CN111909539A - Industrial preparation method for improving affinity of nano calcium carbonate for adhesive - Google Patents
Industrial preparation method for improving affinity of nano calcium carbonate for adhesive Download PDFInfo
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- CN111909539A CN111909539A CN202010557480.7A CN202010557480A CN111909539A CN 111909539 A CN111909539 A CN 111909539A CN 202010557480 A CN202010557480 A CN 202010557480A CN 111909539 A CN111909539 A CN 111909539A
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- calcium carbonate
- nano calcium
- lime milk
- limestone
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/021—Calcium carbonates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/185—After-treatment, e.g. grinding, purification, conversion of crystal morphology
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
Abstract
The invention discloses an industrial preparation method for improving the affinity of nano calcium carbonate for an adhesive, which is characterized in that the nano calcium carbonate takes limestone as a raw material and is calcined at high temperature, meanwhile, water is added into the calcined limestone as a solvent to be dissolved, then, grinding is carried out to obtain lime milk, and finally, the nano calcium carbonate is obtained by purification. According to the industrial preparation method for improving the affinity of the nano calcium carbonate for the adhesive, a proper amount of coconut oil, silicic acid, lactic acid and oleic acid are added into the finished product of the nano calcium carbonate as an adhesive and are fully stirred, so that the adhesive and the nano calcium carbonate are fully fused, the adhesiveness of the nano calcium carbonate can be effectively improved, the affinity of the nano calcium carbonate can be improved, the fusion effect of the nano calcium carbonate can be conveniently increased during subsequent processing, and the quality of the finished product during subsequent processing by using the nano calcium carbonate can be conveniently improved.
Description
Technical Field
The invention relates to the technical field of a preparation method of nano calcium carbonate, in particular to an industrial preparation method for improving the affinity of nano calcium carbonate for an adhesive.
Background
The nano calcium carbonate is a novel superfine solid material developed in the 80 th century, compared with the common calcium carbonate, the physical property of the nano calcium carbonate is greatly improved, so that the nano calcium carbonate can play roles of strengthening and toughening in a plurality of application fields, the usability and the appearance of the product are improved, expensive raw materials such as white carbon black can be partially replaced, the product cost is reduced, and the quality is greatly improved, so that the nano calcium carbonate shows wide applicability and vigorous market demand once appearing, has wide application in the fields of coatings, plastics, rubber, adhesives, papermaking, printing ink, paint, cosmetics, medicines and the like, and in the last two years, the nano calcium carbonate is concerned by more and more people in the industry, and international and domestic famous enterprises actively research the production and application technology of the nano calcium carbonate, the application field of the method is continuously expanded, and the market scale is gradually enlarged.
As disclosed in publication No.: CN102491396B a method for preparing nano calcium carbonate, relating to a method for preparing nano calcium carbonate. Provides a method for preparing nano calcium carbonate which can carry out carbonization reaction under anhydrous condition under the participation of high-pressure carbon dioxide and ionic liquid. Adding calcium hydroxide, ionic liquid and carbon dioxide into a high-pressure kettle for carbonization reaction; separating the reaction product to obtain the nano calcium carbonate product, and recovering the ionic liquid. The carbon dioxide, especially supercritical carbon dioxide, participates in the carbonization reaction under the assistance of the ionic liquid, and the carbonization reaction has the obvious characteristic that no water participates; the participation of the ionic liquid can greatly improve the reaction rate and control the particle size of the product; the ionic liquid can be conveniently recycled, and the method is a green chemical production process; the ionic liquid can be room-temperature ionic liquid or non-room-temperature ionic liquid, and is convenient for selection of industrial application.
As disclosed in publication No.: the invention relates to the field of nano material preparation, in particular to a preparation method of nano calcium carbonate, and provides CN 106335917A. The invention provides a preparation method of nano calcium carbonate, which comprises the following steps: (1) dissolving calcium oxide in water to obtain suspension of calcium hydroxide; (2) adding a surfactant into the suspension obtained in the step (1), and stirring to prepare mixed slurry; (3) continuously introducing CO2 into the mixed slurry obtained in the step (2) under the condition of continuous stirring until the pH value is reduced to 6-9; (4) filtering, cleaning and drying to obtain the nano calcium carbonate. The nano calcium carbonate prepared by the invention is spherical, the particle size distribution of the nano calcium carbonate is concentrated in the range of 20-100nm, the size distribution is uniform, the preparation process is simple, the cost is low, and the industrial popularization and production of the nano calcium carbonate are easy to realize, but the preparation method of the nano calcium carbonate can cause insufficient adhesion inside the nano calcium carbonate after the nano calcium carbonate is prepared, so that the nano calcium carbonate can cause the phenomenon of insufficient raw material fusion due to poor adhesive viscosity in the subsequent processing and using processes, and further the quality of finished product preparation can be influenced by the insufficiently fused nano calcium carbonate, so that an industrial preparation method for improving the affinity of the nano calcium carbonate for the adhesive is urgently needed to solve the problems.
Disclosure of Invention
The invention aims to provide an industrial preparation method for improving the affinity of nano calcium carbonate for an adhesive, and aims to solve the problem that the prior partial nano calcium carbonate preparation method proposed in the background art has poor internal adhesiveness and influences the quality of a subsequent processed finished product.
In order to achieve the purpose, the invention provides the following technical scheme: an industrial preparation method for improving the affinity of nano calcium carbonate for an adhesive comprises the steps of calcining limestone serving as a raw material at a high temperature, adding water into the calcined limestone serving as a solvent to dissolve the limestone, grinding the limestone to obtain lime milk, and purifying the lime milk to obtain the nano calcium carbonate;
the method comprises the following steps: putting large limestone into equipment for full crushing, adding water, and fusing with crushed limestone to obtain lime milk;
step two: carrying out multi-stage hydrocyclone separation on the lime milk to remove particles and impurities carried in the lime milk to obtain refined lime milk suspension with a certain concentration;
step three: then adding carbon dioxide gas into the lime milk suspension, adding a crystal form control agent, controlling the crystal shape of the nano calcium carbonate, starting carbonization, and concentrating the lime milk solution;
step four: dehydrating and drying the concentrated lime milk solution to obtain lime milk powder;
step five: adding a reagent into the lime milk powder for surface treatment to obtain nano calcium carbonate;
step six: adding adhesive into the nano calcium carbonate to obtain the high-viscosity nano calcium carbonate.
Preferably, the nano calcium carbonate comprises the following components in percentage by mass: the proportion of lime milk is 95 percent, and the whole mass of each group of reagents is 5 percent.
Preferably, the limestone calcining temperature is 1200 ℃, and the water body temperature is 20 ℃.
Preferably, in the step 1, the large limestone is crushed in advance, and then may be calcined, and at the same time, the calcined limestone is added with water to be dissolved to form a mixed solution, and after the mixed solution is changed into the mixed solution, the mixed solution may be ground by using external equipment to obtain a limestone turbid solution, and the limestone turbid solution is extracted to prepare the lime milk.
Preferably, the lime milk obtained in the step 2 is subjected to multi-stage centrifugal separation through a centrifugal machine, impurities and fine particles carried in the lime milk are removed, and the lime milk is sieved through a 200-mesh screen, so that a refined lime milk suspension with a certain concentration and after impurities are removed can be obtained.
Preferably, in the step 3, carbon dioxide with a concentration of 75% is added into the refined lime milk suspension after the impurities are removed, meanwhile, a proper amount of 2% of crystal form control agent is added into the refined lime milk suspension, the crystal shape generated by the subsequent nano calcium carbonate reaction is controlled by controlling the dosage of the added crystal form control agent, and meanwhile, the refined lime milk suspension can be carbonized through oxygen-free high-temperature heating, so that the refined lime milk suspension can be concentrated.
Preferably, in the step 4, the concentrated lime milk suspension is deoxidized and dried at high temperature under the environment of 1000 ℃, and then ground to obtain the lime milk powder.
Preferably, the modified high molecular ionic polymer is added into the lime milk powder in the step 5, and the surface treatment is carried out on the lime milk powder particles, so as to obtain the nano calcium carbonate.
Preferably, after the extraction of the nano calcium carbonate is finished, 2% of a proper amount of adhesive can be added into the nano calcium carbonate, and the nano calcium carbonate with improved adhesiveness can be obtained by fully shaking and mixing.
Compared with the prior art, the invention has the beneficial effects that: according to the industrial preparation method for improving the affinity of the nano calcium carbonate for the adhesive, a proper amount of coconut oil, silicic acid, lactic acid and oleic acid are added into the finished product of the nano calcium carbonate as an adhesive and are fully stirred, so that the adhesive and the nano calcium carbonate are fully fused, the adhesiveness of the nano calcium carbonate can be effectively improved, the affinity of the nano calcium carbonate can be improved, the fusion effect of the nano calcium carbonate can be conveniently increased during subsequent processing, and the quality of the finished product during subsequent processing by using the nano calcium carbonate can be conveniently improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the text in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without any creative effort, shall fall within the protection scope of the present invention.
Please refer to two embodiments provided by the present invention:
the first embodiment is as follows:
5000g of a large limestone is pulverized in advance using a pulverizer, and then the pulverized small limestone particles are put into a high-temperature calcining furnace and calcined at a high temperature of 1000 ℃ for 15 minutes, and then, taking out the limestone calcined at high temperature from the high-temperature calcining furnace, naturally cooling, adding water with the mass of 50 percent of the limestone into the cooled limestone particles for dissolving, putting the dissolved water into mixing equipment, mixing limestone particles with a water body at a rotating speed of 400 revolutions per minute to form a mixed solution, and after the mixed solution is changed into the mixed solution, can be led out from the mixing equipment, the mixed solution is fully ground by the grinding equipment, the finished product after grinding flows out from the grinding equipment, then, the lime turbid liquid can be concentrated and purified to prepare lime milk solution.
And then, introducing the lime milk solution into a high-speed centrifuge, performing multi-stage centrifugal rotation separation at the rotating speed of 12000 rpm, removing undissolved particulate matters and impurity particles carried in the lime milk solution, and leading the separated solution out of the high-speed centrifuge to obtain a refined lime milk suspension with a certain concentration.
And then putting the refined lime milk suspension into a sealing device, adding saturated carbon dioxide gas into the sealing device, adding 5% of a crystal form control agent, effectively controlling the crystal shape of the nano calcium carbonate by controlling the solution amount of the crystal form control agent, and heating the nano calcium carbonate at a high temperature of 1000 ℃ in an air-isolated environment to conveniently concentrate the nano calcium carbonate, thereby preparing the concentrated lime milk solution.
And then placing the concentrated lime milk solution into a high-temperature furnace to be dehydrated and dried at the high temperature of 800 ℃ so that the lime milk solution is gradually changed into powder, and grinding the dehydrated and dried lime milk to obtain the lime milk powder.
Then, the lime milk powder can be put into the mixing equipment, 2.5% of modified high-molecular ionic polymer is added into the mixing equipment, the surface treatment of the particles of the lime milk powder can be conveniently carried out, the surface treatment effect of the lime milk powder can be controlled by controlling the addition amount of the modified high-molecular ionic polymer, and then the finished lime milk powder is collected, so that the nano calcium carbonate can be obtained.
Then 2.5 percent of coconut oil, 1.5 percent of silicic acid and 1 percent of arbitrary acid are added into the nano calcium carbonate, 1.5 percent of oleic acid is used as an adhesive, the mixture is injected into stirring equipment, meanwhile, the adhesive and the nano calcium carbonate are fully stirred and mixed at the rotating speed of 1200 r/min, and the high-viscosity nano calcium carbonate can be obtained after the finished product is stirred.
Example two:
the process flow is that-quantitative quick lime is mixed according to the water cement ratio of 8: 1 in the proportion of the calcium hydroxide suspension, placing the calcium hydroxide suspension in hot water of 80 ℃ for mixed digestion at a speed of 600 revolutions per minute, collecting and taking out the solution after digestion to obtain a crude calcium hydroxide solution, then placing the crude calcium hydroxide solution in a holding device for standing and aging for 24 hours, adding carbon dioxide into the calcium hydroxide suspension after purification is finished, wherein the amount of the introduced carbon dioxide is 10-20% of the volume of a semi-finished calcium hydroxide suspension, sieving the calcium hydroxide solution by using a 400-mesh sieve while slowly introducing CO2, and fully mixing and stirring to obtain the refined calcium hydroxide slurry.
Putting the refined calcium hydroxide slurry into a glass reactor, adding 5% of additive, carbonizing the refined calcium hydroxide slurry according to the carbonization temperature of 1000 ℃ and the rotation speed of 800 rpm, then introducing sufficient mixed gas of carbon dioxide and nitrogen or pure carbon dioxide gas into the glass reactor by using a rotameter, starting carbonization reaction in the glass reactor, detecting the pH of the calcium hydroxide slurry in the carbonization reaction process, continuing high-temperature carbonization for 15 minutes after the pH is detected to be acidic, namely the pH value is reduced to below 7, obtaining nano calcium carbonate solution, naturally cooling the obtained slurry, heating the slurry to 80 ℃ again after the slurry is completely cooled, adding 5% of sodium stearate, and keeping the temperature for 2 hours, and then, sieving and filtering the slurry by using a 600-mesh sieve, drying the slurry at the high temperature of 800 ℃ again, crushing the blocky calcium hydroxide solid after drying, and crushing to obtain the nano calcium carbonate solid.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (9)
1. An industrial preparation method for improving the affinity of nano calcium carbonate for an adhesive is characterized in that the nano calcium carbonate takes limestone as a raw material and is calcined at high temperature, meanwhile, water is added into the calcined limestone as a solvent to be dissolved, then grinding is carried out to obtain lime milk, and finally, the nano calcium carbonate is obtained by purification;
the method comprises the following steps: putting large limestone into equipment for full crushing, adding water, and fusing with crushed limestone to obtain lime milk;
step two: carrying out multi-stage hydrocyclone separation on the lime milk to remove particles and impurities carried in the lime milk to obtain refined lime milk suspension with a certain concentration;
step three: then adding carbon dioxide gas into the lime milk suspension, adding a crystal form control agent, controlling the crystal shape of the nano calcium carbonate, starting carbonization, and concentrating the lime milk solution;
step four: dehydrating and drying the concentrated lime milk solution to obtain lime milk powder;
step five: adding a reagent into the lime milk powder for surface treatment to obtain nano calcium carbonate;
step six: adding adhesive into the nano calcium carbonate to obtain the high-viscosity nano calcium carbonate.
2. The industrial preparation method for improving the affinity of the nano calcium carbonate for the adhesive according to claim 1, which is characterized in that: the nano calcium carbonate comprises the following components in percentage by mass: the proportion of lime milk is 95 percent, and the whole mass of each group of reagents is 5 percent.
3. The industrial preparation method for improving the affinity of the nano calcium carbonate for the adhesive according to claim 1, which is characterized in that: the calcining temperature of the limestone is 1200 ℃, and the temperature of the water body is 20 ℃.
4. The industrial preparation method for improving the affinity of the nano calcium carbonate for the adhesive according to claim 1, which is characterized in that: in the step 1, large limestone is crushed in advance, then the large limestone can be calcined, meanwhile, calcined limestone is added with water to be dissolved to form a mixed solution, after the mixed solution is changed into the mixed solution, external equipment can be used for grinding the mixed solution to obtain limestone turbid liquid, and the limestone turbid liquid is extracted to prepare the lime milk.
5. The industrial preparation method for improving the affinity of the nano calcium carbonate for the adhesive according to claim 1, which is characterized in that: and 2, performing multi-stage centrifugal separation on the obtained lime milk through a centrifugal machine to remove impurities and fine particles carried in the lime milk, and sieving the lime milk through a 200-mesh sieve to obtain a refined lime milk suspension with a certain concentration and after impurity removal.
6. The industrial preparation method for improving the affinity of the nano calcium carbonate for the adhesive according to claim 1, which is characterized in that: and 3, adding 75% concentration carbon dioxide into the refined lime milk suspension liquid after impurity removal, simultaneously adding 2% of proper crystal form control agent into the refined lime milk suspension liquid, controlling the crystal shape generated by the subsequent nano calcium carbonate reaction by controlling the dosage of the added crystal form control agent, and carbonizing the refined lime milk suspension liquid by oxygen-free high-temperature heating, thereby concentrating the refined lime milk suspension liquid.
7. The industrial preparation method for improving the affinity of the nano calcium carbonate for the adhesive according to claim 1, which is characterized in that: and 4, deoxidizing and drying the concentrated lime milk suspension at high temperature at 1000 ℃, dehydrating, and grinding to obtain lime milk powder.
8. The industrial preparation method for improving the affinity of the nano calcium carbonate for the adhesive according to claim 1, which is characterized in that: and 5, adding a modified high-molecular ionic polymer into the lime milk powder, and performing surface treatment on the lime milk powder particles to obtain the nano calcium carbonate.
9. The industrial preparation method for improving the affinity of the nano calcium carbonate for the adhesive according to claim 1, which is characterized in that: and sixthly, after the extraction of the nano calcium carbonate is finished, adding a proper amount of 2 percent of adhesive into the nano calcium carbonate, and fully vibrating and mixing to obtain the nano calcium carbonate with improved adhesiveness.
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| CN107555459A (en) * | 2017-09-13 | 2018-01-09 | 泰兴市诚盛化工有限公司 | A kind of preparation method of nanometer of spindle winnofil |
| CN108727872A (en) * | 2018-06-01 | 2018-11-02 | 芜湖卓越纳米新材料股份有限公司 | A kind of preparation process of the special low oil factor nano-calcium carbonate of adhesive |
| CN109650430A (en) * | 2018-12-20 | 2019-04-19 | 广西华纳新材料科技有限公司 | A kind of method of high content of magnesium lime stone preparation nanometer calcium carbonate |
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2020
- 2020-06-18 CN CN202010557480.7A patent/CN111909539A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475199A (en) * | 2009-01-21 | 2009-07-08 | 山东海泽纳米材料有限公司 | Industrial preparation of calcium carbonate nano bead string |
| CN102701255A (en) * | 2012-06-21 | 2012-10-03 | 石家庄市红日钙业有限公司 | Method for high-concentration carbonization production of spherical nano calcium carbonate |
| CN104477961A (en) * | 2014-12-22 | 2015-04-01 | 南通市飞宇精细化学品有限公司 | Preparation method of high-purity fine calcium carbonate |
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| CN107555459A (en) * | 2017-09-13 | 2018-01-09 | 泰兴市诚盛化工有限公司 | A kind of preparation method of nanometer of spindle winnofil |
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