
Preferably, calcium carbonate particle diameter is 15-30nm in the cubic calcium carbonate slurries.
Preferably, the carburizing reagent is to be passed through CO2The uninterrupted of gas is 20-38m3/ min, temperature control is in 20-
50 DEG C, it is reacted to terminal pH=8-9.
Preferably, the concentration of the random calcium carbonate serosity is 5-15%, temperature is 15-35 DEG C, wherein calcium carbonate
Particle diameter is 300-500nm.
Preferably, the mass ratio of the random calcium carbonate serosity and the calcium carbonate in cubic calcium carbonate slurries is 1-2：
1；The addition of the crystal formation dispersant for random crystal formation calcium carbonate serosity in weight of calcium carbonate 0.2-1.2%.
Preferably, the crystal formation dispersant is metaphosphate or polyacrylate.
It is further preferred that the metaphosphate is in two polymetaphosphate, four polymetaphosphate and polyphosphate
At least one.
It is further preferred that the polyacrylate is Sodium Polyacrylate.
Beneficial effects of the present invention：
The crystal formation for the active nano-calcium carbonate that the method for the present invention is prepared is controllable, has well dispersed and excellent
Different glossiness.The BET of the nano-calcium carbonate of the present invention is 25 ± 2 ㎡/g, DOP oil factors：45ml/100g.
Embodiment
Embodiment 1
A kind of preparation method of active nano-calcium carbonate, comprises the following steps：
(1) to 20 DEG C, concentration is that chemical additives are added in 10% calcium hydroxide emulsion, carries out carburizing reagent, is passed through
CO2The uninterrupted of gas is 38m3/ min, temperature control are reacted to terminal pH=8-9, obtain cubic calcium carbonate at 40 DEG C
Slurries；
(2) by 35 DEG C, the random calcium carbonate serosity that concentration is 10% is added to the cube carbon that step (1) is prepared
In sour calcium slurries, and crystal formation dispersant is added, reacted 2 hours in dynamic mixer, be then placed in the anti-of favorable sealing property
Answer insulation reaction 48 hours, press filtration, drying, crushing, sieving at 70 DEG C in tank, you can.
Preferably, the addition of the chemical additives is 2% of calcium hydroxide weight in calcium hydroxide emulsion.
Preferably, the chemical additives are that phosphoric acid and cellulose are 1 by weight:2 mixture.
Preferably, the mass ratio of the random calcium carbonate serosity and the calcium carbonate in cubic calcium carbonate slurries is 2：1.
Preferably, the addition of the crystal formation dispersant is weight of calcium carbonate in the calcium carbonate serosity of random crystal formation
0.8%.
It is further preferred that it is 3 by weight that the crystal formation dispersant, which is polyphosphate and Sodium Polyacrylate,:7 it is mixed
Compound.
Embodiment 2
A kind of preparation method of active nano-calcium carbonate, comprises the following steps：
(1) to 15 DEG C, concentration is that chemical additives are added in 5% calcium hydroxide emulsion, carries out carburizing reagent, is passed through
CO2The uninterrupted of gas is 38m3/ min, temperature control are reacted to terminal pH=8-9, obtain cubic calcium carbonate at 40 DEG C
Slurries；
(2) by 50 DEG C, the random calcium carbonate serosity that concentration is 5% is added to the cube carbon that step (1) is prepared
In sour calcium slurries, and crystal formation dispersant is added, reacted 2 hours in dynamic mixer, be then placed in the anti-of favorable sealing property
Answer insulation reaction 48 hours, press filtration, drying, crushing, sieving at 70 DEG C in tank, you can.
Preferably, the addition of the chemical additives is 2.4% of calcium hydroxide weight in calcium hydroxide emulsion.
Preferably, the chemical additives are that phosphoric acid and cellulose are 1 by weight:2 mixture.
Preferably, the mass ratio of the random calcium carbonate serosity and the calcium carbonate in cubic calcium carbonate slurries is 2：1.
Preferably, the addition of the crystal formation dispersant is weight of calcium carbonate in the calcium carbonate serosity of random crystal formation
1.2%.
It is further preferred that it is 3 by weight that the crystal formation dispersant, which is sodium polyphosphate and Sodium Polyacrylate,:7 it is mixed
Compound.
Embodiment 3
A kind of preparation method of active nano-calcium carbonate, comprises the following steps：
(1) to 35 DEG C, concentration is that chemical additives are added in 15% calcium hydroxide emulsion, carries out carburizing reagent, is passed through
CO2The uninterrupted of gas is 38m3/ min, temperature control are reacted to terminal pH=8-9, obtain cubic calcium carbonate at 40 DEG C
Slurries；
(2) by 35 DEG C, the random calcium carbonate serosity that concentration is 15% is added to the cube carbon that step (1) is prepared
In sour calcium slurries, and crystal formation dispersant is added, reacted 2 hours in dynamic mixer, be then placed in the anti-of favorable sealing property
Answer insulation reaction 36 hours, press filtration, drying, crushing, sieving at 70 DEG C in tank, you can.
Preferably, the addition of the chemical additives is 0.5% of calcium hydroxide weight in calcium hydroxide emulsion.
Preferably, the chemical additives are that acetic acid, starch and pectin are 1 by weight:1:1 mixture.
Preferably, the mass ratio of the random calcium carbonate serosity and the calcium carbonate in cubic calcium carbonate slurries is 2：1.
Preferably, the addition of the crystal formation dispersant is weight of calcium carbonate in the calcium carbonate serosity of random crystal formation
1.2%.
It is further preferred that it is 3 by weight that the crystal formation dispersant, which is sodium polyphosphate and Sodium Polyacrylate,:7 it is mixed
Compound.
Claims (10)
1. a kind of preparation method of active nano-calcium carbonate, it is characterised in that comprise the following steps：
(1) chemical additives are added into calcium hydroxide emulsion, carburizing reagent is carried out, obtains cubic calcium carbonate slurries；
(2) random calcium carbonate serosity is added in the cubic calcium carbonate slurries that step (1) is prepared, adds crystal formation point
Powder, in dynamic mixer react 1-3 hours, then at 50-80 DEG C after insulation reaction 30-50 hours, press filtration, drying,
Crush, sieving, you can.
2. the preparation method of active nano-calcium carbonate according to claim 1, it is characterised in that the calcium hydroxide emulsion
Concentration be 5-15%, temperature is 15-35 DEG C.
3. the preparation method of active nano-calcium carbonate according to claim 1, it is characterised in that the chemical additives
Addition is the 0.2-3% of calcium hydroxide weight in calcium hydroxide emulsion.
4. the preparation method of the active nano-calcium carbonate according to claim 1 or 3, it is characterised in that the crystal formation control
Agent is acid and polysaccharide is 1-3 by weight:1-3 mixture.
5. the preparation method of active nano-calcium carbonate according to claim 4, it is characterised in that it is described acid selected from hydrochloric acid,
At least one of sulfuric acid, acetic acid, citric acid；The polysaccharide is at least one of starch, cellulose and pectin.
6. the preparation method of active nano-calcium carbonate according to claim 1, it is characterised in that the cubic calcium carbonate
Calcium carbonate particle diameter is 15-30nm in slurries.
7. the preparation method of active nano-calcium carbonate according to claim 1, it is characterised in that the carburizing reagent is logical
Enter CO2The uninterrupted of gas is 20-38m3/ min, temperature control are reacted to terminal pH=8-9 at 20-50 DEG C.
8. the preparation method of active nano-calcium carbonate according to claim 1, it is characterised in that the random calcium carbonate
The concentration of slurries is 35-75%, and temperature is 35-80 DEG C, and the wherein particle diameter of calcium carbonate is 300-500nm.
9. the preparation method of active nano-calcium carbonate according to claim 1, it is characterised in that the random calcium carbonate
The mass ratio of slurries and the calcium carbonate in cubic calcium carbonate slurries is 1-2：1；The addition of the crystal formation dispersant is random
Then in the calcium carbonate serosity of crystal formation weight of calcium carbonate 0.2-1.2%.
10. the preparation method of the active nano-calcium carbonate according to claim 1 or 9, it is characterised in that the crystal formation disperses
Agent is metaphosphate or polyacrylate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711189298.5A CN107892318A (en) | 2017-11-24 | 2017-11-24 | A kind of preparation method of active nano-calcium carbonate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711189298.5A CN107892318A (en) | 2017-11-24 | 2017-11-24 | A kind of preparation method of active nano-calcium carbonate |
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| Publication Number | Publication Date |
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| CN107892318A true CN107892318A (en) | 2018-04-10 |
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| CN201711189298.5A Pending CN107892318A (en) | 2017-11-24 | 2017-11-24 | A kind of preparation method of active nano-calcium carbonate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109850931A (en) * | 2019-03-29 | 2019-06-07 | 桂林理工大学 | A kind of preparation method of low-surface-energy dispersed nano calcium carbonate |
| CN112830509A (en) * | 2021-01-25 | 2021-05-25 | 连州市凯恩斯纳米材料有限公司 | Olive-shaped submicron calcium carbonate and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103508479A (en) * | 2013-10-22 | 2014-01-15 | 山西兰花华明纳米材料有限公司 | Production method of nanometer calcium carbonate for electronic glue |
-
2017
- 2017-11-24 CN CN201711189298.5A patent/CN107892318A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103508479A (en) * | 2013-10-22 | 2014-01-15 | 山西兰花华明纳米材料有限公司 | Production method of nanometer calcium carbonate for electronic glue |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109850931A (en) * | 2019-03-29 | 2019-06-07 | 桂林理工大学 | A kind of preparation method of low-surface-energy dispersed nano calcium carbonate |
| CN109850931B (en) * | 2019-03-29 | 2023-07-14 | 桂林理工大学 | Preparation method of low-surface-energy monodisperse nano calcium carbonate |
| CN112830509A (en) * | 2021-01-25 | 2021-05-25 | 连州市凯恩斯纳米材料有限公司 | Olive-shaped submicron calcium carbonate and preparation method and application thereof |
| CN112830509B (en) * | 2021-01-25 | 2023-03-17 | 连州市凯恩斯纳米材料有限公司 | Olive-shaped submicron calcium carbonate and preparation method and application thereof |
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Application publication date: 20180410 |