CN107601541A - A kind of production method of nano-calcium carbonate - Google Patents
A kind of production method of nano-calcium carbonate Download PDFInfo
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- CN107601541A CN107601541A CN201710919720.1A CN201710919720A CN107601541A CN 107601541 A CN107601541 A CN 107601541A CN 201710919720 A CN201710919720 A CN 201710919720A CN 107601541 A CN107601541 A CN 107601541A
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Abstract
The present invention relates to technical field of chemical material preparation, more particularly to a kind of production method of nano-calcium carbonate, after limestone calcination plus percentage by weight is made as 5% 10% aqua calcis in water, aqua calcis is spilled into autoclave again, carbon dioxide and nitrogen mixed gas are passed through into autoclave simultaneously, stearmide and higher aliphatic are added in the solid that reaction obtains, then by separation of solid and liquid, dehydrates to obtain nano-calcium carbonate calcium powder；Calcium carbonate crystal body epigranular that the present invention prepares, steady quality.
Description
【Technical field】
The present invention relates to technical field of chemical material preparation, and in particular to a kind of production method of nano-calcium carbonate.
【Background technology】
Nano-calcium carbonate is also known as super fine calcium carbonate, and the title of standard is calcium carbonate superfine powder, nano-calcium carbonate application most into
Ripe industry is that plastics industry is mainly used in high-grade plastic products.Nano-calcium carbonate can improve the rheological characteristic of plastic matrix, carry
Its high mouldability, it is used as having the function that during plastic filler toughened and reinforced, and can improve the bending strength of plastics, the elasticity of flexure
Modulus, heat distortion temperature and dimensional stability, while it is stagnant hot also to assign plastics.Nano-calcium carbonate is when in for ink product
Excellent dispersed and transparent, fabulous gloss and excellent ink absorption and high drying property are embodied.And nanometer
When calcium carbonate makees ink filler in resin type ink, with stability is good, glossiness is high, does not influence the drying property of printing-ink
The advantages that energy, strong adaptability.Specifically, nano-calcium carbonate is consolidated as a kind of Novel super-thin to grow up the 1980s
Body dusty material, its granularity is between 10~100nm.Due to the fine of Nano particles of calcium carbonate, its crystal structure and table
Face electronic structure changes, and generates quantum size effect, small-size effect, skin effect that ordinary calcium carbonate does not have
And macroscopic quantum effect.So nano-calcium carbonate is widely used in plastics, rubber, ink, painting frequently as filler or reinforcing agent
The industry such as material, papermaking, adhesive, sealant, it is also applied to the industries such as toothpaste, food, medicine, feed, building materials, chemical fibre.At present,
There is the problems such as granularity is larger, rank is wider, quality is unstable, reunites in the nano-calcium carbonate that the country is produced, this is directly affected
The application performance of nano-calcium carbonate.
【The content of the invention】
It is an object of the invention to：In view of the above-mentioned problems, providing a kind of production method of nano-calcium carbonate, solves nano-sized carbon
The problem of sour calcium granularity is larger, rank is wider, quality is unstable.
To achieve these goals, the technical solution adopted by the present invention is as follows：
A kind of production method of nano-calcium carbonate, comprises the following steps：
A) calcium oxide is made in lime stone with calciner, and manufactured calcium oxide is put into reactor, in reactor
The aqua calcis that percentage by weight is 5%-10% is made in the middle water that adds；
B) aqua calcis of preparation is spilled at the top of autoclave with shower nozzle, then from autoclave
Middle part is passed through the carbon dioxide and nitrogen mixed gas that carbon dioxide content is 3%-5%, and the flow rate for controlling mixed gas is
40m3/(h·m3Aqua calcis), while control mixed gas to discharge autoclave with identical flow velocity；
C) aqua calcis for falling into autoclave bottom is filtered using solid-liquid separator, collects consolidating for filtering
Body, and the top of filtrate return autoclave is spilled into again, circulate operation, until the solution pH value of autoclave bottom
Between 7-7.2, stop circulation, the solution of autoclave bottom is discharged；
D) added in the solid collected in step c) and account for solid masses than the stearmide and 4%-6% for 2%-4%
Higher aliphatic, place 5h in 80-100 DEG C of environment, obtain nano-calcium carbonate calcium compound；
E) nano-calcium carbonate calcium compound implementation separation of solid and liquid is obtained into solid nano calcium carbonate with solid-liquid separator, then will
Solid nano calcium carbonate, which is placed in vacuum desiccator, dries 10h, finally gives nano-calcium carbonate calcium powder.
Further, the limestone calcination temperature is 1050-1090 DEG C.
Further, the calcium oxide in a kettle with water course of reaction, side border ring is stirred.
Further, the aqua calcis is positioned in isolation space after preparing and precipitates 20-24 hours, hydrogen-oxygen
After change calcium solution temperature drops to normal temperature, filtering reuses.
Further, the reaction temperature of the aqua calcis and carbon dioxide is controlled at 20-60 DEG C.
Further, the reaction pressure of the aqua calcis and carbon dioxide is controlled in 0.5-1MPa.
By adopting the above-described technical solution, the beneficial effects of the invention are as follows：
The present invention controls titanium dioxide in carbon dioxide and nitrogen mixed gas by controlling the concentration of aqua calcis
Carbon content controls the formation speed of calcium carbonate so that the same position same time can be only generated a small amount of calcium carbonate, so as to make
For the calcium carbonate crystal body of required particle diameter is gone out, calcium carbonate crystal body epigranular, particle diameter are small, steady quality.Hydrogen in the present invention
Calcium oxide solution, carbon dioxide and nitrogen mixed gas, water recycle, and reduce the waste of carbon dioxide, reduce production
Cost.
【Embodiment】
For a better understanding of the present invention, technical scheme is described in detail with instantiation below, but originally
Invention is not limited thereto.
Embodiment 1：
A kind of production method of nano-calcium carbonate, comprises the following steps：
A) calcium oxide is made in lime stone with calciner, calcining heat is 1050 DEG C, manufactured calcium oxide is put into anti-
Answer in kettle, add water in a kettle, side border ring is stirred, and the aqua calcis that percentage by weight is 5% is made, just
The aqua calcis prepared is positioned in isolation space and precipitates 20 hours, and after temperature drops to normal temperature, filtering is again
Use；
B) aqua calcis of preparation is spilled at the top of autoclave with shower nozzle, then from autoclave
Middle part is passed through the carbon dioxide and nitrogen mixed gas that carbon dioxide content is 3%, and the flow rate for controlling mixed gas is 40m3/
(h·m3Aqua calcis), while control mixed gas to discharge autoclave, autoclave medium temperature with identical flow velocity
Degree control is at 20 DEG C, and pressure control is in 0.5MPa；
C) aqua calcis for falling into autoclave bottom is filtered using solid-liquid separator, collects consolidating for filtering
Body, and the top of filtrate return autoclave is spilled into again, circulate operation, until the solution pH value of autoclave bottom
Between 7, stop circulation, the solution of autoclave bottom is discharged；
D) added in the solid collected in step c) and account for solid masses than the stearmide for 2% and 4% advanced fat
Fat alcohol, 5h is placed in 80 DEG C of environment, obtain nano-calcium carbonate calcium compound；
E) nano-calcium carbonate calcium compound implementation separation of solid and liquid is obtained into solid nano calcium carbonate with solid-liquid separator, then will
Solid nano calcium carbonate, which is placed in vacuum desiccator, dries 10h, finally gives nano-calcium carbonate calcium powder.
Embodiment 2：
A kind of production method of nano-calcium carbonate, comprises the following steps：
A) calcium oxide is made in lime stone with calciner, calcining heat is 1090 DEG C, manufactured calcium oxide is put into anti-
To answer in kettle, add water in a kettle, side border ring is stirred, and the aqua calcis that percentage by weight is 10% is made,
The aqua calcis just prepared is positioned in isolation space and precipitated 24 hours, and after temperature drops to normal temperature, filtering is again
Use；
B) aqua calcis of preparation is spilled at the top of autoclave with shower nozzle, then from autoclave
Middle part is passed through the carbon dioxide and nitrogen mixed gas that carbon dioxide content is 5%, and the flow rate for controlling mixed gas is 40m3/
(h·m3Aqua calcis), while control mixed gas to discharge autoclave, autoclave medium temperature with identical flow velocity
Degree control is at 60 DEG C, and pressure control is in 1MPa；
C) aqua calcis for falling into autoclave bottom is filtered using solid-liquid separator, collects consolidating for filtering
Body, and the top of filtrate return autoclave is spilled into again, circulate operation, until the solution pH value of autoclave bottom
Between 7.2, stop circulation, the solution of autoclave bottom is discharged；
D) added in the solid collected in step c) and account for solid masses than the stearmide for 4% and 6% advanced fat
Fat alcohol, 5h is placed in 100 DEG C of environment, obtain nano-calcium carbonate calcium compound；
E) nano-calcium carbonate calcium compound implementation separation of solid and liquid is obtained into solid nano calcium carbonate with solid-liquid separator, then will
Solid nano calcium carbonate, which is placed in vacuum desiccator, dries 10h, finally gives nano-calcium carbonate calcium powder.
Embodiment 3：
A kind of production method of nano-calcium carbonate, comprises the following steps：
A) calcium oxide is made in lime stone with calciner, calcining heat is 1070 DEG C, manufactured calcium oxide is put into anti-
Answer in kettle, add water in a kettle, side border ring is stirred, and the aqua calcis that percentage by weight is 7% is made, just
The aqua calcis prepared is positioned in isolation space and precipitated 22 hours, and after temperature drops to normal temperature, filtering makes again
With；
B) aqua calcis of preparation is spilled at the top of autoclave with shower nozzle, then from autoclave
Middle part is passed through the carbon dioxide and nitrogen mixed gas that carbon dioxide content is 4%, and the flow rate for controlling mixed gas is 40m3/
(h·m3Aqua calcis), while control mixed gas to discharge autoclave, autoclave medium temperature with identical flow velocity
Degree control is at 40 DEG C, and pressure control is in 0.7MPa；
C) aqua calcis for falling into autoclave bottom is filtered using solid-liquid separator, collects consolidating for filtering
Body, and the top of filtrate return autoclave is spilled into again, circulate operation, until the solution pH value of autoclave bottom
Between 7.1, stop circulation, the solution of autoclave bottom is discharged；
D) added in the solid collected in step c) and account for solid masses than the stearmide for 3% and 5% advanced fat
Fat alcohol, 5h is placed in 90 DEG C of environment, obtain nano-calcium carbonate calcium compound；
E) nano-calcium carbonate calcium compound implementation separation of solid and liquid is obtained into solid nano calcium carbonate with solid-liquid separator, then will
Solid nano calcium carbonate, which is placed in vacuum desiccator, dries 10h, finally gives nano-calcium carbonate calcium powder.
Experimental result：The scheme that embodiment 1-3 is respectively adopted prepares 100kg nano-calcium carbonates, the nano-sized carbon prepared
Sour calcium mean particle 86nm, is fluctuated within 28nm, result of the test is shown in Table 1.
The experimental result table of table 1
Described above is the detailed description for the present invention preferably possible embodiments, but embodiment is not limited to this hair
Bright patent claim, the equal change completed or modification change under the technical spirit suggested by all present invention, all should belong to
Cover the scope of the claims in the present invention.
Claims (6)
1. a kind of production method of nano-calcium carbonate, it is characterised in that comprise the following steps：
A) calcium oxide is made in lime stone with calciner, and manufactured calcium oxide is put into reactor, added in a kettle
Enter water and the aqua calcis that percentage by weight is 5%-10% is made；
B) aqua calcis of preparation is spilled at the top of autoclave with shower nozzle, then from the middle part of autoclave
The carbon dioxide and nitrogen mixed gas that carbon dioxide content is 3%-5% are passed through, the flow rate for controlling mixed gas is 40m3/
(h·m3Aqua calcis), while control mixed gas to discharge autoclave with identical flow velocity；
C) aqua calcis for falling into autoclave bottom is filtered using solid-liquid separator, collects the solid of filtering, and
The top that filtrate is returned to autoclave is spilled into again, circulate operation, until the solution pH value of autoclave bottom is in 7-
Between 7.2, stop circulation, the solution of autoclave bottom is discharged；
D) add that to account for solid masses higher than the stearmide for 2%-4% and 4%-6% in the solid collected in the step c)
Level fatty alcohol, places 5h in 80-100 DEG C of environment, obtains nano-calcium carbonate calcium compound；
E) nano-calcium carbonate calcium compound implementation separation of solid and liquid is obtained into solid nano calcium carbonate with solid-liquid separator, then by solid
Nano-calcium carbonate, which is placed in vacuum desiccator, dries 10h, finally gives nano-calcium carbonate calcium powder.
2. the preparation method of high dispersion of nano-calcium carbonate according to claim 1, it is characterised in that the lime stone is forged
It is 1050-1090 DEG C to burn temperature.
3. the preparation method of high dispersion of nano-calcium carbonate according to claim 1, it is characterised in that the calcium oxide exists
In reactor with water course of reaction, side border ring is stirred.
4. the preparation method of high dispersion of nano-calcium carbonate according to claim 1, it is characterised in that the calcium hydroxide
Solution is positioned in isolation space after preparing and precipitates 20-24 hours, after aqua calcis temperature drops to normal temperature, filtering
Reuse.
5. the preparation method of high dispersion of nano-calcium carbonate according to claim 1, it is characterised in that the calcium hydroxide
The reaction temperature of solution and carbon dioxide is controlled at 20-60 DEG C.
6. the preparation method of high dispersion of nano-calcium carbonate according to claim 5, it is characterised in that the calcium hydroxide
The reaction pressure of solution and carbon dioxide is controlled in 0.5-1MPa.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110484023A (en) * | 2019-09-30 | 2019-11-22 | 建德市华宇纳米科技有限公司 | A kind of high-dispersion nano calcium carbonate Preparation equipment and preparation method |
| CN111704153A (en) * | 2020-07-01 | 2020-09-25 | 临澧鑫众钙业有限公司 | Method for processing and refining calcium hydroxide by using lime |
| CN112209347A (en) * | 2020-10-10 | 2021-01-12 | 吴剑华 | Preparation method of hydrogen chloride-free hypochlorous acid for producing epoxide by using monochloro alcohol monoacid method |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS54149399A (en) * | 1978-05-15 | 1979-11-22 | Shiraishi Kogyo Kaisha Ltd | Manufacture of cubic calcium carbonate |
| CN1453216A (en) * | 2002-04-26 | 2003-11-05 | 北京化工大学 | Eddy flow process of preparing ultramicro calcium carbonate precipitate |
| CN101027253A (en) * | 2004-07-13 | 2007-08-29 | Fp颜料有限公司 | Method and apparatus for manufacturing of a calcium carbonate product, the product and its use |
| CN101970753A (en) * | 2008-03-07 | 2011-02-09 | Fp颜料有限公司 | A pigment particle composition, its method of manufacture and its use |
| CN103011226A (en) * | 2012-12-07 | 2013-04-03 | 池州凯尔特纳米科技有限公司 | Method for preparing nano calcium carbonate through nucleation and growth step by step |
| CN105800658A (en) * | 2016-04-22 | 2016-07-27 | 广西合山东来化工科技有限公司 | Method for efficiently preparing nano calcium carbonate |
-
2017
- 2017-09-30 CN CN201710919720.1A patent/CN107601541A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS54149399A (en) * | 1978-05-15 | 1979-11-22 | Shiraishi Kogyo Kaisha Ltd | Manufacture of cubic calcium carbonate |
| CN1453216A (en) * | 2002-04-26 | 2003-11-05 | 北京化工大学 | Eddy flow process of preparing ultramicro calcium carbonate precipitate |
| CN101027253A (en) * | 2004-07-13 | 2007-08-29 | Fp颜料有限公司 | Method and apparatus for manufacturing of a calcium carbonate product, the product and its use |
| CN101970753A (en) * | 2008-03-07 | 2011-02-09 | Fp颜料有限公司 | A pigment particle composition, its method of manufacture and its use |
| CN103011226A (en) * | 2012-12-07 | 2013-04-03 | 池州凯尔特纳米科技有限公司 | Method for preparing nano calcium carbonate through nucleation and growth step by step |
| CN105800658A (en) * | 2016-04-22 | 2016-07-27 | 广西合山东来化工科技有限公司 | Method for efficiently preparing nano calcium carbonate |
Non-Patent Citations (1)
| Title |
|---|
| 曾人泉: "《塑料加工助剂》", 30 September 1997 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110484023A (en) * | 2019-09-30 | 2019-11-22 | 建德市华宇纳米科技有限公司 | A kind of high-dispersion nano calcium carbonate Preparation equipment and preparation method |
| CN110484023B (en) * | 2019-09-30 | 2021-05-14 | 建德市华宇纳米科技有限公司 | Preparation equipment and preparation method of high-dispersion nano calcium carbonate |
| CN111704153A (en) * | 2020-07-01 | 2020-09-25 | 临澧鑫众钙业有限公司 | Method for processing and refining calcium hydroxide by using lime |
| CN111704153B (en) * | 2020-07-01 | 2022-05-03 | 临澧鑫众钙业有限公司 | Method for processing and refining calcium hydroxide by using lime |
| CN112209347A (en) * | 2020-10-10 | 2021-01-12 | 吴剑华 | Preparation method of hydrogen chloride-free hypochlorous acid for producing epoxide by using monochloro alcohol monoacid method |
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Application publication date: 20180119 |