CN113044869A - Preparation process of high-dispersity pure nano calcium carbonate - Google Patents
Preparation process of high-dispersity pure nano calcium carbonate Download PDFInfo
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Abstract
The invention discloses a preparation process of high-dispersity pure nano calcium carbonate, which belongs to the technical field of calcium carbonate preparation, and can be used for triggering photo-thermal conversion action by guiding a carbonization reaction capsule on the surface of a carbonization ball to strong light through introducing the carbonization ball and giving strong light stimulation, forcing the carbonization ball to open a channel communicated with the outside through heat, accelerating sublimation of internal dry ice to release carbon dioxide in a low-temperature state, then distributing the carbon dioxide on the surface of the carbonization reaction capsule to be fully contacted with Ca (OH)2 slurry, rapidly dissolving the carbon dioxide in the slurry, and pushing Ca (OH)2 to accelerate dissolution, so that the carbonation reaction rate is accelerated to control the crystal nucleation rate, in addition, the channel is forced to be closed again by the low temperature of the released carbon dioxide, and the carbon dioxide can be fully dissolved and reacted in the next open time period, so that the prepared nano calcium carbonate has high purity and good dispersibility.
Description
Technical Field
The invention relates to the technical field of calcium carbonate preparation, in particular to a preparation process of high-dispersity pure nano calcium carbonate.
Background
Calcium carbonate is an inorganic compound of the formula CaCO3Limestone, stone powder, marble, etc. Calcium carbonate is neutral, substantially insoluble in water, and soluble in hydrochloric acid. It is one of the common substances on earth, exists in aragonite, calcite, chalk, limestone, marble, travertine and other rocks, and is also the main component of animal bones or shells. Calcium carbonate is also an important building material and has a wide range of industrial applications.
The nano calcium carbonate has good affinity with resin when being used in plastic, can effectively increase or adjust the rigidity, toughness, bending strength and the like of materials, can improve the rheological property of a plastic processing system, reduce the plasticizing temperature, and improve the size stability, heat resistance and surface smoothness of products; in rubber systems such as NR, BR, SBR and the like, the rubber is easy to knead and uniformly dispersed, the colloid is soft, and the extrusion processing performance and the model fluidity can be improved, so that the rubber product has the characteristics of smooth surface, large elongation, high tensile strength, small permanent deformation, good bending resistance, high tear resistance and the like.
An industrial preparation method of nano active calcium carbonate. The method comprises the step of introducing carbon dioxide gas into a suspension of Ca (OH)2 with a certain concentration for carbonization. Controlling the nucleation rate of calcium carbonate crystal nucleus by controlling the temperature of the Ca (OH)2 suspension and the flow of the carbon dioxide gas; after the carbonization is carried out until a certain number of crystal nuclei are formed, the crystal nucleus formation control is converted into crystal growth control, and at the moment, a crystal form regulator is added to control the growth rate of each crystal face, so that the controllable appearance is achieved; continuously carbonizing until the end point, adding a dispersing agent to adjust the surface charge of the particles to obtain evenly dispersed cubic calcium carbonate nano particles; then carrying out liquid phase surface coating treatment on the evenly dispersed cubic nano calcium carbonate particles. The obtained nano active calcium carbonate particles are controllable between 25 nm and 100nm, are cubic, have specific surface more than 25m2/g, particle size distribution GSD of 1.57, oil absorption value less than 28g/100g CaCO3, and have no agglomeration phenomenon. The obtained product has excellent performance and can be used as functional filler in high-grade rubber, plastics and automobile primers.
However, in the actual preparation process of the nano calcium carbonate, a freezing method is usually adopted, in order to increase the solubility of calcium hydroxide to accelerate the carbonation reaction rate and control the crystal nucleation rate, but the temperature distribution of the suspension is not uniform, and the dissolution rates of carbon dioxide and calcium hydroxide are not uniform, so that the prepared nano calcium carbonate is not easy to control, and the agglomeration phenomenon is easy to occur.
Disclosure of Invention
1. Technical problem to be solved
Aiming at the problems in the prior art, the invention aims to provide a preparation process of high-dispersity pure nano calcium carbonate, which can be realized by introducing a carbonization ball manner and giving strong light stimulation, a carbonization reaction capsule on the surface of the carbonization ball is used for guiding the strong light to trigger a photothermal conversion action, the carbonization ball is forced to open a channel communicated with the outside by using heat, meanwhile, dry ice in the carbonization ball is accelerated to sublimate and release carbon dioxide in a low-temperature state, then the carbon dioxide is distributed on the surface of the carbonization reaction capsule and is fully contacted with Ca (OH)2 slurry, the carbon dioxide can be rapidly dissolved in the slurry, Ca (OH)2 is pushed to be accelerated to dissolve, so that the carbonation reaction rate is accelerated to control the crystal nucleation rate, in addition, the channel is forced to be closed again by the low temperature after the carbon dioxide is released, the carbon dioxide can be fully dissolved, meanwhile, the compression action on the surface of the carbonization reaction capsule is triggered when the next time of release is carried out, and the formed nano calcium carbonate falls off to reserve a reaction space, so that the prepared nano calcium carbonate has high purity and good dispersibility.
2. Technical scheme
In order to solve the above problems, the present invention adopts the following technical solutions.
A preparation process of pure nano calcium carbonate with high dispersibility comprises the following steps:
s1, adding amino acid into a charging bucket containing Ca (OH)2 slurry, wherein the weight ratio of the amino acid to the Ca (OH)2 slurry is 0.2-2:100, and stirring and mixing uniformly;
s2, putting a plurality of uniformly distributed carbonization balls into the charging bucket, giving strong light stimulation to the carbonization balls, forcing the carbonization balls to indirectly adhere to the wall to release low-temperature carbon dioxide, and carrying out carbonization reaction on the carbon dioxide and Ca (OH)2 slurry;
s3, detecting the pH value of the slurry in the material tank in real time, and stopping strong light stimulation when the pH value reaches 7-8 to obtain the calcium carbonate cooked slurry;
s4, heating the calcium carbonate cooked slurry to 60-75 ℃, adding a surface treating agent for activation treatment, and filtering to obtain filter residue;
and S5, washing, drying and dehydrating the filter residue, and then crushing, refining and screening to obtain the nano calcium carbonate.
Further, the charging bucket in the step S1 is made of a light-proof heat insulation material and is placed in a dark environment.
Further, the amino acid in step S1 is one or a combination of two or more of alanine, glycine, and glutamic acid.
Further, the temperature of the slurry in the material tank in the step S2 is controlled to be 10-30 ℃, and the carbonization reaction time is controlled to be 40-60 min.
Further, the carbonization ball in the step S2 includes a light-weight thermal insulation ball shell and a plurality of carbonization reaction capsules, and the carbonization reaction capsules are uniformly embedded in the outer surface of the light-weight thermal insulation ball shell, dry ice is filled in the light-weight thermal insulation ball shell, the carbonization reaction capsules force the dry ice inside to accelerate sublimation and release carbon dioxide in a low-temperature state after being stimulated by strong light, and then the carbonization reaction capsules are fully contacted with ca (oh)2 slurry on the surface thereof to perform carbonization reaction.
Further, the carbonization reaction bag sequentially comprises a carbon dioxide adsorption material layer, a waterproof breathable film, a black carbon base layer and a combined heat preservation layer from outside to inside, the waterproof breathable film is coated on the inner surface of the carbon dioxide adsorption material layer, a plurality of photo-thermal expansion balls which are uniformly distributed are embedded and connected on the black carbon base layer, one end, far away from the combined heat preservation layer, of each photo-thermal expansion ball is connected with a light guide wire, each light guide wire penetrates through the carbon dioxide adsorption material layer and extends to the outside, each light guide wire is connected with the waterproof breathable film, and the photo-thermal expansion balls convert light energy into heat energy to be heated and expanded after receiving illumination through the light guide wires, so that on one hand, the nano calcium carbonate formed by compression and extrusion of the carbon dioxide adsorption material layer is replaced by Ca (OH)2 slurry, on the other hand, the combined heat, and heating the dry ice inside to force the dry ice to sublimate and release the carbon dioxide in a low-temperature state, and fully dissolving the carbon dioxide in the carbon dioxide adsorbing material layer to carry out carbonization reaction with the Ca (OH)2 slurry.
Further, the light and heat inflation ball includes astigmatism hemisphere, heat conduction band piece and thermal expansion hemisphere, the heat conduction band piece is connected between astigmatism hemisphere and thermal expansion hemisphere, and the heat conduction band piece is connected with black charcoal basal layer, astigmatism hemisphere and thermal expansion hemisphere symmetric distribution, and the astigmatism hemisphere is connected with the light guide wire, and the astigmatism hemisphere can disperse the illumination that the light guide wire received, then absorbs and converts the heat by black charcoal basal layer to heat the heat conduction band piece, the thermal expansion hemisphere expands under the heated state, compresses the carbon dioxide adsorption material layer earlier, then extrudees its open channel to the combination heat preservation again.
Further, the combination heat preservation includes polylith stiff end, removal end and many reset wires, it inlays on the fixed end to remove the even activity of end, and removes the end and correspond with light and heat expansion ball, reset wire connects between removal end and black charcoal basal layer, and stiff end and removal end play the heat preservation effect for a whole under the normal condition, after receiving the extrusion of light and heat expansion ball, remove the end to the inboard remove to communicate with the external world, and the heat of light and heat expansion ball can enter into in the light heat preservation spherical shell and heat the dry ice, and carbon dioxide releases away from the clearance after the dry ice sublimation, then reduces the temperature to the light and heat expansion ball and resume the shape, and it is closed again that the removal end also can reset, and then realizes carbon dioxide's intermittent type nature release.
Further, the surface treatment agent in the step S4 is a mixture of sodium resinate and cocoyl diethanolamine gemini quaternary ammonium salt, and the weight ratio of the sodium resinate to the cocoyl diethanolamine gemini quaternary ammonium salt is 3-7: 7-3.
Further, the weight ratio of the surface treating agent to the calcium carbonate cooked pulp in the step S4 is 3-6:100, and the surface treating agent is heated to 80-95 ℃ and then mixed and stirred for more than 1h for activation treatment.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
(1) the scheme can trigger photo-thermal conversion action by introducing a carbonization ball and giving stimulation to strong light, the carbonization reaction capsule on the surface of the carbonization ball guides the strong light, the carbonization ball is forced to open a channel communicated with the outside by using heat, simultaneously, the internal dry ice is accelerated to sublimate and release the carbon dioxide in a low-temperature state, and then the carbon dioxide is distributed on the surface of the carbonization reaction capsule to be fully contacted with Ca (OH)2 slurry, the carbon dioxide can be quickly dissolved in the slurry and pushes Ca (OH)2 to be dissolved in an accelerating manner, so that the carbonation reaction rate is accelerated to control the crystal nucleation rate, in addition, the channel can be forced to be closed again by the low temperature of the released carbon dioxide, the carbon dioxide can be fully dissolved and reacted in the next opening time period, meanwhile, the compression action on the surface of the carbonization reaction capsule can be triggered when the carbon dioxide is released next, so that the prepared nano calcium carbonate has high purity and good dispersibility.
(2) The carbonization ball comprises a light heat-preservation ball shell and a plurality of carbonization reaction bags, the carbonization reaction bags are uniformly embedded on the outer surface of the light heat-preservation ball shell, dry ice is filled in the light heat-preservation ball shell, the carbonization reaction bags can force the dry ice in the carbonization reaction bags to be sublimated and release carbon dioxide in a low-temperature state in an accelerating way after being stimulated by strong light, and then the surfaces of the carbonization reaction bags are in full contact with Ca (OH)2 slurry to carry out carbonization reaction.
(3) The carbonization reaction bag sequentially comprises a carbon dioxide adsorption material layer, a waterproof breathable film, a black carbon base layer and a combined heat preservation layer from outside to inside, the waterproof breathable film is coated on the inner surface of the carbon dioxide adsorption material layer, a plurality of photo-thermal expansion balls which are uniformly distributed are embedded and connected on the black carbon base layer, one end, far away from the combined heat preservation layer, of each photo-thermal expansion ball is connected with a light guide wire, each light guide wire penetrates through the carbon dioxide adsorption material layer and extends to the outside, each light guide wire is connected with the waterproof breathable film, and the photo-thermal expansion balls convert light energy into heat energy to be heated and expanded after receiving illumination through the light guide wires, on one hand, the nano calcium carbonate formed by compressing and extruding the carbon dioxide adsorption material layer is replaced by Ca (OH)2 slurry, on the other hand, the combined heat preservation layer is, the dry ice is forced to accelerate sublimation and release the carbon dioxide in a low-temperature state, and the carbon dioxide is fully dissolved in the carbon dioxide adsorbing material layer to carry out carbonization reaction with the Ca (OH)2 slurry.
(4) The light and heat inflation ball includes the astigmatism hemisphere, heat conduction band piece and thermal energy hemisphere, the heat conduction band piece is connected between astigmatism hemisphere and thermal energy hemisphere, and the heat conduction band piece is connected with black charcoal base layer, astigmatism hemisphere and thermal energy hemisphere symmetric distribution, and the astigmatism hemisphere is connected with the light guide wire, the astigmatism hemisphere can disperse the illumination that the light guide wire received, then absorb and turn into the heat by black charcoal base layer, thereby heat the heat conduction band piece, the thermal energy hemisphere expands under the heated state, compress the carbon dioxide adsorbent layer earlier, then extrude its open channel to the combination heat preservation again.
(5) The combination heat preservation includes the polylith stiff end, remove end and many silk that resets, it inlays on the fixed end to remove the even activity of end, and it corresponds with light and heat expansion ball to remove the end, the silk that resets is connected between removal end and black charcoal basal layer, stiff end and removal end play the heat preservation effect for a whole under the normal condition, after receiving the extrusion of light and heat expansion ball, remove the end to the inboard remove to communicate with external world, the heat of light and heat expansion ball can enter into in the light heat preservation spherical shell to heat the dry ice, carbon dioxide releases away from the clearance after the dry ice sublimation, then cool down the heat expansion ball and resume the shape, it is closed again that the removal end also can reset, and then realize the intermittent type nature release of carbon dioxide.
Drawings
FIG. 1 is a schematic flow diagram of the present invention;
FIG. 2 is a schematic structural view of a carbonized sphere of the present invention;
FIG. 3 is a schematic structural view of the photothermal expansion ball of the present invention;
FIG. 4 is a schematic view of the structure of the composite insulation of the present invention;
FIG. 5 is a schematic view showing a structure in a carbonization reaction of a carbonized sphere of the present invention.
The reference numbers in the figures illustrate:
the light heat-insulation composite material comprises a light heat-insulation spherical shell 1, a carbon dioxide adsorption material layer 2, a photo-thermal expansion ball 3, a light-scattering hemisphere 31, a heat conduction band sheet 32, a thermal expansion hemisphere 33, a light-conducting wire 4, a black carbon base layer 5, a combined heat-insulation layer 6, a fixed end 61, a movable end 62, a reset wire 63, dry ice 7 and a waterproof and breathable film 8.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention; it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and all other embodiments obtained by those skilled in the art without any inventive work are within the scope of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "top/bottom", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "sleeved/connected," "connected," and the like are to be construed broadly, e.g., "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1:
referring to fig. 1, a process for preparing pure nano calcium carbonate with high dispersibility includes the following steps:
s1, adding amino acid into a charging bucket containing Ca (OH)2 slurry, wherein the weight ratio of the amino acid to the Ca (OH)2 slurry is 0.2:100, and stirring and mixing uniformly;
s2, putting a plurality of uniformly distributed carbonization balls into the charging bucket, giving strong light stimulation to the carbonization balls, forcing the carbonization balls to indirectly adhere to the wall to release low-temperature carbon dioxide, and carrying out carbonization reaction on the carbon dioxide and Ca (OH)2 slurry;
s3, detecting the pH value of the slurry in the material tank in real time, and stopping strong light stimulation when the pH value reaches 7-8 to obtain the calcium carbonate cooked slurry;
s4, heating the calcium carbonate cooked slurry to 60 ℃, adding a surface treating agent for activation treatment, and filtering to obtain filter residue;
and S5, washing, drying and dehydrating the filter residue, and then crushing, refining and screening to obtain the nano calcium carbonate.
The charging bucket in the step S1 is made of light-proof heat insulation materials and is placed in a light-free environment.
The amino acid in step S1 is one or a combination of two or more of alanine, glycine, and glutamic acid.
In the step S2, the temperature of the slurry in the material tank is controlled at 10 ℃, and the carbonization reaction time is controlled at 40 min.
Referring to fig. 2, the carbonization ball in step S2 includes a light-weight thermal insulation ball shell 1 and a plurality of carbonization reaction capsules, the carbonization reaction capsules are uniformly embedded in the outer surface of the light-weight thermal insulation ball shell 1, dry ice 7 is filled in the light-weight thermal insulation ball shell 1, the carbonization reaction capsules force the dry ice 7 inside to accelerate sublimation and release carbon dioxide in a low-temperature state after being stimulated by strong light, and then the surface of the carbonization reaction capsules is in full contact with ca (oh)2 slurry to perform carbonization reaction.
The carbonization reaction capsule comprises a carbon dioxide adsorption material layer 2, a waterproof breathable film 8, a black carbon base layer 5 and a combined heat preservation layer 6 in sequence from outside to inside, the carbon dioxide adsorption material layer 2 can be any one or more of silicon dioxide, silica gel, silicate and aluminosilicate with a porous structure, the waterproof breathable film 8 is coated on the inner surface of the carbon dioxide adsorption material layer 2, a plurality of photo-thermal expansion balls 3 which are uniformly distributed are embedded and connected on the black carbon base layer 5, one end of each photo-thermal expansion ball 3, which is far away from the combined heat preservation layer 6, is connected with a light guide wire 4, the light guide wire 4 penetrates through the carbon dioxide adsorption material layer 2 and extends to the outside, the light guide wire 4 is connected with the waterproof breathable film 8, the photo-thermal expansion balls 3 convert light energy into heat energy for heating expansion after receiving illumination through the light guide wire 4, and on the one, and replacing the Ca (OH)2 slurry, on the other hand, reversely extruding the combined heat-insulating layer 6 to open a channel after the continuous compression is not available, heating the dry ice 7 in the heat-insulating layer, forcing the dry ice 7 to be sublimated rapidly to release carbon dioxide in a low-temperature state, and fully dissolving the carbon dioxide in the carbon dioxide adsorption material layer 2 to perform carbonization reaction with the Ca (OH)2 slurry.
Referring to fig. 3, the photo-thermal expansion ball 3 includes a light diffusion hemisphere 31, a heat conduction band sheet 32 and a thermal expansion hemisphere 33, the light diffusion hemisphere 31 is made of a light reflection material into an irregular spherical shape, the heat conduction band sheet 32 is connected between the light diffusion hemisphere 31 and the thermal expansion hemisphere 33, the heat conduction band sheet 32 is connected to the black carbon base layer 5, the light diffusion hemisphere 31 and the thermal expansion hemisphere 33 are symmetrically distributed, the light diffusion hemisphere 31 is connected to the light guide wire 4, the light diffusion hemisphere 31 can disperse the light received by the light guide wire 4, and the light is absorbed and converted into heat by the black carbon base layer 5, so as to heat the heat conduction band sheet 32, the thermal expansion hemisphere 33 expands in a heated state, the carbon dioxide adsorption material layer 2 is compressed, and then the combined thermal insulation layer 6 is extruded to force the opening of.
Please refer to fig. 4, the combined insulating layer 6 includes a plurality of fixed ends 61, a movable end 62 and a plurality of reset wires 63, the movable end 62 is embedded on the fixed end 61, and the movable end 62 corresponds to the photo-thermal expansion ball 3, the reset wires 63 are connected between the movable end 62 and the black carbon base layer 5, the fixed end 61 and the movable end 62 in a normal state are a whole to play a role in insulating heat, after being extruded by the photo-thermal expansion ball 3, the movable end 62 is moved to the inner side to be communicated with the outside, the heat of the photo-thermal expansion ball 3 can enter the light insulating ball shell 1 to heat the dry ice 7, carbon dioxide is released from the gap after the dry ice 7 is sublimated, then the photo-thermal expansion ball 3 is cooled to restore the shape, the movable end 62 is also reset and closed again, and then the intermittent release of.
The surface treatment agent in the step S4 is a mixture of sodium resinate and cocoyl diethanolamine gemini quaternary ammonium salt, and the weight ratio of the sodium resinate to the cocoyl diethanolamine gemini quaternary ammonium salt is 3: 7.
The weight ratio of the surface treating agent to the calcium carbonate cooked pulp in the step S4 is 3:100, and the surface treating agent is heated to 80 ℃ and then mixed and stirred for more than 1h for activation treatment.
Example 2:
a preparation process of pure nano calcium carbonate with high dispersibility comprises the following steps:
s1, adding amino acid into a charging bucket containing Ca (OH)2 slurry, wherein the weight ratio of the amino acid to the Ca (OH)2 slurry is 1:100, and stirring and mixing uniformly;
s2, putting a plurality of uniformly distributed carbonization balls into the charging bucket, giving strong light stimulation to the carbonization balls, forcing the carbonization balls to indirectly adhere to the wall to release low-temperature carbon dioxide, and carrying out carbonization reaction on the carbon dioxide and Ca (OH)2 slurry;
s3, detecting the pH value of the slurry in the material tank in real time, and stopping strong light stimulation when the pH value reaches 7-8 to obtain the calcium carbonate cooked slurry;
s4, heating the calcium carbonate cooked slurry to 70 ℃, adding a surface treating agent for activation treatment, and filtering to obtain filter residue;
and S5, washing, drying and dehydrating the filter residue, and then crushing, refining and screening to obtain the nano calcium carbonate.
In the step S2, the temperature of the slurry in the slurry tank is controlled at 20 ℃, and the carbonization reaction time is controlled at 50 min.
The surface treatment agent in the step S4 is a mixture of sodium resinate and cocoyl diethanolamine gemini quaternary ammonium salt, and the weight ratio of the sodium resinate to the cocoyl diethanolamine gemini quaternary ammonium salt is 5: 5.
The weight ratio of the surface treating agent to the calcium carbonate cooked pulp in the step S4 is 4:100, and the surface treating agent is heated to 90 ℃ and then mixed and stirred for more than 1h for activation treatment.
The remainder was in accordance with example 1.
Example 3:
a preparation process of pure nano calcium carbonate with high dispersibility comprises the following steps:
s1, adding amino acid into a charging bucket containing Ca (OH)2 slurry, wherein the weight ratio of the amino acid to the Ca (OH)2 slurry is 2:100, and stirring and mixing uniformly;
s2, putting a plurality of uniformly distributed carbonization balls into the charging bucket, giving strong light stimulation to the carbonization balls, forcing the carbonization balls to indirectly adhere to the wall to release low-temperature carbon dioxide, and carrying out carbonization reaction on the carbon dioxide and Ca (OH)2 slurry;
s3, detecting the pH value of the slurry in the material tank in real time, and stopping strong light stimulation when the pH value reaches 7-8 to obtain the calcium carbonate cooked slurry;
s4, heating the calcium carbonate cooked slurry to 75 ℃, adding a surface treating agent for activation treatment, and filtering to obtain filter residue;
and S5, washing, drying and dehydrating the filter residue, and then crushing, refining and screening to obtain the nano calcium carbonate.
In the step S2, the temperature of the slurry in the charging basket is controlled at 30 ℃, and the carbonization reaction time is controlled at 60 min.
The surface treatment agent in the step S4 is a mixture of sodium resinate and cocoyl diethanolamine gemini quaternary ammonium salt, and the weight ratio of the sodium resinate to the cocoyl diethanolamine gemini quaternary ammonium salt is 7: 3.
The weight ratio of the surface treating agent to the calcium carbonate cooked pulp in the step S4 is 6:100, and the surface treating agent is heated to 95 ℃ and then mixed and stirred for more than 1h for activation treatment.
The remainder was in accordance with example 1.
Referring to fig. 5, the present invention can trigger photothermal conversion by introducing a carbonization ball and giving strong light stimulation, the carbonization reaction capsule on the surface of the carbonization ball guides the strong light, the carbonization ball is forced to open a channel communicated with the outside by heat, meanwhile, dry ice inside the carbonization reaction capsule is accelerated to sublimate and release carbon dioxide in a low temperature state, and then the carbon dioxide is distributed on the surface of the carbonization reaction capsule and fully contacts with ca (oh)2 slurry, the carbon dioxide can be rapidly dissolved in the slurry, and the ca (oh)2 is pushed to be dissolved rapidly, so that the carbonation reaction rate is accelerated to control the nucleation rate of crystals, in addition, the channel is forced to close again by the low temperature after the carbon dioxide is released, the carbon dioxide can be dissolved and reacted sufficiently in the next opening time period, meanwhile, the compression action on the surface of the carbonization reaction capsule is triggered when the next release is performed, and the formed nano, so that the prepared nano calcium carbonate has high purity and good dispersibility.
The above are merely preferred embodiments of the present invention; the scope of the invention is not limited thereto. Any person skilled in the art should be able to cover the technical scope of the present invention by equivalent or modified solutions and modifications within the technical scope of the present invention.
Claims (10)
1. A preparation process of pure nano calcium carbonate with high dispersibility is characterized by comprising the following steps: the method comprises the following steps:
s1, adding amino acid into a charging bucket containing Ca (OH)2 slurry, wherein the weight ratio of the amino acid to the Ca (OH)2 slurry is 0.2-2:100, and stirring and mixing uniformly;
s2, putting a plurality of uniformly distributed carbonization balls into the charging bucket, giving strong light stimulation to the carbonization balls, forcing the carbonization balls to indirectly adhere to the wall to release low-temperature carbon dioxide, and carrying out carbonization reaction on the carbon dioxide and Ca (OH)2 slurry;
s3, detecting the pH value of the slurry in the material tank in real time, and stopping strong light stimulation when the pH value reaches 7-8 to obtain the calcium carbonate cooked slurry;
s4, heating the calcium carbonate cooked slurry to 60-75 ℃, adding a surface treating agent for activation treatment, and filtering to obtain filter residue;
and S5, washing, drying and dehydrating the filter residue, and then crushing, refining and screening to obtain the nano calcium carbonate.
2. The process for preparing pure nano calcium carbonate with high dispersibility according to claim 1, wherein the process comprises the following steps: the charging bucket in the step S1 is made of light-proof heat insulation materials and is placed in a dark environment.
3. The process for preparing pure nano calcium carbonate with high dispersibility according to claim 1, wherein the process comprises the following steps: the amino acid in the step S1 is one or the combination of more than two of alanine, glycine and glutamic acid.
4. The process for preparing pure nano calcium carbonate with high dispersibility according to claim 1, wherein the process comprises the following steps: in the step S2, the temperature of the slurry in the slurry tank is controlled to be 10-30 ℃, and the carbonization reaction time is controlled to be 40-60 min.
5. The process for preparing pure nano calcium carbonate with high dispersibility according to claim 1, wherein the process comprises the following steps: the carbonization ball in the step S2 comprises a light heat-preservation ball shell (1) and a plurality of carbonization reaction bags, the carbonization reaction bags are uniformly embedded in the outer surface of the light heat-preservation ball shell (1), and dry ice (7) is filled in the light heat-preservation ball shell (1).
6. The process for preparing pure nano calcium carbonate with high dispersibility according to claim 5, wherein the process comprises the following steps: the carbonization reaction bag includes carbon dioxide adsorption material layer (2), waterproof ventilated membrane (8), black charcoal basic unit (5) and combination heat preservation (6) from outer to interior in proper order, waterproof ventilated membrane (8) cladding is in the internal surface of carbon dioxide adsorption material layer (2), inlay on black charcoal basic unit (5) and be connected with a plurality of evenly distributed's light and heat inflation ball (3), light and heat inflation ball (3) are kept away from combination heat preservation (6) one end and are connected with light guide wire (4), and light guide wire (4) run through carbon dioxide adsorption material layer (2) and extend to the outside, light guide wire (4) are connected with waterproof ventilated membrane (8).
7. The process for preparing pure nano calcium carbonate with high dispersibility according to claim 6, wherein the process comprises the following steps: the photo-thermal expansion ball (3) comprises an astigmatism hemisphere (31), a heat conduction band sheet (32) and a thermal expansion hemisphere (33), the heat conduction band sheet (32) is connected between the astigmatism hemisphere (31) and the thermal expansion hemisphere (33), the heat conduction band sheet (32) is connected with a black carbon base layer (5), the astigmatism hemisphere (31) and the thermal expansion hemisphere (33) are symmetrically distributed, and the astigmatism hemisphere (31) is connected with a light guide wire (4).
8. The process for preparing pure nano calcium carbonate with high dispersibility according to claim 6, wherein the process comprises the following steps: combination heat preservation (6) include polylith stiff end (61), remove end (62) and many silk (63) that reset, it inlays on stiff end (61) to remove the even activity of end (62), and removes end (62) and light and heat inflation ball (3) corresponding, silk (63) that reset are connected between removal end (62) and black carbon basal layer (5).
9. The process for preparing pure nano calcium carbonate with high dispersibility according to claim 1, wherein the process comprises the following steps: the surface treatment agent in the step S4 is a mixture of sodium resinate and cocoyl diethanolamine gemini quaternary ammonium salt, and the weight ratio of the sodium resinate to the cocoyl diethanolamine gemini quaternary ammonium salt is 3-7: 7-3.
10. The process for preparing pure nano calcium carbonate with high dispersibility according to claim 1, wherein the process comprises the following steps: the weight ratio of the surface treating agent to the calcium carbonate cooked pulp in the step S4 is 3-6:100, and the surface treating agent is heated to 80-95 ℃ and then mixed and stirred for more than 1h for activation treatment.
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