CN113797874B - Device for preparing precipitated calcium carbonate by adopting supercritical carbon dioxide - Google Patents
Device for preparing precipitated calcium carbonate by adopting supercritical carbon dioxide Download PDFInfo
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Abstract
The invention discloses a device for preparing precipitated calcium carbonate by adopting supercritical carbon dioxide, which comprises a fine pulp inlet and supercritical CO 2 An input spray pipe, a carbonization reactor, a positive and negative paddle turbine combination, a crystal form control agent inlet, a Laval nozzle, a central shaft and supercritical CO 2 The input spray pipe is arranged on the fine pulp inlet, the fine pulp inlet is arranged at the inlet of the carbonization reactor, the fine pulp inlet is a flared pipe which is gradually reduced, the inlet of the carbonization reactor is a small opening of a horn, and the outlet of the carbonization reactor is connected with a Laval nozzle. The carbonization reactor is a sealed tank body which is gradually increased from a feeding port to a discharging end and then gradually reduced, a crystal form control agent inlet is arranged at the upper part of the front end of the carbonization reactor, and a positive and negative paddle turbine is combined and arranged in the carbonization reactor and is arranged on a central shaft. The device has controllable carbonization process, length-diameter ratio and crystal form, and the finished product has uniform granularity and narrow distribution, and can be used for generating various crystal forms of calcium carbonate in different fields.
Description
Technical Field
The invention belongs to the field of production of light and nano calcium carbonate, and particularly relates to a device for preparing precipitated calcium carbonate by using supercritical carbon dioxide.
Background
PCC (Precipitated Calcium Carbonate) is an abbreviation for Precipitated Calcium Carbonate, a common inorganic compound, of limestone rock (limestone for short)The main component of which has the molecular formula of CaCO 3 And the relative molecular weight is 100.09. Calcium carbonate is classified into light calcium carbonate, heavy calcium carbonate and activated calcium carbonate according to different production methods.
1. Precipitated calcium carbonate (abbreviated as light calcium carbonate). Calcining limestone and other raw materials to generate lime and carbon dioxide, and then adding water to digest the lime to generate lime milk (the main component is calcium hydroxide); then introducing carbon dioxide, carbonizing the lime milk, and generating calcium carbonate precipitate; dehydrating, drying and pulverizing.
2. Ground calcium carbonate (called triple superphosphate for short) is prepared by directly crushing natural limestone, calcite, chalk, shells and the like by using a mechanical method. Heavy calcium carbonate is called heavy calcium carbonate because its precipitation volume is smaller than that of light calcium carbonate.
3. The active calcium carbonate, modified calcium carbonate, surface treated calcium carbonate, colloidal calcium carbonate or (called active calcium for short) is prepared by surface modifying light calcium carbonate or heavy calcium carbonate with a surface modifier. Since calcium carbonate modified with a surface modifier generally has various functions of enhancing related properties, modified calcium carbonate is conventionally called activated calcium carbonate.
In 1909, nireni Baishidian invented the use of lime milk and CO in kiln gas produced by lime kiln 2 The process for producing precipitated calcium carbonate by reaction is called carbonization. The nano calcium and light calcium powder obtained by the method has the main characteristics that: the particle size is small, and the average particle size is in the micron order; the particle size distribution specificity is high, and the powder can be regarded as monodisperse powder; the crystal form of the powder is diversified. In the carbonization process, different crystal form directing agents or surfactants can be added according to different requirements to obtain the light calcium carbonate with different types and particle sizes.
One of the most critical processes in the PCC production process for product quality is the carbonization process. The carbonization process is a key control operation that determines the shape and size of the PCC crystals. According to the difference of carbonization process, its production technology roughly has following four kinds: low-temperature intermittent bubbling carbonization method, continuous spray carbonization method, stirred tank carbonization method anda high gravity reaction column method, etc. The PCC produced by the carbonization process is not ideal in dispersibility and stability, and the reasons are the carbonization process and CO 2 The utilization rate of (a) is related to the gap of equipment technology control operations, and particularly the difference between batch qualities is obvious.
The carbonization method involves the following chemical reaction formula:
lime baking:
digestion reaction (also called ashing reaction): caO + H 2 O→Ca(OH) 2 +Q 2
And (3) carbonization reaction: ca (OH) 2 +CO 2 →CaCO 3 ↓+Q 3
Overcarbonization reaction (also referred to as saturated carbonization reaction):
CaCO 3 +H 2 O+CO 2 →Ca(HCO 3 ) 2
as the temperature and pressure of the environment change, any one substance exists in three phases: gas phase, liquid phase, solid phase. The point where three phases coexist in an equilibrium state is called a three-phase point. The point at which the interface between the liquid and gas phases disappears is called the supercritical point. The temperature and pressure at the critical point are called critical temperature and critical pressure, and the pressure and temperature at the critical point are different for different substances. Supercritical fluid (SCF) refers to a fluid having a temperature and pressure above its Critical point. Carbon dioxide has a property that changes at a temperature higher than the critical temperature Tc =31.26 ℃ and a pressure higher than the critical pressure Pc =72.9 atm. It has a density close to that of liquid, a viscosity close to that of gas, and a diffusion coefficient 100 times that of liquid, and thus has a surprising dissolving power. Thus using supercritical CO 2 The calcium hydroxide is subjected to carbonization reaction, and the PCC powder with finer granularity, narrower granularity distribution range, good crystal form consistency and stronger comprehensive performance can be prepared.
The laval nozzle is widely applied to tail nozzles of hypersonic speed aircrafts, hypersonic speed aircrafts and rockets. The Laval nozzle is an important component of an aircraft engine thrust chamber. The front half part of the nozzle is contracted from big to small to a narrow throat from the middle. The narrow throat is expanded from small to large to the arrow bottom. The gas in the rocket body flows into the front half part of the nozzle under high pressure, passes through the narrow throat and escapes from the rear half part. At this stage, the fluid movement follows the principle of "when the fluid moves in the pipe, the flow velocity is high at the small section and the flow velocity is low at the large section", so the fluid is accelerated continuously. When the narrow throat is reached, the flow rate has increased substantially. The high-speed fluid does not follow the principle of large flow velocity at small section and small flow velocity at large section any more during movement, but the contrary is that the larger the section is, the faster the flow velocity is, so that huge thrust is generated. The structure can make the speed of the fluid change due to the change of the jet cross section area, so that the airflow is accelerated from subsonic speed to sonic speed to supersonic speed. Therefore, the trumpet-shaped nozzle is called a transonic nozzle. It is also called a laval nozzle, since it is invented by laval, sweden. The laval nozzle acts in effect as a "flow rate amplifier".
Disclosure of Invention
The technical problem to be solved by the invention is to provide a device for preparing precipitated calcium carbonate by using supercritical carbon dioxide, so as to improve the problems of dispersibility and stability in the production process of PCC carbonization, promote carbonization reaction, and ensure that the produced PCC has small particle size range and good quality consistency.
In order to achieve the purpose, the invention adopts the following technical means:
a device for preparing precipitated calcium carbonate by using supercritical carbon dioxide comprises a fine pulp inlet and supercritical CO 2 An input spray pipe, a carbonization reactor, a crystal form control agent inlet, a positive and negative paddle turbine combination, a Laval nozzle, a central shaft and supercritical CO 2 On the seminal plasma entry was located to the input spray tube, the entrance of seminal plasma entry linkage carbonization reactor, the seminal plasma entry is a bellmouth that reduces gradually, connects the osculum of bellmouth is connected to the pan feeding mouth of carbonization reactor, laval spout is connected to the discharge gate of carbonization reactor, carbonization reactor is a pan feeding mouth to the sealed tank body that reduces gradually again after the discharge end crescent, carbonization reactor's front end upper portion is equipped withThe inlet of the crystal form control agent, the combination of the positive and negative paddle turbines is arranged in the carbonization reactor and is arranged on a central shaft, and the central shaft is arranged on the central line of the carbonization reactor.
The positive and negative oar turbine combination has 1 group at least.
The positive and negative oar turbine wheel group constitute three groups, every group oar comprises positive oar and reversal oar, the positive oar and the reversal oar rotation direction of same group's thick liquid are opposite, three group's oar radius ratio is 1:1.5:2.
the ratio of the maximum diameter of the seminal plasma inlet to the maximum diameter of the carbonization reactor is 1.
The fine pulp inlet and the supercritical CO 2 The input spray pipe adopts heat preservation treatment measures.
A plurality of the devices are connected in series for use.
The carbonization reactor is provided with an inspection manhole.
A method for preparing PCC using an apparatus for preparing precipitated calcium carbonate using supercritical carbon dioxide, comprising the steps of:
(1) Feeding saturated calcium hydroxide slurry from a fine slurry inlet under pressure;
(2) From supercritical CO 2 The supercritical CO is fed into the input spray pipe 2 ；
(3) Mixing the saturated calcium hydroxide slurry with supercritical CO 2 The mixture is accelerated to be pressed into a carbonization reactor through a reducing pipeline which is gradually reduced;
(4) Feeding the saturated calcium hydroxide slurry and supercritical CO into the carbonization reactor through a combination of positive and negative paddle turbines 2 Stirring, and simultaneously adding a crystal form control agent through a crystal form control agent inlet;
(5) Discharging calcium carbonate slurry generated by the reaction from the Wahr nozzle.
The invention achieves the following beneficial effects:
1. by using supercritical liquid CO 2 The method has the characteristics of extremely strong dissolving power, and during the rapid phase change and multi-state mass and heat transfer processes, the carbonization reactants can fully react, so that the generated slurry is finer, the particle size range is small, and the shape consistency is good.
2. The device has simple structure and convenient maintenance and daily maintenance.
3. The positive and negative paddle turbine combination can homogenize the reactant and accelerate the multi-state heat and mass transfer process.
4. The device has higher reliability and is convenient to operate.
5. The forward and reverse paddle turbine combination can accelerate the reaction generation of the precipitated calcium carbonate.
Drawings
FIG. 1 is a schematic cross-sectional view of the structure of the present invention.
Fig. 2 is a schematic view of a blade of the present invention.
FIG. 3 is a schematic view of a positive and negative pitch turbine assembly of the present invention.
Labeled in the figure as: seminal plasma inlet 1, supercritical CO 2 The device comprises an input spray pipe 2, a carbonization reactor 3, a positive and negative paddle turbine combination 4, a crystal form control agent inlet 5, a Laval nozzle 6, a central shaft 7 and an inspection manhole 8.
Detailed Description
The invention is described below with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting.
Example 1
As shown in FIG. 1, this embodiment is the invention of the supercritical CO 2 An example of a multiphase spiral casing continuous carbonizing device for preparing PCC comprises a fine slurry inlet 1, supercritical CO 2 The device comprises an input spray pipe 2, a carbonization reactor 3, a positive and negative paddle turbine combination 4, a crystal form control agent inlet 5, a Laval nozzle 6, a central shaft 7 and an inspection manhole 8. The specific positions and connection relationships of the constituent members are as follows:
the supercritical CO 2 Input spray pipe 2 is located on seminal plasma entry 1, seminal plasma entry 1 connects carbonization reactor 3's entrance, seminal plasma entry 1 is a horn pipe that reduces gradually, carbonization reactor 3's pan feeding mouth is connected the osculum of seminal plasma entry, carbonization reactor's discharge gate is connected the laval spout, carbonization reactor is from the sealed jar body that reduces gradually again after a pan feeding mouth to the discharge end crescent, carbonization reactor's front end upper portionThe device is provided with a crystal form control agent inlet, the positive and negative paddle turbines are combined and arranged in the carbonization reactor and are arranged on a central shaft through a bearing, and the central shaft is arranged on the central line of the carbonization reactor.
The positive and negative paddle turbine combination is a combination body which is not connected together in practice, and the positive transmission paddle and the reverse rotation paddle of each positive and negative paddle turbine combination can rotate independently.
The combination of the positive and negative paddle turbines depends on fluid to rotate, and the drive module is not required to drive. The combined use of positive and negative paddle turbines can promote CO 2 And the flow of seminal plasma, thereby promoting the reaction.
The heat preservation treatment is carried out at the feed inlet so as to ensure that the supercritical CO is treated 2 Does not vaporize in advance.
Example 2
This example is an example of a method for producing PCC using an apparatus for producing precipitated calcium carbonate from supercritical carbon dioxide, comprising the steps of:
(1) The saturated calcium hydroxide slurry was fed under pressure from the fine slurry inlet so that the flow rate of the saturated calcium hydroxide slurry was mach 1.
(2) From supercritical CO 2 The supercritical CO is fed into the input spray pipe 2 (ii) a And accelerated to mach 1.5.
(3) Mixing the saturated calcium hydroxide slurry with supercritical CO 2 The mixture is accelerated to be pressed into a carbonization reactor through a reducing pipeline which is gradually reduced;
(4) Feeding the saturated calcium hydroxide slurry and supercritical CO into the carbonization reactor through a combination of positive and negative paddle turbines 2 Stirring, and simultaneously adding the crystal form control agent through a crystal form control agent inlet;
(5) Discharging calcium carbonate slurry generated by the reaction from the Wall nozzle, wherein the discharge is precipitated calcium carbonate.
It should be noted that supercritical CO will be used 2 The purpose of accelerating to Mach 1.5 is only to accelerate supercritical CO 2 Pressed into the seminal plasma inlet and penetrated into the saturated calcium hydroxide slurry.
The working principle and the process of the device are as follows:
saturated calcium hydroxide solution enters the carbonization reactor 3 from the seminal plasma inlet 1 and is supercriticalBoundary CO 2 From supercritical CO 2 The inlet lance 2 sprays into the carbonisation reactor 3. Saturated calcium hydroxide solution and supercritical CO 2 And simultaneously enters a carbonization reactor 3 for reaction to generate calcium carbonate slurry. Positive and negative oar turbine combination 4 passes through the bearing with center pin 7 and is connected, because the assembly direction is different, and a turbine corotation, another reversal stirs precipitation calcium carbonate slurry jointly for the calcium carbonate particle diameter that generates is more tiny, and constantly promotes the calcium carbonate slurry that generates backward, also plays high-speed homogenization's effect simultaneously. The crystal form control agent is added from a crystal form control agent inlet 5 to carry out surface coating modification on the calcium carbonate slurry. The processed calcium carbonate slurry is discharged from the laval nozzle 6. When the equipment is overhauled, the equipment enters from the manhole 8 to be overhauled and maintained.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical scope of the present invention and the equivalent alternatives or modifications according to the technical solution and the inventive concept of the present invention within the technical scope of the present invention.
Claims (8)
1. A device for preparing precipitated calcium carbonate by using supercritical carbon dioxide comprises a fine pulp inlet and supercritical CO 2 An input spray pipe, a carbonization reactor, a crystal form control agent inlet, and is characterized by also comprising a positive and negative paddle turbine combination, a Laval nozzle, a central shaft and supercritical CO 2 The input spray pipe is arranged on a fine slurry inlet, the fine slurry inlet is connected with the inlet of the carbonization reactor, the fine slurry inlet is a flared pipe which is gradually reduced, a feeding port connected with the carbonization reactor is connected with a small opening of the flared pipe, a discharging port of the carbonization reactor is connected with a laval nozzle, the carbonization reactor is a sealed tank body which is gradually reduced after the feeding port is gradually increased to the discharging end, the upper part of the front end of the carbonization reactor is provided with a crystal form control agent inlet, the positive and negative paddle turbines are combined and arranged in the carbonization reactor and are arranged on a central shaft, and the central shaft is arranged on the central line of the carbonization reactor; the combination of the positive and negative paddle turbines depends on fluid to rotate without being driven by a driving module, and each group of paddles consists of a positive rotating paddle and a negative rotating paddleThe rotating directions of the forward rotating paddle and the reverse rotating paddle of the same group of paddles are opposite.
2. The apparatus of claim 1, wherein the combination of positive and negative propellers comprises at least 1 set of turbines.
3. The apparatus according to claim 1, wherein the turbines of the forward and reverse paddles are combined into three groups, each group of paddles comprises a forward rotating paddle and a reverse rotating paddle, the forward rotating paddle and the reverse rotating paddle of the same group of paddles rotate in opposite directions, and the ratio of the radii of the three groups of paddles is 1:1.5:2.
4. the apparatus for preparing precipitated calcium carbonate using supercritical carbon dioxide as claimed in claim 1, wherein the ratio of the maximum diameter of the fine slurry inlet to the maximum diameter of the carbonization reactor is 1.
5. The apparatus of claim 1, wherein the refiner inlet and the supercritical CO are provided in the refiner inlet 2 The input spray pipe adopts heat preservation treatment measures.
6. The apparatus for producing precipitated calcium carbonate using supercritical carbon dioxide as claimed in claim 1, wherein a plurality of said apparatuses are used in series.
7. The apparatus for preparing precipitated calcium carbonate using supercritical carbon dioxide as claimed in claim 1, wherein the carbonation reactor is provided with a manhole.
8. A method for preparing precipitated calcium carbonate using the apparatus for preparing precipitated calcium carbonate using supercritical carbon dioxide according to claim 1, comprising the steps of:
(1) Feeding saturated calcium hydroxide slurry from a fine slurry inlet under pressure;
(2) From supercritical CO 2 The supercritical CO is fed into the input spray pipe 2 ；
(3) Mixing saturated calcium hydroxide slurry with supercritical CO 2 The mixture is accelerated to be pressed into a carbonization reactor through a reducing pipeline which is gradually reduced;
(4) Feeding the saturated calcium hydroxide slurry and supercritical CO into the carbonization reactor through a combination of positive and negative paddle turbines 2 Stirring, and simultaneously adding the crystal form control agent through a crystal form control agent inlet;
(5) Discharging calcium carbonate slurry generated by the reaction from the Wall nozzle.
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| JP2003200040A (en) * | 2001-11-01 | 2003-07-15 | Nikkiso Co Ltd | Fine powder collect unit |
| 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 |
| CN103601227A (en) * | 2013-09-11 | 2014-02-26 | 宜兴天力化工纳米科技有限公司 | Pre-nucleation reactor of nanometer calcium carbonate and preparation technology of the nanometer calcium carbonate |
| CN111204769A (en) * | 2020-01-14 | 2020-05-29 | 中南大学 | Method for preparing spherical white carbon black by supersonic carbon dioxide fluid carbonization method |
| CN111232077A (en) * | 2020-01-16 | 2020-06-05 | 宋承宣 | Positive and negative paddle negative pressure adsorption device based on Bernoulli principle |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003200040A (en) * | 2001-11-01 | 2003-07-15 | Nikkiso Co Ltd | Fine powder collect unit |
| 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 |
| CN103601227A (en) * | 2013-09-11 | 2014-02-26 | 宜兴天力化工纳米科技有限公司 | Pre-nucleation reactor of nanometer calcium carbonate and preparation technology of the nanometer calcium carbonate |
| CN111204769A (en) * | 2020-01-14 | 2020-05-29 | 中南大学 | Method for preparing spherical white carbon black by supersonic carbon dioxide fluid carbonization method |
| CN111232077A (en) * | 2020-01-16 | 2020-06-05 | 宋承宣 | Positive and negative paddle negative pressure adsorption device based on Bernoulli principle |
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