CN105084404A - Preparation method for micro-calcium-carbonate particles - Google Patents
Preparation method for micro-calcium-carbonate particles Download PDFInfo
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- CN105084404A CN105084404A CN201510497740.5A CN201510497740A CN105084404A CN 105084404 A CN105084404 A CN 105084404A CN 201510497740 A CN201510497740 A CN 201510497740A CN 105084404 A CN105084404 A CN 105084404A
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Abstract
The invention belongs to the field of preparation of calcium carbonate, and particularly relates to a preparation method for micro-calcium-carbonate particles. The micro-calcium-carbonate particles are made of, by mass, 0.10-0.12 part of calcium chloride, 0.08-0.10 part of ammonium carbonate, 0.88-0.92 part of water and a small amount of additives. The preparation method comprises the steps that firstly, the calcium chloride is dissolved, and a proper amount of organic alcohol and a proper amount of emulsifier are added; secondly, the ammonium carbonate is dissolved, and a proper amount of phosphoric acid compound and a proper amount of emulsifier are added; thirdly, the calcium chloride and the ammonium carbonate are mixed at certain temperature and certain rotating speed to obtain micro-calcium-carbonate. According to the preparation method, the raw materials are easy to obtain, the preparation method is simple, easy to operate and low in energy consumption, industrial production is facilitated, and the obtained micro-calcium-carbonate particles have the advantages of being compact in structure, stable in size, uniform in distribution within several micrometers and low in cost.
Description
technical field:
The present invention relates to a kind of preparation method of micro-calcium carbonate particle.
background technology:
Calcium carbonate is the mineral filler that in current macromolecular material, consumption is maximum, due to inexpensive, nontoxic and be widely used in the fields such as rubber, plastics, papermaking, ink, coating, daily-use chemical industry, is both domestic and externally in great demand.At present, industrial main employing Wingdale, as raw material, though cost is cheap, causes comparatively havoc to physical environment, will consume mass energy in high-temperature exercise process, and product cut size skewness.
In recent years; people are devoted to the preparation method developing new micro-calcium carbonate; such as gravity Method, microemulsion method, double decomposition etc., have protection of the environment, reduce energy consumption while the traditional calcium carbonate product performance of change, is that calcium carbonate industry produces urgent problem.
summary of the invention:
The invention provides a kind of preparation method of micro-calcium carbonate particle, utilize a large amount of side product chlorinated calcium in Chemical Manufacture to replace Wingdale to be raw material, its preparation method is simple, stable operation, cost-saving, reduce energy consumption, the Carbonate Particle Size of preparation is evenly distributed, technique is simple, be easy to industrialization.
Technical scheme of the present invention is:
A preparation method for micro-calcium carbonate particle, is characterized in that, the mass parts of each feed composition is: calcium chloride 0.10-0.12, volatile salt 0.08-0.10, water 0.88-0.92, a small amount of additive.
The preparation method of described a kind of micro-calcium carbonate particle, is characterized in that comprising the following steps:
(1) calcium chloride is proceeded to the main still of reaction, water is added than the ratio for 1:8-10 in calcium chloride and quality, the ratio being 1:0.02-0.04 in calcium chloride and Organic Alcohol mass ratio adds Organic Alcohol, adds emulsifying agent, start stirring by the 0.04-0.06% of calcium chloride quality;
(2) be that volatile salt to proceed to and reacts secondary still by the ratio of 1:0.85-0.95 in calcium chloride and volatile salt mass ratio, the ratio being 1:9-11 in the mass ratio of volatile salt and water adds water, be that 1:0.015-0.025 ratio adds phosphoric acid based compound in volatile salt and phosphoric acid based compound mass ratio, add emulsifying agent by the 0.035-0.045% of ammonium chloride quality, start stirring;
(3) sal volatile is slowly proceeded to the main still of reaction, accelerate to stir, control to shift in 1.5-2.0 hour complete, insulation at 25 DEG C-30 DEG C, then to react after 1.5-2.0 hour decompress filter immediately, washes with water 2-3 time, vacuum-drying again, discharging, metering, packaging.
The preparation method of described a kind of micro-calcium carbonate particle, is characterized in that: described Organic Alcohol is ethylene glycol or glycerol.
The preparation method of described a kind of micro-calcium carbonate particle, is characterized in that: described emulsifying agent is Sodium dodecylbenzene sulfonate or cetyl trimethylammonium bromide.
Described phosphoric acid based compound is Sodium phosphate dibasic or Secondary ammonium phosphate.
The mixing speed of described (1) and (2) step is 100-200 rev/min, and the mixing speed of (3) step is 400-500 rev/min.
Preparation method's advantages of simple, the raw material of micro-calcium carbonate particle of the present invention are easy to get, cheap, there is good size-grade distribution and stability.Preparation method's safety performance of the present invention is stablized, reduces energy consumption, is easy to suitability for industrialized production, reduces production cost, improves production efficiency.
Accompanying drawing explanation
The scanning electron microscopic picture of the micro-calcium carbonate of Fig. 1 obtained by embodiment 3.
Embodiment
Following examples further illustrate of the present invention, is not limitation of the present invention.
A kind of preparation method of micro-calcium carbonate particle:
[embodiment 1]
(1) 0.3t calcium chloride is proceeded to the main still of reaction, add 2.7t water, start stirring 15 minutes, rotating speed 100-200 rev/min, add 9Kg ethylene glycol, 150g Sodium dodecylbenzene sulfonate, then stir 15 minutes.
(2) 0.27t volatile salt is proceeded to the secondary still of reaction, add 2.7t water, start stirring 15 minutes, rotating speed 100-200 rev/min, add 5.4Kg Secondary ammonium phosphate, 100g cetyl trimethylammonium bromide, then stir 15 minutes.
(3) sal volatile is slowly proceeded to the main still of reaction, mixing speed is adjusted to 400-500 rev/min, control was shifted complete in 1.5-2.0 hour, insulation is at 25 DEG C-30 DEG C, to react after 1.5-2.0 hour decompress filter immediately again, wash with water 2-3 time, then vacuum-drying, discharging, metering, packaging.
[embodiment 2]
(1) 0.3t calcium chloride is proceeded to the main still of reaction, add 2.7t water, start stirring 15 minutes, rotating speed 100-200 rev/min, add 9Kg glycerol, 150g Sodium dodecylbenzene sulfonate, then stir 15 minutes.
(2) 0.27t volatile salt is proceeded to the secondary still of reaction, add 2.7t water, start stirring 15 minutes, rotating speed 100-200 rev/min, add 5.4Kg Sodium phosphate dibasic, 100g cetyl trimethylammonium bromide, then stir 15 minutes.
(3) sal volatile is slowly proceeded to the main still of reaction, mixing speed is adjusted to 400-500 rev/min, control was shifted complete in 1.5-2.0 hour, insulation is at 25 DEG C-30 DEG C, to react after 1.5-2.0 hour decompress filter immediately again, wash with water 2-3 time, then vacuum-drying, discharging, metering, packaging.
[embodiment 3]
(1) 0.3t calcium chloride is proceeded to the main still of reaction, add 2.7t water, start stirring 15 minutes, rotating speed 100-200 rev/min, add 9Kg ethylene glycol and glycerol (mass ratio of ethylene glycol and glycerol is 1:1), 150g Sodium dodecylbenzene sulfonate, then stir 15 minutes.
(2) 0.27t volatile salt is proceeded to the secondary still of reaction, add 2.7t water, start stirring 15 minutes, rotating speed 100-200 rev/min, add 5.4Kg Sodium phosphate dibasic and Secondary ammonium phosphate (Sodium phosphate dibasic and Secondary ammonium phosphate mass ratio are 1:1), 100g cetyl trimethylammonium bromide, then stir 15 minutes.
(3) sal volatile is slowly proceeded to the main still of reaction, mixing speed is adjusted to 400-500 rev/min, control was shifted complete in 1.5-2.0 hour, insulation is at 25 DEG C-30 DEG C, to react after 1.5-2.0 hour decompress filter immediately again, wash with water 2-3 time, then vacuum-drying, discharging, metering, packaging.
Claims (6)
1. a preparation method for micro-calcium carbonate particle, is characterized in that, the mass parts of each feed composition is: calcium chloride 0.10-0.12, volatile salt 0.08-0.10, water 0.88-0.92, a small amount of additive.
2. the preparation method of a kind of micro-calcium carbonate particle according to claim 1, is characterized in that comprising the following steps:
(1) calcium chloride is proceeded to the main still of reaction, water is added than the ratio for 1:8-10 in calcium chloride and quality, the ratio being 1:0.02-0.04 in calcium chloride and Organic Alcohol mass ratio adds Organic Alcohol, adds emulsifying agent, start stirring by the 0.04-0.06% of calcium chloride quality;
(2) be that volatile salt to proceed to and reacts secondary still by the ratio of 1:0.85-0.95 in calcium chloride and volatile salt mass ratio, the ratio being 1:9-11 in the mass ratio of volatile salt and water adds water, be that 1:0.015-0.025 ratio adds phosphoric acid based compound in volatile salt and phosphoric acid based compound mass ratio, add emulsifying agent by the 0.035-0.045% of ammonium chloride quality, start stirring;
(3) sal volatile is slowly proceeded to the main still of reaction, accelerate to stir, control to shift in 1.5-2.0 hour complete, insulation at 25 DEG C-30 DEG C, then to react after 1.5-2.0 hour decompress filter immediately, washes with water 2-3 time, vacuum-drying again, discharging, metering, packaging.
3. the preparation method of a kind of micro-calcium carbonate particle according to claim 2, is characterized in that: described Organic Alcohol is ethylene glycol or glycerol.
4. the preparation method of a kind of micro-calcium carbonate particle according to claim 2, is characterized in that: described emulsifying agent is Sodium dodecylbenzene sulfonate or cetyl trimethylammonium bromide.
5. the preparation method of a kind of micro-calcium carbonate particle according to claim 2, is characterized in that: described phosphoric acid based compound is Sodium phosphate dibasic or Secondary ammonium phosphate.
6. the preparation method of a kind of micro-calcium carbonate particle according to claim 2, is characterized in that:
The mixing speed of described (1) and (2) step is 100-200 rev/min, and the mixing speed of (3) step is 400-500 rev/min.
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| CN201510497740.5A CN105084404A (en) | 2015-08-13 | 2015-08-13 | Preparation method for micro-calcium-carbonate particles |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109133137A (en) * | 2018-11-14 | 2019-01-04 | 上海应用技术大学 | A kind of micro-nano calcium carbonate of ellipsoid and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102126736A (en) * | 2011-01-19 | 2011-07-20 | 刘先黎 | Method for preparing nano-calcium carbonate powder by using soluble 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 |
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- 2015-08-13 CN CN201510497740.5A patent/CN105084404A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102126736A (en) * | 2011-01-19 | 2011-07-20 | 刘先黎 | Method for preparing nano-calcium carbonate powder by using soluble 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 |
Non-Patent Citations (1)
| Title |
|---|
| 庄斌等: "由氯化钙制备纳米碳酸钙研究", 《化工矿物与加工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109133137A (en) * | 2018-11-14 | 2019-01-04 | 上海应用技术大学 | A kind of micro-nano calcium carbonate of ellipsoid and preparation method thereof |
| CN109133137B (en) * | 2018-11-14 | 2020-12-08 | 上海应用技术大学 | Ellipsoidal micro-nano calcium carbonate and preparation method thereof |
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