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CN103738993A - Carbonation reactor of energy-efficient nano calcium carbonate and preparation method of energy-efficient nano calcium carbonate - Google Patents

Carbonation reactor of energy-efficient nano calcium carbonate and preparation method of energy-efficient nano calcium carbonate Download PDF

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Publication number
CN103738993A
CN103738993A CN201310640325.1A CN201310640325A CN103738993A CN 103738993 A CN103738993 A CN 103738993A CN 201310640325 A CN201310640325 A CN 201310640325A CN 103738993 A CN103738993 A CN 103738993A
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calcium carbonate
carbonization
energy
slurry
preparation
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CN103738993B (en
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顾达
张和庆
朱士洲
邓丽丽
邵小保
史韦
陈宁
倪春慧
茅旭东
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Wuhu excellent nanometer new material Limited by Share Ltd
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WUHU ZHUOYUE NANO NEW MATERIAL Co Ltd
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Abstract

The invention relates to a preparation method of energy-efficient nano calcium carbonate, the main steps are as follows: in carbonization, first a compressed kiln gas is cooled to 25 DEG C by deep well water, during the carbonization process, carbonized slurry is directly cooled by the kiln gas, the cooling effect is increased, the heat produced in the slurry carbonization process can be absorbed directly, and the carbonized slurry temperature is effectively controlled. During the carbonization, the kiln gas enters into an interlayer of an outer barrel and an inner barrel from the periphery of an umbrella-shaped gas distributor to drive the slurry in the interlayer to move from bottom to up, under the action of a porous helical baffle plate, on the one hand, a gas liquid passes through multiple holes of the helical baffle plate to make larger bubbles smaller by division; on the other hand, under the action of the helical baffle plate, the upward gas liquid forms a vortex for enhancement of mixing effects. The upward slurry in the interlayer returns back to the bottom through the inner barrel to form a slurry cyclic carbonation process to facilitate kiln gas absorption and accelerate the carbonation process.

Description

A kind of carbonization reactor of energy-saving nano-calcium carbonate and preparation method
Technical field
The present invention relates to a kind of preparation method of energy-saving nano-calcium carbonate, specifically, relate to a kind of in the building-up process of nano-calcium carbonate, thereby by the temperature of cooling kiln gas, control the temperature of carbonization slurry, by porous helical baffle strengthening gas-liquid mixed, without the industrialized process for preparing with regard to energy synthesis of nano calcium carbonate to the cooling and mechanical stirring of carbonization slurry.
Technical background
Calcium carbonate is a kind of important inorganic chemical product, is one of inorganic fillings that current purposes is the widest, is widely used in the chemical fields such as rubber, plastics, papermaking, coating, ink.Along with developing rapidly of industry, all trades and professions are increasing to the demand of nano-calcium carbonate.And prior art while producing nano-calcium carbonate carbonization except adding chemical additives, key is under low temperature condition, by mechanical stirring, carry out carburizing reagent, most typical method is as patent of invention (patent No. ZL01.1.26405.5) " a kind of industrial production process of nm-class active calcium carbonate ".This method adopts intermittently bubbling stirring reactor, when adding chemical additives during carbonization, by the cooling carbonization slurry of chuck, and produces nano-calcium carbonate in churned mechanically situation.When this method is produced, energy consumption is large, and production cost is high, has restricted the increase of nano-calcium carbonate output and the expansion of Application Areas.The present invention, in the production process of nano-calcium carbonate, does not need freezing and mechanical stirring for reaction solution, and the energy consumption while reducing carbonization is produced cube, size distribution evenly and equally without the nano-calcium carbonate of agglomeration.The nano-calcium carbonate being synthesized by the method can be used as high-grade silicone adhesive or vehicle paint base filler after surface treatment.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method of energy-saving synthesis of nano calcium carbonate, and avoiding needs freezing and mechanical stirring, the drawback that energy consumption is large in the production process of current most of nano-calcium carbonate.
When concrete summary of the invention is carbonization, first the kiln gas after compression is cooled to below 25 ℃ with phreatic water.And conventional carbonization method is that the kiln gas after compression is directly carried out to carbonization, the temperature of this kiln gas is up to more than 60 ℃, and when carbonization, the heat of kiln gas is directly passed to carbonization slurry, has increased the energy consumption that carbonization slurry cools.And adopt the phreatic water kiln gas after cooled compressed, in carbonization process, the slurry of the direct cooling carbonization of kiln gas of low temperature, has increased cooling effect, effectively controls the temperature of carbonization slurry.
During carbonization, do not need mechanical stirring, under static state, still can reach good gas-liquid mixed effect.When kiln gas enters the interlayer of outer barrel and inner core from umbrella shape gas distributor surrounding, drive the slurry between interlayer to move from bottom to top, and under the effect of porous helical baffle, when gas-liquid is passed through the porous of helical baffle on the one hand, larger bubble is cut apart and diminished; The gas-liquid rising on the other hand, under the effect of helical baffle, forms vortex, enhancing mixed effect.The slurry rising between interlayer, is back to bottom by inner core again, forms the circulation carbonization process of slurry, the absorption of favourable kiln gas, accelerated carbonation process.
the invention has the advantages that:
In the production process of synthesis of nano calcium carbonate product, do not need cooling slurry and carry out mechanical stirring, the energy consumption while greatly having saved carbonization, reduces production costs, and is a kind of production method of energy-saving nano-calcium carbonate.
embodiment
Below in conjunction with Figure of description, technical scheme of the present invention is described, so that those skilled in the art understand.
The principle of the carbonization reactor that this is energy-saving and structure are as shown in the figure.
Fig. 1 is energy-saving carbonization reactor.
In figure: 1-carbonizer outer barrel; 2-water conservancy diversion inner core; 3-porous helical baffle; 4-umbrella shape gas distributor; 5-calcium hydroxide slurry opening for feed; 6-calcium carbonate slurry discharge port; 7-cooled kiln gas import; 8-tubular heater exchhanger; 9-deep-well entrance of cooling water; 10-cooling water outlet; The import of 11-kiln gas.
First the kiln gas after compression is cooled to below 25 ℃ with phreatic water, when this kiln gas enters the interlayer of outer barrel and inner core from umbrella shape gas distributor surrounding, drive the slurry between interlayer to move from bottom to top, and under the effect of porous helical baffle, larger bubble is cut apart to diminish, form vortex, enhancing mixed effect simultaneously.The slurry rising between interlayer, is back to bottom by inner core again, forms the circulation carbonization process of slurry, the absorption of favourable kiln gas, accelerated carbonation process.
Embodiment
In order to make technique means of the present invention, creation characteristic, reach object and effect is easy to understand, below in conjunction with embodiment, further set forth the present invention.
embodiment 1
As shown in Figure 1: 1.2 meters of shell of reactor diameters, high 5.0 meters, 0.6 meter of inner diameter of steel flue, high 4.0 meters, inside shell, helical baffle width is that 25cm, length are 20cm, has 4cm porous on helical baffle, and is up spaced installation with the pitch angle spiral of 45 °.
In the calcium hydroxide slurry injecting reactor that is 9.0% 4.5 cubic metres of mass concentrations, add 3.0 kilograms of chemical additives sucrose, the starting temperature of calcium hydroxide slurry is 25 ℃, adopt the roots blower that pressure is 78Kpa, to after kiln gas compression, with phreatic water, be cooled to below 25 ℃, enter again umbrella shape gas distributor, the flow of controlling kiln gas is 9 cubic metres of per minutes, in kiln gas, the volume content of carbonic acid gas is 26~30%, after carbonization 60 minutes, the temperature of slurry is upgraded to 33 ℃, and the pH value of material is down to 6.5~7.0, is the terminal of carbonization.By the synthetic calcium carbonate slurry of this reactor carbonization, recording particle diameter on transmission electron microscope is 100~150 nanometers, and size distribution is even, and good dispersity, without agglomeration.
embodiment 2
With the identical equipment of embodiment 1 and similar method, in the calcium hydroxide slurry injecting reactor that is 8.0% 4.5 cubic metres of mass concentrations, add 2.5 kilograms of chemical additives sucrose, the starting temperature of calcium hydroxide slurry is 24 ℃, to after kiln gas compression, with phreatic water, be cooled to below 24 ℃, enter again umbrella shape gas distributor, the flow of controlling kiln gas is 7 cubic metres of per minutes, in kiln gas, the volume content of carbonic acid gas is 26~30%, after carbonization 66 minutes, the temperature of slurry is upgraded to 31 ℃, and the pH value of material is down to 6.5~7.0, is the terminal of carbonization.By the synthetic calcium carbonate slurry of this reactor carbonization, recording particle diameter on transmission electron microscope is 80~130 nanometers, and size distribution is even, and good dispersity, without agglomeration.
embodiment 3
With the identical equipment of embodiment 1 and similar method, in the calcium hydroxide slurry injecting reactor that is 7.2% 4.5 cubic metres of mass concentrations, add 3.0 kilograms of chemical additives sucrose, the starting temperature of calcium hydroxide slurry is 24 ℃, to after kiln gas compression, with phreatic water, be cooled to below 23 ℃, enter again umbrella shape gas distributor, the flow of controlling kiln gas is 7 cubic metres of per minutes, in kiln gas, the volume content of carbonic acid gas is 26~30%, after carbonization 60 minutes, the temperature of slurry is upgraded to 30 ℃, and the pH value of material is down to 6.5~7.0, is the terminal of carbonization.By the synthetic calcium carbonate slurry of this reactor carbonization, recording particle diameter on transmission electron microscope is 70~100 nanometers, and size distribution is even, and good dispersity, without agglomeration.
  
More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements all fall in the scope of the invention of claims protection.

Claims (8)

1. the carbonization reactor of energy-saving nano-calcium carbonate and a preparation method, this reactor comprises the compositions such as carbonizer outer barrel, water conservancy diversion inner core, porous helical baffle, umbrella shape gas distributor, tubular heater exchhanger.
2. the carbonization reactor of a kind of energy-saving nano-calcium carbonate according to claim 1 and preparation method, is characterized in that: the diameter of described water conservancy diversion inner core is 2/5~3/5 of outer barrel diameter.
3. the carbonization reactor of a kind of energy-saving nano-calcium carbonate according to claim 1 and preparation method, it is characterized in that: described porous helical baffle width is the plate body that 20~25cm, length are 20~25cm, on plate washer, evenly have the aperture that diameter is 3.5~5.0cm, helical baffle is up spaced installation with the pitch angle spiral of 45 °.
4. the carbonization reactor of a kind of energy-saving nano-calcium carbonate according to claim 1 and preparation method, is characterized in that: the area of tubular heater exchhanger and the flow of phreatic water are enough to make the kiln gas temperature after compression to be down to below 25 ℃ from 60 ℃.
5. the carbonization reactor of an energy-saving nano-calcium carbonate and preparation method, it is characterized in that, the method comprises the steps:, in refining calcium hydroxide slurry, to add chemical additives sucrose, then cooled kiln gas is passed into and in reactor, carry out carbonization, the calcium carbonate of synthesis nano.
6. the carbonization reactor of a kind of energy-saving nano-calcium carbonate according to claim 5 and preparation method, is characterized in that: the concentration of calcium hydroxide slurry is 6.0~9.0%, and the starting temperature of calcium hydroxide slurry and the temperature of kiln gas are all lower than 25 ℃.
7. the carbonization reactor of a kind of energy-saving nano-calcium carbonate according to claim 5 and preparation method, is characterized in that: the amount that adds chemical additives sucrose before carbonization is 0.4~0.8% of calcium hydroxide weight.
8. the carbonization reactor of a kind of energy-saving nano-calcium carbonate according to claim 5 and preparation method, is characterized in that: the flow of controlling kiln gas during carbonization is 1.0~2.0 cubes ms/min of every cubic metre of calcium hydroxide slurry amount.
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104891545A (en) * 2015-05-25 2015-09-09 福建鸿丰纳米科技有限公司 Carbonization reaction device and method for nano calcium carbonate production
CN105271345A (en) * 2015-10-19 2016-01-27 上海南卓新材料科技有限公司 Preparation method of special functional filling superfine activated calcium carbonate for hard PVC (polyvinyl chloride)
CN106241851A (en) * 2016-07-26 2016-12-21 四川高绿平环境科技有限公司 A kind of processing method of useless phosphoric acid,diluted
CN106552560A (en) * 2016-10-28 2017-04-05 江南大学 A kind of airlift reactor with spiral porous sieve plate
CN108101091A (en) * 2017-12-30 2018-06-01 石家庄市红星钙业有限公司 A kind of method and apparatus of dynamic carbonizatin method production calcium carbonate
CN110893333A (en) * 2019-12-19 2020-03-20 靖江神驹容器制造有限公司 O-chlorobenzonitrile fluidized bed reactor
CN112831397A (en) * 2021-02-22 2021-05-25 西安交通大学 Column type photobioreactor with built-in turbulence component and microalgae culture method
CN115178212A (en) * 2022-07-08 2022-10-14 安徽皖江纳米科技有限公司 Carbonization reaction device for producing energy-saving superfine calcium carbonate and working method thereof

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CN101863503A (en) * 2010-06-22 2010-10-20 恩平市燕华化工实业有限公司 Preparation method of nanometer calcium carbonate applied to top-grade silicone adhesive
CN102491398A (en) * 2011-12-20 2012-06-13 广西华纳新材料科技有限公司 Gas stripping precipitated calcium carbonate carbonation reactor
CN202594800U (en) * 2012-04-17 2012-12-12 池州凯尔特纳米科技有限公司 Ultrafine calcium carbonate carbonizing reactor capable of enhancing gas and liquid mixing
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

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Publication number Priority date Publication date Assignee Title
CN101863503A (en) * 2010-06-22 2010-10-20 恩平市燕华化工实业有限公司 Preparation method of nanometer calcium carbonate applied to top-grade silicone adhesive
CN102491398A (en) * 2011-12-20 2012-06-13 广西华纳新材料科技有限公司 Gas stripping precipitated calcium carbonate carbonation reactor
CN202594800U (en) * 2012-04-17 2012-12-12 池州凯尔特纳米科技有限公司 Ultrafine calcium carbonate carbonizing reactor capable of enhancing gas and liquid mixing
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

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104891545A (en) * 2015-05-25 2015-09-09 福建鸿丰纳米科技有限公司 Carbonization reaction device and method for nano calcium carbonate production
CN105271345A (en) * 2015-10-19 2016-01-27 上海南卓新材料科技有限公司 Preparation method of special functional filling superfine activated calcium carbonate for hard PVC (polyvinyl chloride)
CN106241851A (en) * 2016-07-26 2016-12-21 四川高绿平环境科技有限公司 A kind of processing method of useless phosphoric acid,diluted
CN106241851B (en) * 2016-07-26 2018-01-05 四川高绿平环境科技有限公司 A kind of processing method of useless phosphoric acid,diluted
CN106552560A (en) * 2016-10-28 2017-04-05 江南大学 A kind of airlift reactor with spiral porous sieve plate
CN106552560B (en) * 2016-10-28 2019-10-22 江南大学 A kind of airlift reactor with spiral porous sieve plate
CN108101091A (en) * 2017-12-30 2018-06-01 石家庄市红星钙业有限公司 A kind of method and apparatus of dynamic carbonizatin method production calcium carbonate
CN110893333A (en) * 2019-12-19 2020-03-20 靖江神驹容器制造有限公司 O-chlorobenzonitrile fluidized bed reactor
CN110893333B (en) * 2019-12-19 2021-11-12 靖江神驹容器制造有限公司 O-chlorobenzonitrile fluidized bed reactor
CN112831397A (en) * 2021-02-22 2021-05-25 西安交通大学 Column type photobioreactor with built-in turbulence component and microalgae culture method
CN112831397B (en) * 2021-02-22 2022-10-25 西安交通大学 Column type photobioreactor with built-in turbulence component and microalgae culture method
CN115178212A (en) * 2022-07-08 2022-10-14 安徽皖江纳米科技有限公司 Carbonization reaction device for producing energy-saving superfine calcium carbonate and working method thereof

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Address after: 241201 Anhui city of Wuhu province Fanchang County Digang town of new building materials Industrial Park

Patentee after: Wuhu excellent nanometer new material Limited by Share Ltd

Address before: 241201 Anhui city of Wuhu province Fanchang County Digang town of new building materials Industrial Park

Patentee before: WUHU ZHUOYUE NANO NEW MATERIAL CO., LTD.