CN104229849A - Method for preparing nano calcium carbonate - Google Patents
Method for preparing nano calcium carbonate Download PDFInfo
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- CN104229849A CN104229849A CN201310252801.2A CN201310252801A CN104229849A CN 104229849 A CN104229849 A CN 104229849A CN 201310252801 A CN201310252801 A CN 201310252801A CN 104229849 A CN104229849 A CN 104229849A
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- Prior art keywords
- calcium carbonate
- reaction tower
- nano
- carbonation reaction
- pressure
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 85
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 63
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 23
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 239000002002 slurry Substances 0.000 claims abstract description 13
- 238000005255 carburizing Methods 0.000 claims description 10
- 239000003153 chemical reaction reagent Substances 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 8
- 238000007670 refining Methods 0.000 claims description 5
- 238000000889 atomisation Methods 0.000 claims description 4
- 238000010276 construction Methods 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 18
- 238000003763 carbonization Methods 0.000 abstract description 7
- 238000005507 spraying Methods 0.000 abstract description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 abstract 3
- 239000000047 product Substances 0.000 description 16
- 238000005516 engineering process Methods 0.000 description 5
- 235000011089 carbon dioxide Nutrition 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000005587 bubbling Effects 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a method for preparing nano calcium carbonate. The method comprises the following steps: introducing carbon dioxide gas into a carbonization reaction tower; spraying an atomized calcium hydroxide solution into the carbonization reaction tower by virtue of a fine slurry pump to ensure that the calcium hydroxide solution performs carbonization reaction with the carbon dioxide gas so as to generate calcium carbonate turbid liquid boiled slurry; and keeping the pressure of the carbonization reaction tower by introducing the calcium carbonate turbid liquid boiled slurry into a boiled slurry tank, controlling the quantity of the carbon dioxide gas introduced into the carbonization reaction tower, and controlling the quantity of the sprayed calcium hydroxide solution. By adopting the method for preparing nano calcium carbonate provided by the invention, nano calcium carbonate of types such as cube type, chain type and delta type in a particle size range of 10-100nm can be prepared. Moreover, production equipment is simple in structure and easy to maintain, the production cost is relatively low and the yield is relatively high; therefore, the method can be economically and massively used in the industry.
Description
Technical field
The present invention relates to chemical technology field, particularly relate to a kind of method preparing nano-calcium carbonate.
Background technology
Calcium carbonate is a kind of important inorganic chemical product, is widely used in the industries such as coating, rubber, plastics, tackiness agent, seal gum, medicine, food.Nano-calcium carbonate is a kind of Novel super-thin solid powder material grown up the eighties in 20th century, and its granularity is between 10nm-100nm.Due to the super-refinement of Nano particles of calcium carbonate, its crystalline structure and Electronic Structure change, and create quantum size effect, small-size effect, surface effects and macroscopic quantum effect that ordinary calcium carbonate does not have.
When nano-calcium carbonate adds in some product, there is significant strengthening action, the mechanical properties such as rheological, thixotropy, flow, levelling property and toughness prepared by product can be improved to some extent, thus there is higher added value.
Along with the development of nanometer grade calcium carbonate technology and the universal of universal technology, market is further vigorous to the demand of nanometer grade calcium carbonate, and the output of nanometer grade calcium carbonate also improves constantly.At present, the industrialized producing technology of nano-calcium carbonate mainly contains: interval bubbling carbonation method, continuously spraying multistage carborization and high-gravity reactive precipitation.
Wherein, the investment of interval bubbling carbonation method is relatively less and easy and simple to handle, and its process parameter control is workable, but its requirement of putting into concentration and pressure to unstripped gas carbonic acid gas is high.Once carbonic acid gas puts into concentration and pressure does not reach requirement, the absorption mass transfer effect of carbon dioxide will be made to be deteriorated, and the corresponding product cut size that makes is difficult to refinement.The utilization ratio of its carbonic acid gas is low simultaneously, and its general utilization is still less than 30%.
Compared with interval bubbling carbonation method, the production efficiency of continuous spraying multistage carborization is relatively high, and the utilization ratio of its carbonic acid gas can be increased to about 50%, but the operability of its stably manufactured is relatively poor, the particle size distribution range of product is wider, and the application characteristic of product is generally relatively low.
The advantages such as the product median size of high-gravity reactive precipitation is little, has narrow diameter distribution, and the relatively stable and carbonization time of quality product is relatively short.But its investment of production is comparatively large, and power consumption in producing is high, thus causes production cost higher, there is no method large-scale application at present.
Therefore, how to reduce the manufacturing cost of nano-calcium carbonate, improve nano-calcium carbonate production efficiency and just become problem demanding prompt solution.
Summary of the invention
The invention provides a kind of method preparing nano-calcium carbonate.
The invention provides a kind of method preparing nano-calcium carbonate, comprise the following steps:
Carbon dioxide is passed in carbonation reaction tower;
In described carbonation reaction tower, sprayed into the aqua calcis of atomization by refining pump, make described aqua calcis and described carbon dioxide generation carburizing reagent, to generate the ripe slurry of calcium carbonate suspension liquid;
By ripe for described calcium carbonate suspension liquid slurry is imported ripe stock tank, and control passes into the carbon dioxide gas scale of construction in described carbonation reaction tower and sprays into described aqua calcis amount to keep the pressure of described carbonation reaction tower.
The pressure of described carbonation reaction tower is greater than 0.08Mpa, and the concentration of described aqua calcis is greater than 80kg/m
3.
The pressure of described carbonation reaction tower is greater than 0.2Mpa, and temperature of reaction is less than 38 DEG C, and the particle diameter of obtained nano-calcium carbonate is less than 100nm.
The pressure of described carbonation reaction tower is greater than 0.05Mpa, and temperature of reaction is less than 28 DEG C, and the particle diameter of obtained nano-calcium carbonate is less than 100nm.
The pressure of described carbonation reaction tower is greater than 0.3Mpa, and temperature of reaction is less than 25 DEG C, and the particle diameter of obtained nano-calcium carbonate is 50nm to 100nm.
The product type of described nano-calcium carbonate comprises: cubes, chain and Chinese character pin-shaped.
The method preparing nano-calcium carbonate of the present invention can prepare the cubes of 10nm-100nm scope, chain, the product type nano-calcium carbonate such as Chinese character pin-shaped.And production unit structure is simple, be easy to safeguard, production cost is relatively low, and output is higher, industrially large-scale application that can be economic.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the production unit schematic diagram that the present invention prepares the embodiment of the method for nano-calcium carbonate.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly, below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Fig. 1 is the production unit schematic diagram that the present invention prepares the embodiment of the method for nano-calcium carbonate, and as shown in Figure 1, the method preparing nano-calcium carbonate of the present embodiment can comprise:
In carbonation reaction tower, 1 passes into carbon dioxide.
Particularly, first confirm that variable valve 9 is closing condition, then in carbonation reaction tower 1, carbon dioxide is passed into by dashpot 5, passing in process, need the pressure being monitored reaction tower 1 by tensimeter 8, until the pressure of carbon dioxide reaches the optimum pressure state that carburizing reagent occurs in carbonation reaction tower 1.
In carbonation reaction tower 1, sprayed into the aqua calcis of atomization by refining pump 7, make aqua calcis and carbon dioxide generation carburizing reagent, to generate the ripe slurry of calcium carbonate suspension liquid.
After in carbonation reaction tower 1, the pressure of carbon dioxide reaches the optimum pressure state that carburizing reagent occurs, by refining pump 7, aqua calcis is extracted out from refining groove 6, then pass into carbonation reaction tower 1 by pipeline and nozzle 2 and after atomization, aerial, the tower wall and liquid distributing board 3 of carbonation reaction tower 1 carry out carburizing reagent (Ca(OH) with carbon dioxide
2+ CO
2=CaCO
3+ H
2thus generate calcium carbonate suspension liquid ripe slurry O).
By ripe for calcium carbonate suspension liquid slurry is imported ripe stock tank 4, and control passes into the carbon dioxide gas scale of construction in carbonation reaction tower 1 and sprays into aqua calcis amount to keep the pressure of carbonation reaction tower 1.
By observing liquid height in carbonation reaction tower 1 tower from liquidometer 10, thus the situation of the carburizing reagent carried out in monitoring carbonation reaction tower 1, after in carbonation reaction tower 1 tower, liquid reaches the height of production requirement, variable valve 9 can be opened, the ripe slurry of calcium carbonate suspension liquid produced is imported in ripe stock tank 4.In importing process, the speed to unlatching size and the carbon dioxide of variable valve 9 pass into is needed to control, to guarantee that the pressure of carbonation reaction tower 1 maintains the size required by carburizing reagent, thus carburizing reagent can be stablized go on always, thus realize uninterrupted production.
In carbonation reaction, the absorption mass transfer process due to carbon dioxide is the committed step of whole carbonization process.Therefore strengthening carbon dioxide rate of mass transfer is in the liquid phase the effective way improving whole process rate.Simultaneously due to the CO in liquid phase
3 2-generated by the chemical absorption of carbon dioxide, the uptake rate of the carbon dioxide therefore controlled also is one of effective means of calcium carbonate degree of supersaturation height in the hierarchy of control, drastically increased the solubleness of carbon dioxide by the pressure controlling carbonation reaction tower 1, thus considerably improve the degree of supersaturation of reaction system.
The method preparing nano-calcium carbonate of the present embodiment can prepare the cubes of 10nm-100nm scope, chain, the product type nano-calcium carbonate such as Chinese character pin-shaped.And production unit structure is simple, be easy to safeguard, production cost is relatively low, and output is higher, industrially large-scale application that can be economic.
Preferably, the pressure of carbonation reaction tower 1 is greater than 0.08Mpa, and the concentration of aqua calcis is greater than 80kg/m
3.Show by experiment, be greater than 0.08Mpa at the pressure of carbonation reaction tower 1, the concentration of aqua calcis is greater than 80kg/m
3time, general production requirement can be met, and after the pressure of carbonation reaction tower 1 improves, the concentration of aqua calcis also correspondingly can improve.
Preferably, the pressure of carbonation reaction tower is greater than 0.2Mpa, and temperature of reaction is less than 38 DEG C, and the particle diameter of obtained nano-calcium carbonate is less than 100nm.When the particle diameter of required nano-calcium carbonate is less than 100nm, the pressure of carbonation reaction tower 1 needs to be greater than 0.2Mpa, and temperature of reaction should be less than 38 DEG C, if temperature of reaction is too high, nano-calcium carbonate particulate can be caused to reunite under severe thermal motion, thus reduce the quality of product.If the pressure of suitable raising carbonation reaction tower 1, temperature of reaction also can suitably raise, but when process temperature is more than 45 DEG C, needs to select to add suitable dispersion agent, to guarantee that nano-calcium carbonate particulate can not be reunited under severe thermal motion.
Preferably, the pressure of carbonation reaction tower 1 is greater than 0.05Mpa, and temperature of reaction is less than 28 DEG C, and the particle diameter of obtained nano-calcium carbonate is 100nm.Temperature of reaction is down to less than 28 DEG C, when the pressure of carbonation reaction tower 1 is greater than 0.05Mpa, carburizing reagent also can normally be carried out, and can obtain the nano-calcium carbonate calcium product that particle diameter is less than 100nm equally.
Preferably, the pressure of carbonation reaction tower 1 is greater than 0.3Mpa, and temperature of reaction is less than 25 DEG C, and the particle diameter of obtained nano-calcium carbonate is 50nm to 100nm.When the particle diameter of the nano-calcium carbonate prepared is 50nm to 100nm, the pressure of carbonation reaction tower 1 needs to be greater than 0.3Mpa, and temperature of reaction controls within 25 DEG C, just can obtain the nano-calcium carbonate calcium product that particle diameter is 50nm to 100nm.
Further preferred, the product type of nano-calcium carbonate can comprise: cubes, chain and Chinese character pin-shaped.The cubes of 10nm-100nm scope, chain, the product type nano-calcium carbonate such as Chinese character pin-shaped can be prepared by adjusting the tower internal pressure of carbonation reaction tower 1, slurry temperature or suitably adding additive.
The method preparing nano-calcium carbonate of the present invention can prepare the cubes of 10nm-100nm scope, chain, the product type nano-calcium carbonate such as Chinese character pin-shaped.And production unit structure is simple, be easy to safeguard, production cost is relatively low, and output is higher, industrially large-scale application that can be economic.
Last it is noted that above embodiment is only in order to illustrate technical scheme of the present invention, be not intended to limit; Although with reference to previous embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that: it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (6)
1. prepare a method for nano-calcium carbonate, it is characterized in that, comprise the following steps:
Carbon dioxide is passed in carbonation reaction tower;
In described carbonation reaction tower, sprayed into the aqua calcis of atomization by refining pump, make described aqua calcis and described carbon dioxide generation carburizing reagent, to generate the ripe slurry of calcium carbonate suspension liquid;
By ripe for described calcium carbonate suspension liquid slurry is imported ripe stock tank, and control passes into the carbon dioxide gas scale of construction in described carbonation reaction tower and sprays into described aqua calcis amount to keep the pressure of described carbonation reaction tower.
2. the method preparing nano-calcium carbonate according to claim 1, is characterized in that, the pressure of described carbonation reaction tower is greater than 0.08Mpa, and the concentration of described aqua calcis is greater than 80kg/m
3.
3. the method preparing nano-calcium carbonate according to claim 1, is characterized in that, the pressure of described carbonation reaction tower is greater than 0.2Mpa, and temperature of reaction is less than 38 DEG C, and the particle diameter of obtained nano-calcium carbonate is less than 100nm.
4. the method preparing nano-calcium carbonate according to claim 1, is characterized in that, the pressure of described carbonation reaction tower is greater than 0.05Mpa, and temperature of reaction is less than 28 DEG C, and the particle diameter of obtained nano-calcium carbonate is less than 100nm.
5. the method preparing nano-calcium carbonate according to claim 1, is characterized in that, the pressure of described carbonation reaction tower is greater than 0.3Mpa, and temperature of reaction is less than 25 DEG C, and the particle diameter of obtained nano-calcium carbonate is 50nm to 100nm.
6. the method preparing nano-calcium carbonate according to claim arbitrary in claim 1 to 5, is characterized in that, the product type of described nano-calcium carbonate comprises: cubes, chain and Chinese character pin-shaped.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201310252801.2A CN104229849A (en) | 2013-06-24 | 2013-06-24 | Method for preparing nano calcium carbonate |
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| CN201310252801.2A CN104229849A (en) | 2013-06-24 | 2013-06-24 | Method for preparing nano calcium carbonate |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104826552A (en) * | 2015-05-29 | 2015-08-12 | 厦门大学 | Pressurized carbonation reaction device and method |
| CN107601542A (en) * | 2017-09-30 | 2018-01-19 | 广西华洋矿源材料有限公司 | A kind of preparation method of nano-calcium carbonate |
| CN107673379A (en) * | 2017-11-20 | 2018-02-09 | 绵阳市远达新材料有限公司 | The preparation method of high purity magnesium carbonate |
| CN109911924A (en) * | 2017-12-13 | 2019-06-21 | 财团法人工业技术研究院 | Preparation method of calcium carbonate particles |
| CN110240188A (en) * | 2019-07-19 | 2019-09-17 | 良德纳米粉体创新科技(安徽)有限公司 | A kind of processing method of nanometer calcium carbonate |
| CN111013521A (en) * | 2019-12-25 | 2020-04-17 | 广西华纳新材料科技有限公司 | Nano calcium carbonate pressurized carbonation and surface modification integrated reaction kettle and application |
| CN118125486A (en) * | 2024-03-05 | 2024-06-04 | 广州安赛化工有限公司 | Method and system for preparing nano calcium carbonate by self-vacuum liquid impact method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101027253A (en) * | 2004-07-13 | 2007-08-29 | Fp颜料有限公司 | Method and apparatus for producing calcium carbonate products, said products and their use |
| CN101172636A (en) * | 2007-10-16 | 2008-05-07 | 陈杰 | Method of producing nano-calcium carbonate |
-
2013
- 2013-06-24 CN CN201310252801.2A patent/CN104229849A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101027253A (en) * | 2004-07-13 | 2007-08-29 | Fp颜料有限公司 | Method and apparatus for producing calcium carbonate products, said products and their use |
| CN101172636A (en) * | 2007-10-16 | 2008-05-07 | 陈杰 | Method of producing nano-calcium carbonate |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104826552A (en) * | 2015-05-29 | 2015-08-12 | 厦门大学 | Pressurized carbonation reaction device and method |
| US10913040B2 (en) | 2015-05-29 | 2021-02-09 | Xiamen University | Pressurized carbonation reaction apparatus and its method |
| CN107601542A (en) * | 2017-09-30 | 2018-01-19 | 广西华洋矿源材料有限公司 | A kind of preparation method of nano-calcium carbonate |
| CN107673379A (en) * | 2017-11-20 | 2018-02-09 | 绵阳市远达新材料有限公司 | The preparation method of high purity magnesium carbonate |
| CN107673379B (en) * | 2017-11-20 | 2019-07-30 | 绵阳市远达新材料有限公司 | The preparation method of high purity magnesium carbonate |
| CN109911924A (en) * | 2017-12-13 | 2019-06-21 | 财团法人工业技术研究院 | Preparation method of calcium carbonate particles |
| CN109911924B (en) * | 2017-12-13 | 2021-10-01 | 财团法人工业技术研究院 | Process for preparing calcium carbonate particles |
| CN110240188A (en) * | 2019-07-19 | 2019-09-17 | 良德纳米粉体创新科技(安徽)有限公司 | A kind of processing method of nanometer calcium carbonate |
| CN111013521A (en) * | 2019-12-25 | 2020-04-17 | 广西华纳新材料科技有限公司 | Nano calcium carbonate pressurized carbonation and surface modification integrated reaction kettle and application |
| CN111013521B (en) * | 2019-12-25 | 2022-06-14 | 广西华纳新材料股份有限公司 | Nano calcium carbonate pressurized carbonation and surface modification integrated reaction kettle and application |
| CN118125486A (en) * | 2024-03-05 | 2024-06-04 | 广州安赛化工有限公司 | Method and system for preparing nano calcium carbonate by self-vacuum liquid impact method |
| CN118125486B (en) * | 2024-03-05 | 2024-08-16 | 广州安赛化工有限公司 | Method and system for preparing nano calcium carbonate by self-vacuum liquid impact method |
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Application publication date: 20141224 |