CN105645451A - Method for preparing micropowder-grade light calcium carbonate - Google Patents
Method for preparing micropowder-grade light calcium carbonate Download PDFInfo
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- CN105645451A CN105645451A CN201610103627.9A CN201610103627A CN105645451A CN 105645451 A CN105645451 A CN 105645451A CN 201610103627 A CN201610103627 A CN 201610103627A CN 105645451 A CN105645451 A CN 105645451A
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- sodium carbonate
- calcium chloride
- containing sodium
- solution
- micro powder
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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
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- 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
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- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (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 method for preparing micropowder-grade light calcium carbonate. The method is characterized in that a calcium chloride solution as a byproduct of chemical production and a solution containing sodium carbonate are taken as raw materials for preparation; the method comprises steps as follows: step one, the concentration of sodium carbonate in the solution containing sodium carbonate and the concentration of calcium chloride in the byproduct are measured through sampling, and the total amount of contained sodium carbonate and the total amount of required calcium chloride are worked out according to the volume of the to-be-processed solution containing sodium carbonate; step two, the byproduct is added to the solution containing sodium carbonate, and a molar ratio of calcium chloride to sodium carbonate is (0.7-1.4):1; step three, a stirring speed in a reactor is controlled at 40-500 r/min, and calcium chloride and sodium carbonate react sufficiently; step four, products obtained after the reaction are subjected to solid-liquid separation, and micropowder-grade light calcium carbonate is obtained.
Description
Technical field
The technical field that the present invention relates to is to utilize by-product calcium chloride solution in Chemical Manufacture to mix with containing sodium carbonate solution, utilizes certain reaction condition to control calcium chloride and reacts with sodium carbonate, produces micro powder grade precipitated calcium carbonate.
Background technology
In current industry, the production method of micro powder grade precipitated calcium carbonate mainly adopts carbonizatin method. The raw material calcinings such as limestone are generated Calx (Main Ingredients and Appearance is calcium oxide) and carbon dioxide, add water digestion Calx and generate lime cream (Main Ingredients and Appearance is calcium hydroxide), then passing into carbon dioxide carbonization lime cream again and generate precipitation of calcium carbonate, last precipitation of calcium carbonate is through dehydration, dry and pulverizing just prepared precipitated calcium carbonate.
Said method is primarily present following shortcoming:
1, the technological process of production is longer, and production cost is of a relatively high;
2, product quality fluctuation is relatively big, and impurity content is higher;
In chemical process, the calcium chloride having a lot of by-product needs to process, also the solution having a lot of containing sodium carbonate to remove sodium carbonate therein, it is an object of the invention to utilize two kinds of material reactions, generate calcium carbonate, be possible not only to remove sodium carbonate in solution, and consume substantial amounts of calcium chloride, low cost produce micro powder grade precipitated calcium carbonate.
Summary of the invention
To achieve these goals, first technical scheme of the present invention is a kind of method producing micro powder grade precipitated calcium carbonate, it is characterised in that in Chemical Manufacture, the calcium chloride solution of by-product and containing sodium carbonate solution are waste, comprise the following steps,
Step one: calcium chloride concentration in the concentration of sodium carbonate in containing sodium carbonate solution and by-product is measured in sampling, and according to the stereometer of the containing sodium carbonate solution of required process calculate containing sodium carbonate total amount and required calcium chloride total amount;
Step 2: add described by-product in containing sodium carbonate solution, and to make the mol ratio of calcium chloride and sodium carbonate be 0.7��1.4:1;
Step 3: speed of agitator controls at 40��500 revs/min in the reactor, makes calcium chloride and sodium carbonate fully react;
Step 4: reacted product is carried out solid-liquid separation, obtains micro powder grade precipitated calcium carbonate.
Second technical scheme is based on the first technical scheme, it is characterised in that in described containing sodium carbonate solution, sodium carbonate is the impurity that need to remove.
3rd technical scheme is based on the first or second technical scheme, it is characterized in that, in described step one, first the containing sodium carbonate solution of certain volume is taken out, be slowly added in containing sodium carbonate solution detection calcium chloride solution or calcium chloride solid until containing sodium carbonate solution no longer has Precipitation, the precipitation generated is weighed after drying through washing and is obtained quality, converses the levels of the sodium carbonate in containing sodium carbonate solution according to the volume of the quality of precipitation and sampling.
4th technical scheme is based on the firstth or second technical scheme, it is characterised in that the time controlling fully reaction in described step 3 is 8��60 minutes.
5th technical scheme is based on the first or second technical scheme, it is characterised in that in step 4, adopts centrifuge to process to reduce the mother solution of solid entrained with in slip isolated slip.
Accompanying drawing explanation
By reading hereafter detailed description of the preferred embodiment, various other advantage and benefit those of ordinary skill in the art be will be clear from understanding. Accompanying drawing is only for illustrating the purpose of preferred implementation, and is not considered as limitation of the present invention.
Fig. 1 illustrates the process chart of embodiment of the present invention.
Detailed description of the invention
The invention provides many applicable creative concepts, this creativeness concept can be reflected in a large number of in concrete context. It is only used as the exemplary illustration of the specific embodiment of the present invention in the specific embodiment described in following embodiments of the present invention, and is not meant to limit the scope of the invention.
Below in conjunction with accompanying drawing and specific embodiment, the invention will be further described.
Raw material is the calcium chloride solution of by-product and containing sodium carbonate solution in Chemical Manufacture in the present embodiment, containing sodium carbonate solution is that various not containing can with the solution of calcium chloride generation chemical reaction, in the present embodiment, the sodium carbonate in containing sodium carbonate solution is the material that need to remove. Utilize the chemical reaction of calcium chloride and sodium carbonate, reach to remove the purpose of sodium carbonate, prepare high-quality micro powder grade precipitated calcium carbonate (product granularity 0.5��5 ��m) simultaneously.
Test through inventor is groped, and utilizes after in Chemical Manufacture, the calcium chloride solution of by-product mixes with containing sodium carbonate solution, calcium chloride and the principle of sodium carbonate generation displacement reaction in solution, can produce high-quality micro powder grade precipitated calcium carbonate by controlling reaction condition.
Fig. 1 is the process chart of present embodiment.
Step one: calcium chloride concentration in the concentration of sodium carbonate in containing sodium carbonate solution and by-product is measured in sampling, and according to the stereometer of the containing sodium carbonate solution (original solution) of required process calculate containing sodium carbonate total amount and required calcium chloride total amount;
Step 2: add the calcium chloride solution of by-product in containing sodium carbonate solution, and to make the mol ratio of calcium chloride and sodium carbonate be 0.7��1.4:1, mixes as put into by the calcium chloride solution 2 of containing sodium carbonate solution 1 and by-product in reactor 3;
Step 3: stirring in reactor 3, rotating speed controls at 40��500 revs/min, makes calcium chloride and sodium carbonate fully react;
Step 4: with filter 4, reacted product (slip) is carried out solid-liquid separation, obtain micro powder grade precipitated calcium carbonate 5.
Wherein, in described step one sampling and measuring original solution, the detailed process of the method for concentration of sodium carbonate is: first take out the containing sodium carbonate solution of certain volume, be slowly added in containing sodium carbonate solution detection calcium chloride solution or calcium chloride solid until containing sodium carbonate solution no longer has Precipitation, the precipitation generated is weighed after drying through washing and is obtained quality, converses the levels of the sodium carbonate in original solution according to the volume of the quality of precipitation and sampling.
Wherein, the time controlling fully reaction in described step 3 is 8��60 minutes.
Further, in step 4, also centrifuge can be adopted to process to reduce the mother solution of solid entrained with in slip isolated slip.
Further, substantially remove complete because of sodium carbonate through the isolated liquid of step 4 so that it is enter next production process (under walk operation) 6.
In present embodiment, reactor is common response still, and reactor size can be determined according to yield. Common pusher stirring joined by reactor, and stirring size can be determined according to reactor size; Rotating speed requires to be determined according to product granularity; Preparation micro powder grade precipitated calcium carbonate, the range of speed control 40��500r/min. In reactor, first add a certain amount of containing sodium carbonate solution (concentration of sodium carbonate 50��200g/l) during charging, in still, after opening stirring, add the calcium chloride solution of by-product again.
Calcium chloride concentration controls about 30%��55% (not only can reduce the diluting effect to containing sodium carbonate solution, and the optium concentration for reacting), within every 10 minutes, charging rate is the 15%��30% of containing sodium carbonate amount of solution, and the mol ratio of calcium chloride and sodium carbonate is 0.7��1.4:1.
After calcium chloride solution has added, in order to ensure that reaction fully uniformly to control the response time with the calcium carbonate crystal generated, it is preferred that the response time is 8��60 minutes, and the concrete response time need to determine according to carbonate content in thick hydrazine hydrate.
In the present embodiment, because course of reaction is exothermic reaction, described course of reaction liquid has intensification.
By the detection to calcium carbonate, the method for present embodiment the calcium carbonate product granularity produced is 0.5��5 ��m, reaches the rank of high-quality micro powder grade precipitated calcium carbonate.
Relative to prior art, method of the present invention has the advantage that
1. the present invention adopts chemical method to remove the sodium carbonate in solution, because being precipitation, so sodium carbonate removal efficiency and effect are all fine;
2. the calcium chloride transformation making by-product becomes the calcium product that added value is higher, and the process saving calcium chloride puts into, and adds production value;
3. shortening relative to traditional mode of production micro powder grade its process route of precipitated calcium carbonate method, therefore cost puts into and decreases. And concrete technological operation also simplifies, technique consuming time is therefore greatly reduced on the whole, improves treatment effeciency.
4. the purity of the solid product calcium carbonate that the process of employing chemical method provided by the invention obtains is higher, and product granularity is relatively thin, reaches micro powder grade precipitated calcium carbonate rank, can be used for outer selling, further increases the economic benefit of the present invention;
To sum up, the present invention has had relative to traditional method, process efficiency and economic benefit and has been obviously improved.
Traditional lightweight calcium carbonate production technology is that the raw material calcinings such as limestone are generated Calx (being mainly composed of calcium oxide) and carbon dioxide, add water digestion Calx and generate lime cream (being mainly composed of calcium hydroxide), then pass into carbon dioxide carbonization lime cream again and generate precipitation of calcium carbonate, through dehydration, dry and pulverize and prepare after, or first carry out metathesis reaction with sodium carbonate and calcium chloride and generate precipitation of calcium carbonate, then prepare through dehydration, dry and pulverizing. Compared with traditional handicraft, this Technology has following characteristics:
1. the present invention realizes One-step production precipitated calcium carbonate, and process route is short, and Productive statistics and operating cost are low;
2. the present invention utilizes the calcium chloride of by-product in Chemical Manufacture to be raw material, produces high-quality precipitated calcium carbonate, and economy is higher;
3. the calcium carbonate produced purity after filtering, washing can reach more than 97%, and (comparing traditional handicraft, product purity is high, and other metal impurities are few, steady quality), primary production granularity reaches 0.5��5 ��m, is fully achieved light calcium carbonate product requirement, and product economy is worth higher;
4. present invention process process realizes one-step method and removes sodium carbonate in thick solution, and precipitation makes sodium carbonate just be completely removed through this step. Not only production process technology route is shorter, and less investment.
By embodiments of the present invention it can be seen that whole technical process reduces removes sodium carbonate, the energy expenditure processing calcium chloride and Meteorological from sodium carbonate liquor, produce and there is relatively high value added product, be more conform to economy, rational Technology. It is low that the micro powder grade sodium carbonate simultaneously prepared has cost, the advantage that impurity is few.
Claims (5)
1. the method producing micro powder grade precipitated calcium carbonate, it is characterised in that the calcium chloride solution of by-product and containing sodium carbonate solution are waste in Chemical Manufacture, comprise the following steps,
Step one: calcium chloride concentration in the concentration of sodium carbonate in containing sodium carbonate solution and by-product is measured in sampling, and according to the stereometer of the containing sodium carbonate solution of required process calculate containing sodium carbonate total amount and required calcium chloride total amount;
Step 2: add described by-product in containing sodium carbonate solution, and to make the mol ratio of calcium chloride and sodium carbonate be 0.7��1.4:1;
Step 3: speed of agitator controls at 40��500 revs/min in the reactor, makes calcium chloride and sodium carbonate fully react;
Step 4: reacted product is carried out solid-liquid separation, obtains micro powder grade precipitated calcium carbonate.
2. the method producing micro powder grade precipitated calcium carbonate according to claim 1, it is characterised in that in described containing sodium carbonate solution, sodium carbonate is the impurity that need to remove.
3. the method producing micro powder grade precipitated calcium carbonate recorded any one of claim 1 to 2, it is characterized in that, in described step one, first the containing sodium carbonate solution of certain volume is taken out, be slowly added in containing sodium carbonate solution detection calcium chloride solution or calcium chloride solid until containing sodium carbonate solution no longer has Precipitation, the precipitation generated is weighed after drying through washing and is obtained quality, converses the levels of the sodium carbonate in containing sodium carbonate solution according to the volume of the quality of precipitation and sampling.
4. the method producing micro powder grade precipitated calcium carbonate recorded any one of claim 1 to 2, it is characterised in that the time controlling fully reaction in described step 3 is 8��60 minutes.
5. the method producing micro powder grade precipitated calcium carbonate recorded any one of claim 1 to 2, it is characterised in that in step 4, adopts centrifuge to process to reduce the mother solution of solid entrained with in slip isolated slip.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52149298A (en) * | 1976-06-07 | 1977-12-12 | Central Glass Co Ltd | Production of globular minute-particle n-cac03 |
| JPS5595617A (en) * | 1979-01-09 | 1980-07-21 | Shiseido Co Ltd | Production of spherical calcium carbonate |
| CN1657413A (en) * | 2004-12-03 | 2005-08-24 | 天津化工研究设计院 | Preparation method of lamellar crystal light calcium carbonate for paper making coating |
| CN1830796A (en) * | 2005-03-11 | 2006-09-13 | 胡志彤 | Manufacturing method of high purity calcium carbonate for electron industry |
| CN104860275A (en) * | 2015-04-15 | 2015-08-26 | 杭州海虹精细化工有限公司 | Method for removing sodium carbonate from hydrazine hydrate crude solution |
| CN105036098A (en) * | 2015-09-01 | 2015-11-11 | 青海盐湖工业股份有限公司 | Method for removing sodium carbonate in solution |
-
2016
- 2016-02-25 CN CN201610103627.9A patent/CN105645451A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52149298A (en) * | 1976-06-07 | 1977-12-12 | Central Glass Co Ltd | Production of globular minute-particle n-cac03 |
| JPS5595617A (en) * | 1979-01-09 | 1980-07-21 | Shiseido Co Ltd | Production of spherical calcium carbonate |
| CN1657413A (en) * | 2004-12-03 | 2005-08-24 | 天津化工研究设计院 | Preparation method of lamellar crystal light calcium carbonate for paper making coating |
| CN1830796A (en) * | 2005-03-11 | 2006-09-13 | 胡志彤 | Manufacturing method of high purity calcium carbonate for electron industry |
| CN104860275A (en) * | 2015-04-15 | 2015-08-26 | 杭州海虹精细化工有限公司 | Method for removing sodium carbonate from hydrazine hydrate crude solution |
| CN105036098A (en) * | 2015-09-01 | 2015-11-11 | 青海盐湖工业股份有限公司 | Method for removing sodium carbonate in solution |
Non-Patent Citations (1)
| Title |
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| 张德: "轻质碳酸钙与重质碳酸钙比较", 《非金属矿》 * |
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Application publication date: 20160608 |