CN111137914A - Method for preparing porous heavy calcium carbonate from artificial granite waste residues - Google Patents

Method for preparing porous heavy calcium carbonate from artificial granite waste residues Download PDF

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Publication number
CN111137914A
CN111137914A CN201911280334.8A CN201911280334A CN111137914A CN 111137914 A CN111137914 A CN 111137914A CN 201911280334 A CN201911280334 A CN 201911280334A CN 111137914 A CN111137914 A CN 111137914A
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China
Prior art keywords
calcium carbonate
artificial granite
heavy calcium
porous
porous heavy
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Pending
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CN201911280334.8A
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Chinese (zh)
Inventor
汤泉
莫福旺
黄玉洁
叶秋燕
韦金膂
黄娜
全婷君
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Hezhou University
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Hezhou University
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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09B—DISPOSAL OF SOLID WASTE
    • B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
    • B09B3/40—Destroying solid waste or transforming solid waste into something useful or harmless involving thermal treatment, e.g. evaporation
    • 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
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
    • C01P2006/65—Chroma (C*)

Abstract

The invention provides a method for preparing porous heavy calcium carbonate from artificial granite waste residues. And (3) putting the precursor and the crucible into a muffle furnace, calcining according to a heating system, and taking out after cooling to obtain the porous heavy calcium carbonate. The raw materials used in the method are waste residues of artificial granite and wastes of artificial granite enterprises, and the prepared porous heavy calcium carbonate has a large number of micro-holes on the surface, is porous, has a large specific surface area and is improved in whiteness.

Description

Method for preparing porous heavy calcium carbonate from artificial granite waste residues
Technical Field
The invention belongs to the technical field of surface treatment methods of nonmetallic minerals, and particularly relates to a method for preparing porous heavy calcium carbonate from artificial granite waste residues.
Background
The appearance, performance and application of the porous calcium carbonate are closely related to the preparation method and process thereof. At present, the methods frequently used for preparing porous calcium carbonate domestically and abroad include a template method, an emulsion membrane method, a coprecipitation method, a solution/hydrothermal method, a gel crystallization method, a salting-out method and the like. Different methods are adopted to obtain porous calcium carbonate particles with different shapes, and the particle size distribution of the porous calcium carbonate particles is approximately between 1 and 8 mu m. The porous calcium carbonate has the advantages of large specific surface area, stable property, controllable structure and the like, and is widely applied to the aspects of papermaking, biomacromolecule loading, drug slow release, super-hydrophobic surface construction, ceramics, bone repair and the like.
The artificial granite is prepared by mixing calcite, marble, limestone and the like serving as raw materials, unsaturated polyester resin serving as an adhesive, a proper amount of curing agent, diluent, accelerant and the like, stirring, performing vacuum compression molding, cutting and polishing. The artificial granite waste residue is produced by naturally drying a large amount of waste slurry generated in the cutting and polishing processes. Because the artificial granite is formed by vacuum pressing of calcium carbonate powder and unsaturated polyester resin, unsaturated double bonds in molecular chains of the unsaturated polyester resin and double bonds of a crosslinking monomer (usually styrene) are subjected to crosslinking polymerization reaction, and a three-dimensional network structure is formed by linear long-chain molecules, heavy calcium carbonate particles in the artificial granite are tightly coated by the three-dimensional network-shaped unsaturated polyester resin and then are cured, the structure is complex, and a low-cost method for separation and resource utilization is not available. Enterprises generally simply bury and stack in the open air, not only occupy a large amount of lands, but also generate a large amount of volatile organic compounds, cause secondary pollution to the environment, bring troubles to the sustainable development of the enterprises, and are also huge waste of resources. Therefore, the reasonable utilization and treatment of the waste residues are imperative, and the method is the only method for fundamentally solving the environmental pollution and reducing the land occupation and the potential safety hazard.
The existing research on porous calcium carbonate is basically prepared by taking light calcium carbonate as a raw material, and through search, although the patent on the porous calcium carbonate is not few, no technical scheme for preparing the porous heavy calcium carbonate by using artificial granite waste residue exists.
Disclosure of Invention
The invention aims to provide a method for preparing porous heavy calcium carbonate by using artificial granite waste residues aiming at the defects of the prior art. The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a method for preparing porous heavy calcium carbonate by using waste residues of artificial granite is characterized by comprising the following steps:
1. according to the solid-liquid ratio of 1: and 5, adding the sieved artificial granite waste residue into 15-30% sodium chloride solution, magnetically stirring for 10min, and placing in a cool and dry place for 24 hours. And pumping, drying, grinding uniformly, and then putting into a crucible for pretreatment to obtain a precursor. And (3) putting the precursor and the crucible into a muffle furnace, calcining according to a heating system, and taking out a sample after cooling to obtain the porous heavy calcium carbonate.
2. Preferably, the pretreatment is drying for 1-2 h on a universal electric furnace.
3. Preferably, the heating system is to heat up to 700-800 ℃ within 60-120 min, and then to keep the temperature for 200-270 min.
The invention has the beneficial effects that:
1. the raw materials used in the invention are artificial granite waste residues, which are wastes that can be comprehensively utilized by artificial granite enterprises without any method;
2. the process for preparing the porous heavy calcium carbonate is simple and is suitable for industrial production;
3. the porous heavy calcium carbonate has a large number of micro-pores on the surface, is porous, has a large specific surface area, and has improved whiteness. Compared with the artificial granite waste residue, the specific surface area is increased by 30-40%, and the whiteness is improved by 1-3 degrees.
Drawings
FIG. 1 is a scanning electron microscope image of artificial granite waste residue.
FIG. 2 is a scanning electron micrograph of the porous ground calcium carbonate of example 4 of the present invention.
FIG. 3 is an X-ray diffraction pattern of the artificial granite waste residue and the porous heavy calcium carbonate of example 4 of the present invention.
FIG. 4 is an infrared spectrum of the artificial granite waste residue and the porous ground calcium carbonate of example 4 of the present invention.
Detailed Description
The following further details the examples of the invention: it should be emphasized that the embodiments described herein are illustrative rather than restrictive, and thus the present invention is not limited to the embodiments described in the detailed description, but other embodiments derived from the technical solutions of the present invention by those skilled in the art are also within the scope of the present invention.
Through detection, the specific surface area of the raw material artificial granite waste residue is 1.95m2G, whiteness was 82.5 degrees.
Example 1
According to the solid-liquid ratio of 1: 5, adding the sieved artificial granite waste residue into a 30% sodium chloride solution, magnetically stirring for 10min, and placing in a cool and dry place for 24 hours. Pumping, drying, grinding, pre-treating in a crucible, and drying in a universal electric furnace for 1 hr to obtain the precursor. Putting the precursor and the crucible into a muffle furnace, and heating according to a heating system: heating to 700 ℃ within 60min, then calcining under the condition of keeping the temperature for 200min, and taking out a sample after cooling to obtain the porous heavy calcium carbonate. The detection proves that the specific surface area of the porous heavy calcium carbonate is 2.32m2Per g, the whiteness is 83.7 degrees.
Example 2
According to the solid-liquid ratio of 1: 5, adding the sieved artificial granite waste residue into a 30% sodium chloride solution, magnetically stirring for 10min, and placing in a cool and dry place for 24 hours. Pumping, drying, grinding, pre-treating in a crucible, and drying in a universal electric furnace for 1 hr to obtain the precursor. Putting the precursor and the crucible into a muffle furnace, and heating according to a heating system: heating to 700 ℃ within 60min, then calcining under the condition of keeping the temperature for 230min, and taking out a sample after cooling to obtain the porous heavy calcium carbonate. The detection proves that the specific surface area of the porous heavy calcium carbonate is 2.47m2G, whiteness was 84.7 degrees.
Example 3
According to the solid-liquid ratio of 1: 5, adding the sieved artificial granite waste residue into 15 percent sodium chloride solution, magnetically stirring for 10min, and placing in a cool and dry place for 24 hours. Warp pumpingFiltering, drying, grinding, pre-treating in crucible, and drying in universal electric furnace for 1.5 hr to obtain precursor. Putting the precursor and the crucible into a muffle furnace, and heating according to a heating system: heating to 700 ℃ within 120min, then calcining under the condition of keeping the temperature for 200min, and taking out a sample after cooling to obtain the porous heavy calcium carbonate. The specific surface area of the porous heavy calcium carbonate is detected to be 3.38m2(g), the whiteness is 85 degrees.
Example 4
According to the solid-liquid ratio of 1: 5, adding the sieved artificial granite waste residue into a 30% sodium chloride solution, magnetically stirring for 10min, and placing in a cool and dry place for 24 hours. Pumping, drying, grinding, pre-treating in a crucible, and drying in a universal electric furnace for 1.5 hr to obtain the precursor. Putting the precursor and the crucible into a muffle furnace, and heating according to a heating system: heating to 800 ℃ within 60min, then calcining under the condition of keeping the temperature for 200min, and taking out a sample after cooling to obtain the porous heavy calcium carbonate. The detection proves that the specific surface area of the porous heavy calcium carbonate is 4.21m2G, whiteness is 85.4 degrees.
Scanning electron microscope detection is carried out on the artificial granite waste residue and the porous heavy calcium carbonate prepared in example 4, and the results are shown in figure 1 and figure 2. As can be seen from figure 1, the surface of the artificial granite waste residue is flat and smooth, the structure is compact, and no holes exist; as can be seen from FIG. 2, the porous ground calcium carbonate prepared has a loose structure, a part of columnar calcium carbonate appears due to the calcination of the cured resin, and the surface has many fine pores and is porous, which are formed by the calcination of the organic matter in the artificial granite and the popping action of the added sodium chloride.
The results of X-ray diffraction measurements carried out on the artificial granite waste residue and the porous ground calcium carbonate prepared in example 4 are shown in FIG. 3. As can be seen from fig. 3, the prepared porous ground calcium carbonate has characteristic peaks of sodium chloride a and calcium carbonate b, indicating that sodium chloride has entered the crystal lattice of calcium carbonate, and calcium carbonate is a typical calcite crystal form.
The infrared spectroscopy of the artificial granite waste residue and the porous heavy calcium carbonate prepared in example 4 was performed, and the results are shown in fig. 4. As can be seen from FIG. 4, manyThe infrared absorption peaks of the porous heavy calcium carbonate and the artificial granite waste slag are approximately coincident. The waste residue of artificial granite and porous heavy calcium carbonate are 1796cm-1、1428cm-1、868cm-1、704cm-1All had obvious absorption peaks, control CaCO3The standard map of (1) shows a C-O stretching vibration peak at 1796cm-1 and a C-O stretching vibration peak at 1428cm-1Has C-O stretching vibration at 868cm-1With CO32-Bending vibration of (2), at 704cm-1And the main components of the artificial granite waste residue and the porous heavy calcium carbonate are calcium carbonate. At 1718cm-1The absorption peak is the double bond in the unsaturated resin, and the unsaturated resin becomes gas to volatilize in the calcining process, so the artificial granite waste residue has the absorption peak and the prepared porous heavy calcium carbonate does not have the absorption peak.

Claims (3)

1. A method for preparing porous heavy calcium carbonate by using waste residues of artificial granite is characterized by comprising the following steps: according to the solid-liquid ratio of 1: and 5, adding the sieved artificial granite waste residue into 15-30% sodium chloride solution, magnetically stirring for 10min, and placing in a cool and dry place for 24 hours. And pumping, drying, grinding uniformly, and then putting into a crucible for pretreatment to obtain a precursor. And (3) putting the precursor and the crucible into a muffle furnace, calcining according to a heating system, and taking out a sample after cooling to obtain the porous heavy calcium carbonate.
2. The method for preparing porous heavy calcium carbonate from the waste residue of the artificial granite according to claim 1, wherein the pretreatment is drying for 1-2 h on a universal electric furnace.
3. The method for preparing porous heavy calcium carbonate from the waste residue of the artificial granite according to claim 1, wherein the heating system is to heat up to 700-800 ℃ within 60-120 min, and then to preserve heat for 200-270 min.
CN201911280334.8A 2019-12-13 2019-12-13 Method for preparing porous heavy calcium carbonate from artificial granite waste residues Pending CN111137914A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113173735A (en) * 2021-06-15 2021-07-27 桂林理工大学 PBS (poly butylenes succinate)/artificial granite waste residue composite material and preparation method thereof
CN114273408A (en) * 2021-12-31 2022-04-05 广西康利岗石有限公司 Method for removing cured unsaturated resin from artificial granite waste residue
CN114644479A (en) * 2020-12-17 2022-06-21 秦皇岛晶维石材有限公司 High-strength curb produced by utilizing quartz stone solid waste and process method thereof
CN115872431A (en) * 2022-12-08 2023-03-31 广西贺源科技发展有限责任公司 Preparation method of formaldehyde high-adsorption porous calcium carbonate

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105195083A (en) * 2015-09-14 2015-12-30 贺州学院 Method for modifying ground calcium carbonate with sodium chloride to prepare heavy metal adsorbent
CN110052237A (en) * 2019-04-19 2019-07-26 贺州学院 A kind of preparation method of porous powdered whiting adsorbent material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105195083A (en) * 2015-09-14 2015-12-30 贺州学院 Method for modifying ground calcium carbonate with sodium chloride to prepare heavy metal adsorbent
CN110052237A (en) * 2019-04-19 2019-07-26 贺州学院 A kind of preparation method of porous powdered whiting adsorbent material

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114644479A (en) * 2020-12-17 2022-06-21 秦皇岛晶维石材有限公司 High-strength curb produced by utilizing quartz stone solid waste and process method thereof
CN113173735A (en) * 2021-06-15 2021-07-27 桂林理工大学 PBS (poly butylenes succinate)/artificial granite waste residue composite material and preparation method thereof
CN114273408A (en) * 2021-12-31 2022-04-05 广西康利岗石有限公司 Method for removing cured unsaturated resin from artificial granite waste residue
CN115872431A (en) * 2022-12-08 2023-03-31 广西贺源科技发展有限责任公司 Preparation method of formaldehyde high-adsorption porous calcium carbonate

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Application publication date: 20200512