CN100509632C - Production of high-purity spherical nano-calcium carbonate - Google Patents
Production of high-purity spherical nano-calcium carbonate Download PDFInfo
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- CN100509632C CN100509632C CNB2007100525565A CN200710052556A CN100509632C CN 100509632 C CN100509632 C CN 100509632C CN B2007100525565 A CNB2007100525565 A CN B2007100525565A CN 200710052556 A CN200710052556 A CN 200710052556A CN 100509632 C CN100509632 C CN 100509632C
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- calcium carbonate
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- calcium chloride
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 58
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 36
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 25
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 25
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 25
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 23
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000001110 calcium chloride Substances 0.000 claims abstract description 13
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 8
- 239000012535 impurity Substances 0.000 claims abstract description 8
- 238000005255 carburizing Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 238000003763 carbonization Methods 0.000 claims description 17
- 239000002002 slurry Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 229920002125 Sokalan® Polymers 0.000 claims description 9
- 150000001408 amides Chemical class 0.000 claims description 9
- 239000004584 polyacrylic acid Substances 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000012295 chemical reaction liquid Substances 0.000 claims description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 6
- 239000012065 filter cake Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 3
- 206010013786 Dry skin Diseases 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 230000005587 bubbling Effects 0.000 abstract description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract 1
- 239000000460 chlorine Substances 0.000 abstract 1
- 229910052801 chlorine Inorganic materials 0.000 abstract 1
- 239000006185 dispersion Substances 0.000 abstract 1
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 229920002401 polyacrylamide Polymers 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 11
- 235000012204 lemonade/lime carbonate Nutrition 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 229920003023 plastic Polymers 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 3
- 239000000292 calcium oxide Substances 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000005060 rubber Substances 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- -1 iron ion Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Production of high-purity spherical calcium carbonate is carried out by taking calcium chloride as chlorine source, taking mixture of calcium hydroxide and polyacrylamide as impurity remover, reacting it with sodium hydroxide, bubbling while carburizing by pure carbon dioxide, growing calcium carbonate crystal grain fast and enlarging. It has excellent purity, activity and dispersion, it simplifies and optimizes process, shortens reactive time and saves energy resources, it costs low and has no environmental pollution.
Description
Technical field
The present invention relates to a kind of production method of lime carbonate, especially relate to a kind of preparation method of high-purity spherical nano-calcium carbonate.
Background technology
Nano-calcium carbonate is meant the ultrafine powder lime carbonate of particle size at 1-100nm, owing to have advantages such as purity height, whiteness are good, fine size, therefore can be used as high-grade packing material, is filled in the various mechanicalss.As be filled in the rubber, but instead of part semi-reinforcing hydrocarbon black or white carbon black, one side can reduce cost, and also can significant reinforcement and sulfuration promoter action be arranged to rubber on the other hand; And be filled in the plastics, then can improve the hardness of plastics and thermotolerance, geometrical stability, and can also allow plastics resistance to wear and performance such as shock resistance greatly improves, exactly because nano-calcium carbonate has above-mentioned various advantages, now be widely used among the industries such as rubber, paper, plastics, coating, textiles, tackiness agent, printing-ink, makeup, feed, therefore improve the performance of product, and reduced production cost of products.
The production process of traditional nano-calcium carbonate is: earlier with selected Wingdale with hard coal in high-temperature calcination, obtain calcium oxide and kiln gas; With calcium oxide digestion, obtain certain density purified calcium hydroxide suspension then; Feed CO afterwards again
2Carry out carbonization, carbonization obtains calcium carbonate serosity to terminal, through subsequent process such as dehydration, drying, surface treatments, finally obtains desired nano-calcium carbonate calcium product again.The production method of above-mentioned lime carbonate is comparatively complicated, to the requirement height of equipment, so that the production cost height, and obtaining lime carbonate impurity height, particle is square, and is active relatively poor.
Summary of the invention
The present invention solves prior art lime carbonate to produce existing complex process, and to conversion unit performance requriements height, reaction process energy consumption height, time are long, cost high-technology problem.
The present invention has also solved prior art lime carbonate simultaneously, and to produce existing product purity low, technical problem such as the big and size-grade distribution of particle is inhomogeneous.
The present invention is mainly solved the problems of the technologies described above by following technical proposals: it may further comprise the steps:
A. solvent temperature is 90-100 ℃, under the condition of continuously stirring, calcium chloride is dissolved in the deionized water, the cleaner that adds calcium chloride weight 3-5% simultaneously, to remove iron ion and suspended substance, filter out impurities then, adding water, to be mixed with 0.2-0.4mol/L calcium chloride solution standby;
B. with dissolution of sodium hydroxide in deionized water, be mixed with 3.5-5.0mol/L sodium hydroxide solution, treat that then it reduces to room temperature, under the condition of continuously stirring, allow it slowly flow in the calcium chloride solution and react, and control reaction temperature is no more than 30 ℃, obtain calcium hydroxide slurry;
C. above-mentioned calcium hydroxide slurry is pumped in the carbonization reactor, feeding flow then is 3.0-5.0m
3/ h pure carbon dioxide carries out carbonization, and control reaction temperature is no more than 30 ℃, and detection reaction liquid pH value is its carburizing reagent terminal point when the reaction solution pH value is 7-7.5, obtain calcium carbonate serosity then;
D. calcium carbonate serosity is put into pressure filter and wash, when washing to washing electrical conductivity of water less than 50us/cm
2The time, press filtration obtains calcium carbonate filter cake, puts it into baking oven then in 110-120 ℃ of constant temperature dryings, when oven dry to its moisture content less than 0.1% the time, take out and pulverize, cross 20 mesh sieves, promptly obtain high-purity spherical nano-calcium carbonate.
As preferably, in the steps A, described cleaner is the mixture of calcium hydroxide and polyacrylic acid amide.
The present invention is the calcium source with calcium chloride, direct and sodium hydroxide reaction, and in conjunction with the control to strength of solution, temperature of reaction, thereby it is complete to have obtained crystal habit, purity is very high, the calcium hydroxide slurry of good dispersity.In addition, owing to generally contain impurity such as molysite, suspended substance in the present industrial calcium chloride, therefore the present invention is a cleaner with the mixture of calcium hydroxide and polyacrylic acid amide, both coordinated, can allow most impurity such as iron ion by coagulate wadding, sedimentary form is removed, guaranteed calcium source high purity like this, thereby laid a good foundation for preparing highly purified lime carbonate.
In order to obtain better impurity-eliminating effect, in the above-mentioned cleaner, the preferred ratio of mixture of calcium hydroxide and polyacrylic acid amide is 3-5: 1, more preferably 4: 1, so both guaranteed good impurity-eliminating effect, prevented again that residual polyacrylic acid amide from influencing the dispersiveness of calcium hydroxide particle.
In carbonization technique of the present invention, by actively imposing cooling measure (Physical temperature-lowering), its temperature of reaction is controlled at below 30 ℃ all the time.In addition, be provided with stirring in the carbonization reactor that the present invention adopts, but its bottom big area feeds carbon dioxide.After calcium hydroxide slurry pumps into this carbonization reactor, through violent stirring, and carry out big area, FR bubbling carbonizing by pure carbon dioxide, its calcium carbonate crystal particle growth is rapid, perfect; Observe under Electronic Speculum: its particle is spherical in shape, and granularity is little and size-grade distribution concentrated, and particle diameter is 40-100nm.
Therefore, the inventive method is compared with the production technique of traditional lime carbonate, not only saved the input of high-temperature calcination equipment in producing, but also significantly reduced energy loss and to the pollution of environment, also simplify, optimized production technique simultaneously, shortened the reaction times, finally made the calcium carbonate powder of preparation have good dispersity, purity height, active advantages of higher.
Description of drawings
Fig. 1 is the electromicroscopic photograph of the calcium carbonate powder of the inventive method preparation;
Fig. 2 is the electromicroscopic photograph of the calcium carbonate powder of the inventive method preparation;
Fig. 3 is the electromicroscopic photograph of the calcium carbonate powder of Comparative Examples preparation.
Embodiment
Below by embodiment, and in conjunction with the accompanying drawings, technical scheme of the present invention is described in further detail.
Embodiment 1: solvent temperature is 90 ℃, under the condition of continuously stirring, calcium chloride is dissolved in the deionized water, the cleaner that in solution, adds calcium chloride weight 3% simultaneously, this cleaner is calcium hydroxide and the polyacrylic acid amide mixture by 4: 1 mixed, filter out impurities then, add water and be mixed with the 0.4mol/L calcium chloride solution; Dissolution of sodium hydroxide in deionized water, is mixed with the 5.0mol/L sodium hydroxide solution, reduces to room temperature then, under the condition of continuously stirring, allow it slowly flow in the calcium chloride solution and react, and control reaction temperature is 30 ℃, obtain calcium hydroxide slurry; Above-mentioned calcium hydroxide slurry is pumped in the carbonization reactor, feed pure carbon dioxide and carry out carbonization, and control reaction temperature is no more than 30 ℃, detection reaction liquid pH value, when being 7, the reaction solution pH value is its carburizing reagent terminal point, to obtain calcium carbonate serosity and put into pressure filter and wash, when washing to washing electrical conductivity of water less than 50us/cm
2The time, press filtration obtains calcium carbonate filter cake, then puts it into baking oven, and temperature is controlled at 110 ℃ and dries, and oven dry to its moisture content was pulverized less than 0.1% o'clock, crossed 20 mesh sieves, promptly obtained high-purity spherical nano-calcium carbonate.
Show that under 10000 times of Electronic Speculum its morphology microstructure is the class ball-type, particle diameter is between 70-100nm, and good dispersity, does not have agglomeration, and the stereoscan photograph of this powder as shown in Figure 1.
Embodiment 2: solvent temperature is 95 ℃, under the condition of continuously stirring, calcium chloride is dissolved in the deionized water, the cleaner that in solution, adds calcium chloride weight 4% simultaneously, this cleaner is calcium hydroxide and the polyacrylic acid amide mixture by 5: 1 mixed, filter out impurities then, add water and be mixed with the 0.2mol/L calcium chloride solution; Dissolution of sodium hydroxide in deionized water, is mixed with the 3.5mol/L sodium hydroxide solution, reduces to room temperature then, under the condition of continuously stirring, allow it slowly flow in the calcium chloride solution and react, and control reaction temperature is 25 ℃, obtain calcium hydroxide slurry; Above-mentioned calcium hydroxide slurry is pumped in the carbonization reactor, feed pure carbon dioxide and carry out carbonization, and control reaction temperature is 25 ℃, detection reaction liquid pH value, when being 7, the reaction solution pH value is its carburizing reagent terminal point, to obtain calcium carbonate serosity and put into pressure filter and wash, when washing to washing electrical conductivity of water less than 50us/cm
2The time, press filtration obtains calcium carbonate filter cake, then puts it into baking oven, and temperature is controlled at 120 ℃ and dries, and oven dry to its moisture content was pulverized less than 0.1% o'clock, crossed 20 mesh sieves, promptly obtained high-purity spherical nano-calcium carbonate.
Show that under 10000 times of Electronic Speculum its morphology microstructure is the class ball-type, particle diameter is between 60-90nm, and good dispersity, does not have agglomeration, and the stereoscan photograph of this powder as shown in Figure 2.
Embodiment 3: solvent temperature is 100 ℃, under the condition of continuously stirring, calcium chloride is dissolved in the deionized water, the cleaner that in solution, adds calcium chloride weight 5% simultaneously, this cleaner be calcium hydroxide and polyacrylic acid amide by the mixture of 3: 1 mixed, add water and be mixed with the 0.3mol/L calcium chloride solution; Dissolution of sodium hydroxide in deionized water, is mixed with the 2.5mol/L sodium hydroxide solution, reduces to room temperature then, under the condition of continuously stirring, allow it slowly flow in the calcium chloride solution and react, and control reaction temperature is 20 ℃, obtain calcium hydroxide slurry; Above-mentioned calcium hydroxide slurry is pumped in the carbonization reactor, feed pure carbon dioxide and carry out carbonization, and control reaction temperature is 20 ℃, detection reaction liquid pH value, when being 7.5, the reaction solution pH value is its carburizing reagent terminal point, to obtain calcium carbonate serosity and put into pressure filter and wash, when washing to washing electrical conductivity of water less than 50us/cm
2The time, press filtration obtains calcium carbonate filter cake, then puts it into baking oven, and temperature is controlled at 115 ℃ and dries, and oven dry is to its moisture content
Show that under 10000 times of Electronic Speculum its morphology microstructure is the class ball-type, particle diameter is between 40-70nm, and good dispersity, does not have agglomeration, and the stereoscan photograph of this powder as shown in Figure 2.
Comparative Examples: 1 part of calcium oxide is dissolved in 10 parts of 80 ℃ of deionized waters, obtain calcium hydroxide slurry, calcium hydroxide slurry is pumped in the carbonization reactor, feeding volumetric concentration is that 40% carbonic acid gas carries out carbonization, and control reaction temperature is 40 ℃, and detection reaction liquid pH value is its carburizing reagent terminal point when the reaction solution pH value is 7, to obtain calcium carbonate serosity and put into pressure filter and wash, when washing to washing electrical conductivity of water less than 50us/cm
2The time, press filtration obtains calcium carbonate filter cake, then dry at 105 ℃, oven dry to its moisture content less than 0.1%, pulverize then, cross 20 mesh sieves, obtain square lime carbonate.
Show that under 10000 times of Electronic Speculum its morphology microstructure is imperfect, particle diameter is big and size-grade distribution is wide, and the stereoscan photograph of this powder as shown in Figure 3.
Claims (3)
1. the preparation method of a high-purity spherical nano-calcium carbonate is characterized in that said method comprising the steps of:
A. solvent temperature is 90-100 ℃, under the condition of continuously stirring, calcium chloride is dissolved in the deionized water, adds the cleaner of calcium chloride weight 3-5% simultaneously, filters out impurities then, and adding water, to be mixed with 0.2-0.4mol/L calcium chloride solution standby;
B. with dissolution of sodium hydroxide in deionized water, be mixed with 3.5-5.0mol/L sodium hydroxide solution, treat that then it reduces to room temperature, under the condition of continuously stirring, it is slowly flow in the calcium chloride solution react, and control reaction temperature is no more than 30 ℃, obtain calcium hydroxide slurry;
C. above-mentioned calcium hydroxide slurry is pumped in the carbonization reactor, feeding flow then is 3.0-5.0m
3/ h pure carbon dioxide carries out carbonization, and control reaction temperature is no more than 30 ℃, and detection reaction liquid pH value is its carburizing reagent terminal point when reacting liquid pH value is 7-7.5, obtain calcium carbonate serosity then;
D. calcium carbonate serosity is put into pressure filter and wash, when washing to washing electrical conductivity of water less than 50us/cm
2The time, press filtration obtains calcium carbonate filter cake, puts it into baking oven then in 110-120 ℃ of constant temperature dryings, when oven dry to its moisture content less than 0.1% the time, take out and pulverize, cross 20 mesh sieves, promptly obtain high-purity spherical nano-calcium carbonate.
2. the preparation method of high-purity spherical nano-calcium carbonate according to claim 1 is characterized in that in steps A, and described cleaner is the mixture of calcium hydroxide and polyacrylic acid amide, and its ratio of mixture is 3-5:1.
3. the preparation method of high-purity spherical nano-calcium carbonate according to claim 2 is characterized in that the ratio of mixture in described calcium hydroxide and polyacrylic acid amide is 4:1.
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| NO328264B1 (en) * | 2008-01-30 | 2010-01-18 | Elkem Solar As | Process for the preparation of calcium compounds |
| CN101508455B (en) * | 2009-03-20 | 2013-11-13 | 仙桃市中星电子材料有限公司 | Process for producing high-purity electronic grade strontium carbonate |
| CN101591033B (en) * | 2009-06-30 | 2012-10-03 | 广东风华高新科技股份有限公司 | Method for preparing calcium carbonate powder |
| CN102730734B (en) * | 2012-06-18 | 2015-05-20 | 佛山市松宝电子功能材料有限公司 | Purification method for calcium carbonate |
| CN103539187B (en) * | 2013-10-22 | 2015-07-08 | 山东大学 | An Indirect Process for Preparation of Light Calcium Carbonate Based on Medium Strengthening |
| CN104909398A (en) * | 2014-07-04 | 2015-09-16 | 池州市富华粉体科技有限公司 | Preparation method for high purity calcium carbonate |
| CN105288637B (en) * | 2015-11-23 | 2018-05-08 | 上海应用技术学院 | A kind of preparation method of calcium carbonate microspheres |
| CN106745214A (en) * | 2017-03-12 | 2017-05-31 | 佛山市松宝电子功能材料有限公司 | A kind of production method of the high-purity calcium titanate of superfine electron-level |
| CN107963649A (en) * | 2017-12-08 | 2018-04-27 | 安徽新涛新材料科技股份有限公司 | A kind of preparation method of super-fine active calcium carbide |
| CN111439769A (en) * | 2020-04-28 | 2020-07-24 | 广西夏阳环保科技有限公司 | Preparation method of high-purity and high-activity nano calcium oxide |
| CN114314629B (en) * | 2021-12-16 | 2022-09-30 | 浙江大学 | Preparation method of nano calcium carbonate based on surface potential control |
| CN115140755B (en) * | 2022-07-14 | 2023-11-10 | 桂林卓瑞食品原料有限公司 | Preparation method of porous calcium carbonate |
| CN116375072B (en) * | 2023-04-11 | 2024-02-27 | 重庆碳福森环保科技有限公司 | Method for producing modified calcium carbonate by aid method |
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| 汉白玉废料制备球形纳米碳酸钙的研究. 康明等.材料导报，第20卷第Ⅵ期. 2006 |
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