CN112340761A - Preparation process of calcium carbonate compound particles - Google Patents
Preparation process of calcium carbonate compound particles Download PDFInfo
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- CN112340761A CN112340761A CN202011076524.0A CN202011076524A CN112340761A CN 112340761 A CN112340761 A CN 112340761A CN 202011076524 A CN202011076524 A CN 202011076524A CN 112340761 A CN112340761 A CN 112340761A
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- calcium carbonate
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- carbon dioxide
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 95
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 65
- -1 calcium carbonate compound Chemical class 0.000 title claims abstract description 36
- 239000002245 particle Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 54
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 49
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 31
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 27
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 27
- 238000001035 drying Methods 0.000 claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000292 calcium oxide Substances 0.000 claims abstract description 18
- 235000012255 calcium oxide Nutrition 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 16
- 239000013078 crystal Substances 0.000 claims abstract description 13
- RCJMVGJKROQDCB-UHFFFAOYSA-N 2-methylpenta-1,3-diene Chemical group CC=CC(C)=C RCJMVGJKROQDCB-UHFFFAOYSA-N 0.000 claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229920001661 Chitosan Polymers 0.000 claims abstract description 11
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003365 glass fiber Substances 0.000 claims abstract description 11
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 11
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims abstract description 11
- 238000010000 carbonizing Methods 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 239000000839 emulsion Substances 0.000 claims abstract description 8
- 238000004537 pulping Methods 0.000 claims abstract description 8
- 229920001909 styrene-acrylic polymer Polymers 0.000 claims abstract description 8
- 238000003763 carbonization Methods 0.000 claims description 28
- 239000002002 slurry Substances 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 27
- 238000001914 filtration Methods 0.000 claims description 26
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 23
- 239000000920 calcium hydroxide Substances 0.000 claims description 23
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 23
- 239000007789 gas Substances 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 238000009423 ventilation Methods 0.000 claims description 9
- 230000032683 aging Effects 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 230000029087 digestion Effects 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 238000011085 pressure filtration Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 230000007547 defect Effects 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 11
- 239000000243 solution Substances 0.000 description 10
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 4
- 235000011941 Tilia x europaea Nutrition 0.000 description 4
- 239000004571 lime Substances 0.000 description 4
- 239000008267 milk Substances 0.000 description 4
- 210000004080 milk Anatomy 0.000 description 4
- 235000013336 milk Nutrition 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 235000019738 Limestone Nutrition 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 230000003712 anti-aging effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000006028 limestone Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229920001944 Plastisol Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- RHZUVFJBSILHOK-UHFFFAOYSA-N anthracen-1-ylmethanolate Chemical compound C1=CC=C2C=C3C(C[O-])=CC=CC3=CC2=C1 RHZUVFJBSILHOK-UHFFFAOYSA-N 0.000 description 1
- 239000003830 anthracite Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 239000004999 plastisol Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Classifications
-
- 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
- C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
-
- 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
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
-
- 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
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
- C01F11/183—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds the additive being an organic compound
-
- 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
- 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
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Health & Medical Sciences (AREA)
- Carbon And Carbon Compounds (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparation process of calcium carbonate compound particles, which comprises the steps of 1, pulping, 2, carbonizing, 3, treating agent, 4, secondary carbonizing and 5, drying the finished product; the composition comprises the following components in parts by weight: 50-80 parts of quicklime; 2-5 parts of a crystal form control agent; 1-2 parts of graphene; 0.5-1 part of chitosan; 1-2 parts of glass fiber; 1-2 parts of sodium stearate; 1-2 parts of aluminum silicate; 1-2 parts of 2-propenyl propylene; 1-2 parts of styrene-acrylic emulsion; the auxiliary materials are as follows: carbon dioxide; methanol or ethanol solution; and (3) water. The calcium carbonate compound particles prepared by the invention have the characteristics of simple process, good effect and wide application range, and effectively overcome the defects of the prior art.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a preparation process of calcium carbonate compound particles.
Background
During or after the generation of the calcium carbonate, various additives are added, so that the calcium carbonate is modified, coated, mixed and the like to form new compound particles, and the new calcium carbonate compound particles have better tensile, compression, adsorption, whiteness and other properties and are widely applied to the fields of plastics, coatings, foods, cosmetics and the like.
Application publication No.: 110028094A, discloses a method for producing high thixotropy active nano calcium carbonate, which comprises the following steps: s1, calcining limestone and anthracite to obtain quicklime and kiln gas, and then digesting the quicklime to obtain lime milk; s2, aging and diluting the lime milk, pumping the lime milk into a carbonization tower, adding a crystal form control agent and a dispersing agent before carbonization reaction, and uniformly stirring; s3, carbonizing the lime milk by taking the kiln gas obtained in the S1 as a gas source of carbonization reaction to obtain calcium carbonate slurry; s4, pumping the calcium carbonate slurry into an activation tank, preparing the surface treating agent into an aqueous solution, and adding the aqueous solution into the activation tank for coating treatment; and S5, carrying out filter pressing on the coated calcium carbonate slurry, drying and crushing to obtain the high-thixotropy active nano calcium carbonate.
Application publication No.: 108948794A, discloses a method for preparing nano calcium carbonate for PVC plastisol, which comprises the steps of calcining limestone with the main content of more than or equal to 98 percent, digesting, aging at high temperature, adding a crystal nucleus formation control agent, and carbonizing to obtain nano calcium carbonate slurry; adding a surface treating agent compounded in advance into calcium carbonate slurry to enable the surface treating agent to be in full contact with the calcium carbonate slurry, wherein the compounded surface treating agent comprises the following components in percentage by mass: castor oil phosphate ester: emulsifier: H2O = 40-55: 40-60: 6-10: 100 and 200; filtering, drying, pulverizing, and sieving to obtain the final product.
The calcium carbonate particles prepared by the scheme are brittle, poor in impact toughness, high in oil absorption value, high in plasticizer consumption and poor in impact toughness of the product.
Disclosure of Invention
The invention aims to solve the technical problems of poor performance and inconvenient use of calcium carbonate compound particles, and provides a preparation process of calcium carbonate compound particles to overcome the defects of the prior art.
In order to achieve the above object, the present invention comprises the following solutions:
a preparation process of calcium carbonate compound particles comprises the steps of 1, pulping, 2, carbonizing, 3, treating agent, 4, secondary carbonizing and 5, drying finished products;
the composition comprises the following components in parts by weight:
50-80 parts of quicklime; 2-5 parts of a crystal form control agent; 1-2 parts of graphene; 0.5-1 part of chitosan; 1-2 parts of glass fiber; 1-2 parts of sodium stearate; 1-2 parts of aluminum silicate; 1-2 parts of 2-propenyl propylene; 1-2 parts of styrene-acrylic emulsion; the auxiliary materials are as follows: carbon dioxide; methanol or ethanol solution; and (3) water.
Specifically, in the step 1, pulping is carried out, calcined quicklime with the impurity content less than 3% is selected, and water and the quicklime are mixed according to the mass ratio of 10: 1, carrying out digestion reaction, then aging for at least 18 hours, sieving by a 200-mesh sieve to obtain calcium hydroxide coarse pulp, adding water into the calcium hydroxide coarse pulp, and continuously stirring the mixture in the water to prepare calcium hydroxide slurry with the concentration of 5 percent;
step 2, carbonization, namely adding the calcium hydroxide slurry obtained in the step 1 into a reaction kettle, heating to 40 ℃, adding a crystal form control agent, and continuously stirring at the stirring speed of 240-; introducing carbon dioxide gas to carry out carbonization reaction, and reducing the stirring rotating speed to 120-180r/min and the pressure to 0.02 MPa; when the pH value is reduced to 8.5, adding chitosan and sodium stearate, continuously introducing carbon dioxide gas, carrying out carbonization reaction, and when the pH value is reduced to 7, carrying out centrifugal filtration to prepare a calcium carbonate wet material with the water content of 300%;
step 3, a treating agent is prepared by uniformly mixing the graphene, the glass fiber, the aluminum silicate and the 2-propenyl propylene with 500 times of water in parts by weight of 350-;
step 4, secondary carbonization, namely mixing the wet calcium carbonate material obtained in the step 2 with the treating agent obtained in the step 3, uniformly stirring, heating to 60 ℃, adjusting the pressure to 0.6 MPa, and then introducing carbon dioxide to perform secondary carbonization; stopping the reaction after 1-3 hours, filtering and drying the calcium carbonate slurry, performing centrifugal filtration, then performing pressure filtration on the solid substance, and controlling the water content ratio to be below 60% to obtain wet compound calcium carbonate;
and 5, drying the finished product, cleaning and filtering the wet compound calcium carbonate by using an ethanol solution with the mass fraction of 30%, repeating for 2-3 times, cleaning and filtering by using clean water again, repeating for 1-2 times, spraying, granulating, and drying at the drying temperature of 90-100 ℃ to obtain the calcium carbonate compound particles.
Furthermore, in the step 2, the ventilation volume is not less than 0.2 cubic meter per second calculated by 1000L of calcium hydroxide slurry, and the ventilation volume after the ventilation volume is reduced is 5-10% of the normal value; the introduced gas is a mixed gas of carbon dioxide and nitrogen, and the content of carbon dioxide is not less than 40%.
Further, in the step 5, the cleaned calcium carbonate slurry is sprayed, dried and granulated, the water content of the sprayed particles is 15-20%, and then the particles are placed in a dryer to be continuously dried until the water content is less than 0.3%.
The calcium carbonate compound particles prepared by the invention have the characteristics of simple process, good effect and wide application range, and effectively overcome the defects of the prior art.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below, and it is obvious that the embodiments described below are some, but not all embodiments of the present invention in the description of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Embodiment 1, a preparation process of calcium carbonate compound particles, comprising the steps of 1, pulping, 2, carbonizing, 3, treating agent, 4, secondary carbonizing, and 5, drying the finished product;
the composition comprises the following components in parts by weight:
50-80 parts of quicklime; 2-5 parts of a crystal form control agent; 1-2 parts of graphene; 0.5-1 part of chitosan; 1-2 parts of glass fiber; 1-2 parts of sodium stearate; 1-2 parts of aluminum silicate; 1-2 parts of 2-propenyl propylene; 1-2 parts of styrene-acrylic emulsion; the auxiliary materials are as follows: carbon dioxide; methanol or ethanol solution; and (3) water.
Specifically, in the step 1, pulping is carried out, calcined quicklime with the impurity content less than 3% is selected, and water and the quicklime are mixed according to the mass ratio of 10: 1, carrying out digestion reaction, then aging for at least 18 hours, sieving by a 200-mesh sieve to obtain calcium hydroxide coarse pulp, adding water into the calcium hydroxide coarse pulp, and continuously stirring the mixture in the water to prepare calcium hydroxide slurry with the concentration of 5 percent;
step 2, carbonization, namely adding the calcium hydroxide slurry obtained in the step 1 into a reaction kettle, heating to 40 ℃, adding a crystal form control agent, and continuously stirring at the stirring speed of 240-; introducing carbon dioxide gas to carry out carbonization reaction, and reducing the stirring rotating speed to 120-180r/min and the pressure to 0.02 MPa; when the pH value is reduced to 8.5, adding chitosan and sodium stearate, continuously introducing carbon dioxide gas, carrying out carbonization reaction, and when the pH value is reduced to 7, carrying out centrifugal filtration to prepare a calcium carbonate wet material with the water content of 300%;
step 3, a treating agent is prepared by uniformly mixing the graphene, the glass fiber, the aluminum silicate and the 2-propenyl propylene with 500 times of water in parts by weight of 350-;
step 4, secondary carbonization, namely mixing the wet calcium carbonate material obtained in the step 2 with the treating agent obtained in the step 3, uniformly stirring, heating to 60 ℃, adjusting the pressure to 0.6 MPa, and then introducing carbon dioxide to perform secondary carbonization; stopping the reaction after 1-3 hours, filtering and drying the calcium carbonate slurry, performing centrifugal filtration, then performing pressure filtration on the solid substance, and controlling the water content ratio to be below 60% to obtain wet compound calcium carbonate;
and 5, drying the finished product, cleaning and filtering the wet compound calcium carbonate by using an ethanol solution with the mass fraction of 30%, repeating for 2-3 times, cleaning and filtering by using clean water again, repeating for 1-2 times, spraying, granulating, and drying at the drying temperature of 90-100 ℃ to obtain the calcium carbonate compound particles.
In the step 2, the ventilation volume is not less than 0.2 cubic meter per second calculated by 1000L of calcium hydroxide slurry, and the ventilation volume after the ventilation volume is reduced is 5-10% of the normal value; the introduced gas is a mixed gas of carbon dioxide and nitrogen, and the content of carbon dioxide is not less than 40%.
And 5, spraying, drying and granulating the cleaned calcium carbonate slurry, wherein the water content of the sprayed particles is 15-20%, and then placing the particles in a dryer to continuously dry until the water content is less than 0.3%.
Embodiment 2, the calcium carbonate compound granule comprises the following components in parts by weight:
50 parts of quicklime; 2 parts of a crystal form control agent; 1 part of graphene; 0.5 part of chitosan; 1 part of glass fiber; 2 parts of sodium stearate; 1 part of aluminum silicate; 1 part of 2-propenyl propylene; 1 part of styrene-acrylic emulsion; the auxiliary materials are as follows: carbon dioxide; methanol or ethanol solution; and (3) water.
Specifically, in the step 1, pulping is carried out, calcined quicklime with the impurity content less than 3% is selected, and water and the quicklime are mixed according to the mass ratio of 10: 1, carrying out digestion reaction, then aging for at least 18 hours, sieving by a 200-mesh sieve to obtain calcium hydroxide coarse pulp, adding water into the calcium hydroxide coarse pulp, and continuously stirring the mixture in the water to prepare calcium hydroxide slurry with the concentration of 5 percent;
step 2, carbonization, namely adding the calcium hydroxide slurry obtained in the step 1 into a reaction kettle, heating to 40 ℃, adding a crystal form control agent, and continuously stirring at the stirring speed of 240 r/min; introducing carbon dioxide gas, carrying out carbonization reaction, and reducing the stirring speed to 180r/min and the pressure to 0.02 MPa; when the pH value is reduced to 8.5, adding chitosan and sodium stearate, continuously introducing carbon dioxide gas, carrying out carbonization reaction, and when the pH value is reduced to 7, carrying out centrifugal filtration to prepare a calcium carbonate wet material with the water content of 300%;
step 3, uniformly mixing graphene, glass fiber, aluminum silicate and 2-propenyl propylene with 500 times of water by weight, heating the suspension to 60 ℃, adding styrene-acrylic emulsion, and uniformly stirring;
step 4, secondary carbonization, namely mixing the wet calcium carbonate material obtained in the step 2 with the treating agent obtained in the step 3, uniformly stirring, heating to 60 ℃, adjusting the pressure to 0.6 MPa, and then introducing carbon dioxide to perform secondary carbonization; stopping the reaction after 3 hours, filtering and drying the calcium carbonate slurry, performing centrifugal filtration, and then performing pressure filtration on the solid substance to control the water content ratio to be below 60% to obtain wet compound calcium carbonate;
and 5, drying the finished product, cleaning and filtering the wet compound calcium carbonate by using an ethanol solution with the mass fraction of 30%, repeating for 2 times, cleaning and filtering again by using clean water according to the above steps, repeating for 2 times, spraying and granulating, and drying at the drying temperature of 90 ℃ until the water content is less than 0.5% to obtain the calcium carbonate compound particles.
Example 3 PVC parts made with this additive were compared to prior art tensile tests and are shown in Table 1.
TABLE 1
| Product(s) | Tensile strength at break | Elongation at break | Heat variability (130-30 seconds) |
| Example 2 | 12MPa | 355% | Without change |
| Prior Art | 10.5MPa | 390% | Slight melting and collapse of corners |
As can be seen from the table above, the plastic product adopting the calcium carbonate compound particles has higher strength and better heat resistance.
Example 4 rubber parts made with this additive were compared to prior art tensile tests and are shown in table 2.
TABLE 2
| Product(s) | Tensile strength at break | Elongation at break | Thermal shrinkage factor (95 ℃ -3 h) | Tensile set |
| Example 2 | 21.2MPa | 425% | ≤0.1% | 0.55% |
| Prior Art | 20.5MPa | 410% | 0.15% | 0.8% |
As can be seen from Table 2, the rubber product prepared by using the calcium carbonate compound particles has higher strength, better heat resistance and better elasticity than the prior art.
Example 6, the calcium carbonate compound granule comprises the following components in parts by weight:
50 parts of quicklime; 2 parts of a crystal form control agent; 1 part of graphene; 0.5 part of chitosan; 1 part of glass fiber; 2 parts of sodium stearate; 1 part of aluminum silicate; 1 part of 2-propenyl propylene; 1 part of styrene-acrylic emulsion; 1 part of an anti-aging agent; 2 parts of ammonium salt; the auxiliary materials are as follows: carbon dioxide; methanol or ethanol solution; and (3) water.
Specifically, in the step 1, pulping is carried out, calcined quicklime with the impurity content less than 3% is selected, and water and the quicklime are mixed according to the mass ratio of 10: 1, carrying out digestion reaction, then aging for at least 18 hours, sieving by a 200-mesh sieve to obtain calcium hydroxide coarse pulp, adding water into the calcium hydroxide coarse pulp, and continuously stirring the mixture in the water to prepare calcium hydroxide slurry with the concentration of 5 percent;
step 2, carbonization, namely adding the calcium hydroxide slurry obtained in the step 1 into a reaction kettle, heating to 40 ℃, adding a crystal form control agent, and continuously stirring at the stirring speed of 240 r/min; introducing carbon dioxide gas, carrying out carbonization reaction, and reducing the stirring speed to 180r/min and the pressure to 0.02 MPa; when the pH value is reduced to 8.5, adding chitosan and sodium stearate, continuously introducing carbon dioxide gas, carrying out carbonization reaction, and when the pH value is reduced to 7, carrying out centrifugal filtration to prepare a calcium carbonate wet material with the water content of 300%;
step 3, uniformly mixing graphene, glass fiber, aluminum silicate and 2-propenyl propylene with 500 times of water by weight, heating the suspension to 60 ℃, adding styrene-acrylic emulsion, an anti-aging agent and ammonium salt, and uniformly stirring;
step 4, secondary carbonization, namely mixing the wet calcium carbonate material obtained in the step 2 with the treating agent obtained in the step 3, uniformly stirring, heating to 60 ℃, adjusting the pressure to 0.6 MPa, and then introducing carbon dioxide to perform secondary carbonization; stopping the reaction after 3 hours, filtering and drying the calcium carbonate slurry, performing centrifugal filtration, and then performing pressure filtration on the solid substance to control the water content ratio to be below 60% to obtain wet compound calcium carbonate;
and 5, drying the finished product, cleaning and filtering the wet compound calcium carbonate by using an ethanol solution with the mass fraction of 30%, repeating for 2 times, cleaning and filtering again by using clean water according to the above steps, repeating for 2 times, spraying and granulating, and drying at the drying temperature of 90 ℃ until the water content is less than 0.5% to obtain the calcium carbonate compound particles.
The calcium carbonate compound particles prepared by the invention have the characteristics of simple process, good effect and wide application range, and effectively overcome the defects of the prior art.
The embodiments described above are some, but not all embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (4)
1. A preparation process of calcium carbonate compound particles comprises the steps of 1, pulping, 2, carbonizing, 3, treating agent, 4, secondary carbonizing and 5, drying finished products;
the composition comprises the following components in parts by weight:
50-80 parts of quicklime; 2-5 parts of a crystal form control agent; 1-2 parts of graphene; 0.5-1 part of chitosan; 1-2 parts of glass fiber; 1-2 parts of sodium stearate; 1-2 parts of aluminum silicate; 1-2 parts of 2-propenyl propylene; 1-2 parts of styrene-acrylic emulsion; the auxiliary materials are as follows: carbon dioxide; methanol or ethanol solution; and (3) water.
2. The preparation process of the calcium carbonate compound particles as claimed in claim 1, which is characterized in that in the step 1, slurry is prepared, calcined quicklime with the impurity content less than 3% is selected, and water and the quicklime are mixed according to the mass ratio of 10: 1, carrying out digestion reaction, then aging for at least 18 hours, sieving by a 200-mesh sieve to obtain calcium hydroxide coarse pulp, adding water into the calcium hydroxide coarse pulp, and continuously stirring the mixture in the water to prepare calcium hydroxide slurry with the concentration of 5 percent;
step 2, carbonization, namely adding the calcium hydroxide slurry obtained in the step 1 into a reaction kettle, heating to 40 ℃, adding a crystal form control agent, and continuously stirring at the stirring speed of 240-; introducing carbon dioxide gas to carry out carbonization reaction, and reducing the stirring rotating speed to 120-180r/min and the pressure to 0.02 MPa; when the pH value is reduced to 8.5, adding chitosan and sodium stearate, continuously introducing carbon dioxide gas, carrying out carbonization reaction, and when the pH value is reduced to 7, carrying out centrifugal filtration to prepare a calcium carbonate wet material with the water content of 300%;
step 3, a treating agent is prepared by uniformly mixing the graphene, the glass fiber, the aluminum silicate and the 2-propenyl propylene with 500 times of water in parts by weight of 350-;
step 4, secondary carbonization, namely mixing the wet calcium carbonate material obtained in the step 2 with the treating agent obtained in the step 3, uniformly stirring, heating to 60 ℃, adjusting the pressure to 0.6 MPa, and then introducing carbon dioxide to perform secondary carbonization; stopping the reaction after 1-3 hours, filtering and drying the calcium carbonate slurry, performing centrifugal filtration, then performing pressure filtration on the solid substance, and controlling the water content ratio to be below 60% to obtain wet compound calcium carbonate;
and 5, drying the finished product, cleaning and filtering the wet compound calcium carbonate by using an ethanol solution with the mass fraction of 30%, repeating for 2-3 times, cleaning and filtering by using clean water again, repeating for 1-2 times, spraying, granulating, and drying at the drying temperature of 90-100 ℃ to obtain the calcium carbonate compound particles.
3. The process for preparing calcium carbonate compound particles as claimed in claim 2, wherein in the step 2, the ventilation amount is not less than 0.2 cubic meter per second calculated by 1000L of calcium hydroxide slurry, and the ventilation amount after the ventilation amount is reduced is 5-10% of the normal value; the introduced gas is a mixed gas of carbon dioxide and nitrogen, and the content of carbon dioxide is not less than 40%.
4. The preparation process of the calcium carbonate compound particles as claimed in claim 2, wherein in the step 5, the cleaned calcium carbonate slurry is sprayed, dried and granulated, the water content of the sprayed particles is 15-20%, and then the particles are placed in a dryer to be continuously dried until the water content is less than 0.3%.
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Application publication date: 20210209 |