CN105858698A - Preparing method for cambiform-magnesium-carbonate-coated-calcium-carbonate composite material - Google Patents
Preparing method for cambiform-magnesium-carbonate-coated-calcium-carbonate composite material Download PDFInfo
- Publication number
- CN105858698A CN105858698A CN201610237850.2A CN201610237850A CN105858698A CN 105858698 A CN105858698 A CN 105858698A CN 201610237850 A CN201610237850 A CN 201610237850A CN 105858698 A CN105858698 A CN 105858698A
- Authority
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- China
- Prior art keywords
- composite
- fusiform
- magnesium
- magnesium carbonate
- coated caco3
- Prior art date
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- 239000002131 composite material Substances 0.000 title claims abstract description 82
- 239000001095 magnesium carbonate Substances 0.000 title claims abstract description 50
- 229910000021 magnesium carbonate Inorganic materials 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 28
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title abstract description 31
- 229910000019 calcium carbonate Inorganic materials 0.000 title abstract description 17
- 229960003563 calcium carbonate Drugs 0.000 title abstract 3
- 229960001708 magnesium carbonate Drugs 0.000 title abstract 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 64
- 235000019441 ethanol Nutrition 0.000 claims abstract description 34
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims abstract description 32
- 238000005406 washing Methods 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000011777 magnesium Substances 0.000 claims abstract description 13
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 12
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 12
- 239000004202 carbamide Substances 0.000 claims abstract description 7
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 claims abstract description 7
- 239000011654 magnesium acetate Substances 0.000 claims abstract description 7
- 235000011285 magnesium acetate Nutrition 0.000 claims abstract description 7
- 229940069446 magnesium acetate Drugs 0.000 claims abstract description 7
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 47
- 239000012065 filter cake Substances 0.000 claims description 24
- 238000002360 preparation method Methods 0.000 claims description 17
- 239000000047 product Substances 0.000 claims description 17
- 239000011505 plaster Substances 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 159000000003 magnesium salts Chemical class 0.000 claims description 10
- 238000000746 purification Methods 0.000 claims description 10
- 238000001953 recrystallisation Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 230000002378 acidificating effect Effects 0.000 claims description 6
- 239000012670 alkaline solution Substances 0.000 claims description 6
- 235000013877 carbamide Nutrition 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 239000011575 calcium Substances 0.000 abstract description 7
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052791 calcium Inorganic materials 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 6
- 229920001971 elastomer Polymers 0.000 abstract description 5
- 239000005060 rubber Substances 0.000 abstract description 4
- 239000000654 additive Substances 0.000 abstract description 3
- 230000000996 additive effect Effects 0.000 abstract description 3
- 239000004033 plastic Substances 0.000 abstract description 3
- 229920003023 plastic Polymers 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 2
- 238000004079 fireproofing Methods 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract 3
- 229940095672 calcium sulfate Drugs 0.000 abstract 2
- 235000011132 calcium sulphate Nutrition 0.000 abstract 2
- 229910052602 gypsum Inorganic materials 0.000 abstract 2
- 239000010440 gypsum Substances 0.000 abstract 2
- 229960005069 calcium Drugs 0.000 abstract 1
- 229960000443 hydrochloric acid Drugs 0.000 abstract 1
- 235000011167 hydrochloric acid Nutrition 0.000 abstract 1
- 238000002386 leaching Methods 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- 235000014380 magnesium carbonate Nutrition 0.000 description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 239000000843 powder Substances 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 238000004483 ATR-FTIR spectroscopy Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- HHSPVTKDOHQBKF-UHFFFAOYSA-J calcium;magnesium;dicarbonate Chemical compound [Mg+2].[Ca+2].[O-]C([O-])=O.[O-]C([O-])=O HHSPVTKDOHQBKF-UHFFFAOYSA-J 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 235000007926 Craterellus fallax Nutrition 0.000 description 1
- 240000007175 Datura inoxia Species 0.000 description 1
- 244000043261 Hevea brasiliensis Species 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000000035 biogenic effect Effects 0.000 description 1
- 230000003592 biomimetic effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- ZDVLIXBJVNYNSW-UHFFFAOYSA-J calcium dimagnesium dicarbonate Chemical compound [Mg+2].C([O-])([O-])=O.[Ca+2].C([O-])([O-])=O.[Mg+2] ZDVLIXBJVNYNSW-UHFFFAOYSA-J 0.000 description 1
- FYHXNYLLNIKZMR-UHFFFAOYSA-N calcium;carbonic acid Chemical compound [Ca].OC(O)=O FYHXNYLLNIKZMR-UHFFFAOYSA-N 0.000 description 1
- XNEYCQMMVLAXTN-UHFFFAOYSA-N carbonic acid;magnesium Chemical compound [Mg].OC(O)=O XNEYCQMMVLAXTN-UHFFFAOYSA-N 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 230000009429 distress Effects 0.000 description 1
- 239000010459 dolomite Substances 0.000 description 1
- 229910000514 dolomite Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 239000000834 fixative Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 210000004211 gastric acid Anatomy 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 229910003471 inorganic composite material Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002681 magnesium compounds Chemical class 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920003052 natural elastomer Polymers 0.000 description 1
- 229920001194 natural rubber Polymers 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920000747 poly(lactic acid) Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000004626 polylactic acid Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 208000011580 syndromic disease Diseases 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000000606 toothpaste Substances 0.000 description 1
- 229940034610 toothpaste Drugs 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
-
- 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
- C01F5/00—Compounds of magnesium
- C01F5/24—Magnesium carbonates
-
- 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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX 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
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/45—Aggregated particles or particles with an intergrown morphology
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
- C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
Abstract
The invention discloses a preparing method for a cambiform-magnesium-carbonate-coated-calcium-carbonate composite material, and belongs to the technical field of material-chemistry inorganic nonmetallic materials. The preparing method of the composite material includes the following steps that desulphurization gypsum serves as a calcium source, and is reacted for 5 hours to 12 hours in a 0.5 M-6.0 M hydrochloric-acid solution system at the temperature of 100 DEG C to 160 DEG C and filtered, then filter liquid is recrystallized through ethyl alcohol, the recrystallized filter liquid is dried at the temperature of 55 DEG C to 85 DEG C, and a pure calcium-sulfate product is obtained; magnesium acetate serves as a magnesium source, and is reacted with the obtained calcium-sulfate product for 8 hours to 24 hours in a urea solution system at the temperature of 150 DEG C to 180 DEG C, ethyl alcohol serves as leaching liquid, washing is carried out at the room temperature, filtering is carried out, drying is carried out at the temperature of 55 DEG C to 85 DEG C, and the cambiform-magnesium-carbonate-coated-calcium-carbonate composite material is obtained. The method is simple in synthetic route and convenient to operate, secondary utilization of chemical-industry-waste desulphurization gypsum can be achieved, and the product can serve as an additive in the rubber industry, the plastic industry and the like, and can also serve as a preparing raw material of a heat-preservation fireproofing material.
Description
Technical field
The invention belongs to materials chemistry technical field of inorganic nonmetallic materials, relate to a kind of inorganic composite materials, more specifically relate to
And the preparation method of a kind of fusiform magnesium carbonate coated caco3 composite.
Background technology
Along with scientific and technological progress, the mankind are the most diversified to the requirement of material property, and homogenous material cannot meet higher demand,
Thus the superior composite of combination property gradually obtains the attention of scientific circles.Magnesium and calcium belong to alkaline-earth metal (group iia unit
Element), the physicochemical property of its compound is the most similar, the most very likely prepares composite as matrix material.
Magnesium carbonate is nontoxic, tasteless, in monocline crystalline phase or amorphous state, is a kind of important industrial or agricultural inorganic magnesium compound material.
Because of its special structure and physics, chemical property, it is often used as adiabatic and resistant to elevated temperatures fire proofing material, boiler and the insulation of pipeline
Material (low thermal conductivity and low heat capacity), and the adding of food, medicine, cosmetics, rubber, toothpaste, glass, ink etc.
Add agent, also act as magnesium elements compensation, gastric acid nertralizer, desiccant, colour fixative, carrier, anti-caking agent, foam metal
Foaming agent etc..But, although China is rich in minerals, and magnesium resource reserves position is at the forefront in the world, the production of magnesium salt goods but still in
Thick product preparatory phase, it is impossible to meet the demand of social development.The current industrially prepared most popular method of magnesium carbonate goods has
Two kinds: one is to be sintered into magnesium oxide with solid magnesium ore deposit (dolomite, magnesite), and then to its hydration process, then carbonization becomes
Target product.Two is to be raw material with salt and sea water, prepares magnesium carbonate goods by Method of Soda, ammonium carbonate method, ammonia-carbonizatin method etc..
Prepared product is different because of raw material, and method is totally different, and its quality and cost are the most different.Ammonium salt circulation method utilizes natural magnesium ore deposit (Pedicellus et Pericarpium Trapae
Magnesium ore deposit, shepardite) prepare the technique of magnesium carbonate and can substantially solve the waste problem of precipitant and solvent, belong to one and compare ring
The approach that border is friendly, but the method is the most not enough in terms of magnesium carbonate microscopic appearance regulation and control, needs to be improved further.Along with economy
Fast development, the production of magnesian gradually develops with miniaturization direction to industrialization, functionalization, and its market demand also exists
Increase year by year, thus the having special appearance concurrently and will cause the dense emerging of researcher with the magnesium carbonate goods of function of high added value
Interest.
As a kind of excellent inorganic additive and carrier, calcium carbonate is nontoxic, nonirritant and biocompatibility preferable, food,
The fields such as health, medicine, daily use chemicals, rubber, plastics, pottery, printing and papermaking have broad application prospects.Past more than ten
Year, the preparation of calcium carbonate and modification technology have had the development advanced by leaps and bounds, specifically include that Mechanical Method, microemulsion method, double decomposition,
The sedimentation method, coprecipitation, carbonizatin method and biomimetic synthesis (also known as template) etc..Its product function variation have also been obtained into
One step ground is explored, and Li Peihao have studied the bacteria-induction calcium carbonate growth repairing effect to distress in concrete by biogenic deposit method；
Guo Xiao side uses field test method to have studied the calcium carbonate impact on low accumulation corn growth Yu Metal uptake；Wu Baisheng is by starch
Mechanical property to polyethylene compound with calcium carbonate compares and evaluates；Wang Yanyan uses mechanochemical method to be prepared for carbonic acid
Calcium/titanium dioxide composite powder, improves the covering power of composite granule by interpolation iron oxide red or iron oxide black；Hu Zhibo will
Kieselguhr and ground calcium carbonate, as raw material, are prepared for kieselguhr/ground calcium carbonate composite humidity adjusting material with roasting method, and carry out
Moisture absorption dynamics research；It is multiple that Liu Zhitian utilizes direct blending and cladding process to be prepared for polypropylene/natural rubber/calcium carbonate superfine powder ternary
Condensation material, and have studied the mass fraction of elastomer and calcium carbonate to Mechanical Properties of PP and the impact of rheological behavior；Horse
Auspicious gorgeous employing co-rotating twin screw extruder is prepared for polylactic acid/nano calcium carbonate composite material, and has investigated its impact further
Intensity and the influence factor of hot strength.These new technology make calcium carbonate material have good economy, society and ring with application
Border benefit.But, the preparation method of most of materials not only complex operation step, reaction time is long, and consumes a large amount of electric energy
Or coal resources.
It is known that the kind of matrix material is most important on the impact of composite property, the different blend ratios of matrix material are also
The change of material microstructure can be caused, and then affect the overall performance of material.Therefore select the matrix material of adapted varieties, optimize
The blending ratio of matrix material, particularly important to preparing composite.And, utilize chemical industrial waste thing that resource is reclaimed, pure
Change, recycle, and then produce composite, cost can not only be reduced, improve raw material availability and economic benefit, also help
Environmental protection.Therefore, utilize industrial by-products desulfurated plaster for calcium source, by controlling reaction condition and technological parameter, open in conjunction with magnesium salt
Send the composite of novel special appearance and function to have and be of great significance.
Summary of the invention
The deficiency existed for prior art, the kind of horn of plenty composite, solve that material consumption and energy consumption be high, ecological disruption big with
The problem that environmental pollution is serious, the invention provides the preparation method of a kind of fusiform magnesium carbonate coated caco3 composite.Should
Method with desulfurated plaster for calcium source, ethyl alcohol recrystallization after acidifying, and then with magnesium salt for magnesium source, hydro-thermal in weakly alkaline solution system
Method prepares a kind of fusiform magnesium carbonate coated caco3 composite.The method technique is simple and convenient to operate, productivity is higher,
Its product can be as the additive of the industry such as rubber, plastics, and be also expected to become a kind of thermal insulation fire-resistant product prepares raw material.
For achieving the above object, the technical solution adopted in the present invention is as follows:
A kind of preparation method of fusiform magnesium carbonate coated caco3 composite, it comprises the steps of:
A. the purification of desulfurated plaster: desulfurated plaster stirring is added in the reactor containing acidic aqueous solution, is acidified under uniform temperature
Processing, be filtered to remove slightly solubility impurity, filtrate, with ethyl alcohol recrystallization, then carries out secondary filter, washing with alcohol, dried
To pure calcium sulfate product；
B. the preparation of composite: above-mentioned calcium sulfate product stirring after purification is added to the weakly alkaline solution containing magnesium salt,
It is cooled to room temperature under uniform temperature after hydro-thermal reaction, is filtrated to get composite filter cake；
C. washing: by the composite filter cake that is filtrated to get directly with washing with alcohol, or directly with washing with alcohol after drying；
D. it is dried: composite filter cake washing with alcohol crossed dries to obtain fusiform magnesium carbonate coated caco3 composite.
In described step A, the addition of desulfurated plaster is 25.0-200.0g/L, acidic aqueous solution H+Concentration is 0.5-6.0mol/L,
Souring temperature is 100.0-160.0 DEG C, and acidificatoin time is 5.0-12.0 hour.
The acid of described acidic aqueous solution is hydrochloric acid.
In described step B, calcium sulfate addition after purification is 12.5.0-30.0g/L, and the addition of magnesium salt is 15.0-50.0g/L,
In weakly alkaline solution, the concentration of alkalescence material is 30.0-100.0g/L, and hydrothermal temperature is 150.0-180.0 DEG C, during reaction
Between be 8.0-24.0 hour.
Described magnesium salt refers to magnesium acetate.
In described weakly alkaline solution, alkalescence material is carbamide.
In described step C, washing refers to that the composite filter cake being filtrated to get adds ethanol filtered at room temperature drip washing, or is filtrated to get
Composite filter cake 55.0-85.0 DEG C dry after add ethanol filtered at room temperature drip washing.
Described step D is dried and refers to that washed composite filter cake is spun through 55.0-85.0 DEG C of drying for 4.0-8.0 hour
Hammer shape magnesium carbonate coated caco3 composite.
Specific embodiment of the invention process is:
First, under room temperature, the concentrated hydrochloric acid of certain volume is diluted to the substance withdrawl syndrome acid as 0.5-6.0mol/L with deionized water
Property aqueous solution, in stirring add equivalent concentration 25.0-200.0g/L desulfurated plaster, at 100.0-160.0 DEG C by mixed liquor acid
Being cooled to room temperature after changing 5.0-12.0 hour, filter, filtrate is to carry out secondary filter after ethyl alcohol recrystallization, filter cake is with washing with alcohol
Pure calcium sulfate product it is dried to obtain at latter 55.0-85.0 DEG C；Secondly, the carbamide of certain mass is configured to matter with deionized water
Amount concentration is the weak alkaline aqueous solution of 30.0-100.0g/L, adds magnesium acetate and the equivalent concentration of equivalent concentration 15.0-50.0g/L
12.5.0-30.0g/L calcium sulfate product after purification, hydro-thermal reaction 8.0-24.0 hour at 150.0-180.0 DEG C, it is cooled to room temperature
Rear filtration, then by the composite filter cake that obtains directly with ethanol filtered at room temperature drip washing, or with second after drying at 55.0-85.0 DEG C
Alcohol filtered at room temperature drip washing；Finally, washed composite filter cake obtains spindle in 4.0-8.0 hour through 55.0-85.0 DEG C of drying
Shape magnesium carbonate coated caco3 composite.
The fusiform magnesium carbonate coated caco3 composite of the present invention, its surface is to be assembled by nanometer sheet.Fusiform carbonic acid
Magnesium coated caco3 composite is mainly made up of magnesium carbonate, calcium carbonate, magnesium calcium carbonate.
A kind of preparation method of the fusiform magnesium carbonate coated caco3 composite of the present invention, with desulfurated plaster for calcium source, acidifying
Rear ethyl alcohol recrystallization, and then with magnesium salt for magnesium source, in weakly alkaline water solution system, hydro-thermal method prepares a kind of fusiform carbon
Acid magnesium coated caco3 composite.Compared with prior art, the method synthetic route that the present invention provides is simple, easy to operate,
With short production cycle, productivity is higher, easily realizes industrialized production, and the fusiform magnesium carbonate coated caco3 composite of gained
Surface is made up of nano-sheet aggregation.
Accompanying drawing explanation
For more full and accurate the technical scheme stating this inventive embodiments, below embodiment is described used in accompanying drawing make simple
Introduce.Obviously, the accompanying drawing in below describing is only the accompanying drawing of some embodiments of the present invention, for those of ordinary skill in the art
From the point of view of, on the premise of not being put to creative work, also can obtain other accompanying drawing according to this type of accompanying drawing.
Fig. 1 is the whole synthetic route chart of the present invention a kind of fusiform magnesium carbonate coated caco3 composite；
Fig. 2 is the forming process schematic diagram of the present invention a kind of fusiform magnesium carbonate coated caco3 composite；
Fig. 3 is the electron scanning micrograph of the present invention a kind of fusiform magnesium carbonate coated caco3 composite；
Fig. 4 is the X-ray powder diagram of the present invention a kind of fusiform magnesium carbonate coated caco3 composite；
Fig. 5 is the Energy dispersive x-ray spectrogram of the present invention a kind of fusiform magnesium carbonate coated caco3 composite；
Fig. 6 is the attenuated total reflectance Fourier transform infrared spectroscopy of the present invention a kind of fusiform magnesium carbonate coated caco3 composite
Figure.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, those skilled in the art are made to be more fully understood that the present invention,
With embodiment, embodiments of the present invention are elaborated further below in conjunction with the accompanying drawings.
Embodiment 1
First, the concentrated hydrochloric acid (37.5wt%) of 41.7mL is configured to the deionized water of 458.3mL dilute salt of 1.0mol/L
Acid solution, adds the desulfurated plaster of equivalent concentration 50.0g/L, after mixed liquor is acidified 9.0 hours at 110.0 DEG C under stirring at normal temperature
Being cooled to room temperature, filter, filtrate is to carry out secondary filter after ethyl alcohol recrystallization, filter cake is dried at after washing with alcohol 60.0 DEG C
To pure calcium sulfate product；Secondly, the carbamide of 1.5g is configured to the mass concentration alkalescence as 30.0g/L with deionized water
Aqueous solution, the magnesium acetate of addition equivalent concentration 20.0g/L and the calcium sulfate product after purification of equivalent concentration 17.5g/L, 155.0 DEG C
Lower hydro-thermal reaction 12.0 hours, is cooled to after room temperature filter, then by the composite filter cake that obtains directly with ethanol filtered at room temperature
With ethanol filtered at room temperature drip washing after drying at drip washing, or 65.0 DEG C；Finally, washed composite filter cake is through 80.0 DEG C
Dry and within 4.5 hours, obtain fusiform magnesium carbonate coated caco3 composite.
The above-mentioned a kind of fusiform magnesium carbonate coated caco3 composite prepared is carried out microscopic appearance and Phase Structure Analysis,
Obtain result as seen in figures 3-6.Fig. 3 is the scanning electron microscope of this kind of fusiform magnesium carbonate coated caco3 composite
Photo, as shown in Figure 3: this composite is fusiform, surface is made up of nano-sheet aggregation.
Fig. 4 is the X-ray powder diagram of this kind of fusiform magnesium carbonate coated caco3 composite, as shown in Figure 4: this is multiple
Condensation material degree of crystallinity is higher, diffraction maximum 2 θ=32.4 °, peak position and the magnesium carbonate standard X-Ray powder of 2 θ=42.8 ° and 2 θ=53.5 °
The respective peaks peak position of diffraction spectrogram (JCPDF NO.86-2348) is coincide, diffraction maximum 2 θ=26.2 °, 2 θ=27.1 ° and 2 θ=33.1 °
The respective peaks peak position of peak position and calcium carbonate standard X-Ray powder diffraction spectrogram (JCPDF NO.41-1475) coincide, diffraction
θ=30.7 °, peak 2, peak position and magnesium calcium carbonate standard X-Ray powder diffraction spectrogram (the JCPDF NO. of 2 θ=41.0 ° and 2 θ=50.4 °
Respective peaks peak position 79-1342) is coincide.Visible, it is mainly made up of with magnesium calcium carbonate magnesium carbonate, calcium carbonate.
Fig. 5 is the Energy dispersive x-ray spectrogram of this kind of fusiform magnesium carbonate coated caco3 composite, as shown in Figure 5:
This composite is mainly elementary composition by magnesium (Mg), calcium (Ca), carbon (C) and oxygen (O) four kinds.
Fig. 6 is the attenuated total reflectance Fourier transform infrared spectroscopy figure of this kind of fusiform magnesium carbonate coated caco3 composite, by
Fig. 6 understands: 3172.6-3776.3cm-1Neighbouring absorption band belongs to the hydroxyl of a small amount of multi-form water contained by this composite and stretches
Contracting vibration, 1608.5cm-1Neighbouring absorption band belongs to the hydroxyl bending vibration of this composite absorption water, 1527.5cm-1、
1442.6cm-1、1386.7cm-1、1193.8cm-1, and 875.6cm-1Neighbouring absorption band belongs to this composite carbonate
Stretching vibration and bending vibration.
Embodiment 2
First, the concentrated hydrochloric acid (37.5wt%) of 125.0mL is configured to the dilute of 3.0mol/L with the deionized water of 375.0mL
Hydrochloric acid solution, adds the desulfurated plaster of equivalent concentration 160.0g/L under stirring at normal temperature, mixed liquor is acidified 10.0 at 130.0 DEG C
Being cooled to room temperature after hour, filter, filtrate is to carry out secondary filter after ethyl alcohol recrystallization, filter cake is with at after washing with alcohol 75.0 DEG C
It is dried to obtain pure calcium sulfate product；Secondly, the carbamide of 5.0g is configured to mass concentration as 50.0g/L with deionized water
Weak alkaline aqueous solution, adds the magnesium acetate of equivalent concentration 35.0g/L and the calcium sulfate product after purification of equivalent concentration 22.0g/L,
Hydro-thermal reaction 10.0 hours at 165.0 DEG C, are cooled to after room temperature filter, then by the composite filter cake that obtains directly with ethanol room
Filter under temperature after drying at drip washing, or 65.0 DEG C with ethanol filtered at room temperature drip washing；Finally, washed composite filter cake warp
75.0 DEG C of drying obtain fusiform magnesium carbonate coated caco3 composite for 5.5 hours.
The above-mentioned a kind of fusiform magnesium carbonate coated caco3 composite prepared is carried out microscopic appearance and Phase Structure Analysis,
Obtain similar electron scanning micrograph as shown in Figure 3, similar X-ray powder diagram as shown in Figure 4, be similar to such as
Energy dispersive x-ray spectrogram shown in Fig. 5, similar attenuated total reflectance Fourier transform infrared spectroscopy figure as shown in Figure 6.
Embodiment 3
First, the concentrated hydrochloric acid (37.5wt%) of 208.3mL is configured to the dilute of 5.0mol/L with the deionized water of 291.7mL
Hydrochloric acid solution, adds the desulfurated plaster of equivalent concentration 190.0g/L under stirring at normal temperature, mixed liquor is acidified 12.0 at 160.0 DEG C
Being cooled to room temperature after hour, filter, filtrate is to carry out secondary filter after ethyl alcohol recrystallization, filter cake is with at after washing with alcohol 85.0 DEG C
It is dried to obtain pure calcium sulfate product；Secondly, the carbamide of 10.0g is configured to mass concentration as 100.0g/L with deionized water
Weak alkaline aqueous solution, the calcium sulfate after purification of the magnesium acetate and equivalent concentration 30.0g/L that add equivalent concentration 50.0g/L produces
Thing, hydro-thermal reaction 24.0 hours at 180.0 DEG C, it is cooled to after room temperature filter, then by the composite filter cake that obtains directly with second
Alcohol filtered at room temperature drip washing, or at 85.0 DEG C dry after with ethanol filtered at room temperature drip washing；Finally, washed composite filter
Cake obtains fusiform magnesium carbonate coated caco3 composite for 8.0 hours through 85.0 DEG C of drying.
The above-mentioned a kind of fusiform magnesium carbonate coated caco3 composite prepared is carried out microscopic appearance and Phase Structure Analysis,
Obtain similar electron scanning micrograph as shown in Figure 3, similar X-ray powder diagram as shown in Figure 4, be similar to such as
Energy dispersive x-ray spectrogram shown in Fig. 5, similar attenuated total reflectance Fourier transform infrared spectroscopy figure as shown in Figure 6.
The above embodiment is the only present invention be described further, but the present invention is not limited to this, all without departing from this
Any amendment, equivalent or the improvement etc. made in the case of invention core, should be included in protection scope of the present invention.
Claims (10)
1. the preparation method of a fusiform magnesium carbonate coated caco3 composite, it is characterised in that comprise the steps of:
A. the purification of desulfurated plaster: desulfurated plaster stirring is added in the reactor containing acidic aqueous solution, is acidified under uniform temperature
Processing, be filtered to remove slightly solubility impurity, filtrate, with ethyl alcohol recrystallization, then carries out secondary filter, washing with alcohol, dried
To pure calcium sulfate product；
B. the preparation of composite: above-mentioned calcium sulfate product stirring after purification is added to the weakly alkaline solution containing magnesium salt,
It is cooled to room temperature under uniform temperature after hydro-thermal reaction, is filtrated to get composite filter cake；
C. washing: by the composite filter cake that is filtrated to get directly with washing with alcohol, or directly with washing with alcohol after drying；
D. it is dried: composite filter cake washing with alcohol crossed dries to obtain fusiform magnesium carbonate coated caco3 composite.
2., according to the preparation method of a kind of fusiform magnesium carbonate coated caco3 composite described in claim 1, its feature exists
In, in step A, the addition of desulfurated plaster is 25.0-200.0g/L, acidic aqueous solution H+Concentration is 0.5-6.0mol/L, acidifying
Temperature is 100.0-160.0 DEG C, and acidificatoin time is 5.0-12.0 hour.
3., according to the preparation method of a kind of fusiform magnesium carbonate coated caco3 composite described in claim 1, its feature exists
In, the acid of acidic aqueous solution is hydrochloric acid.
4., according to the preparation method of a kind of fusiform magnesium carbonate coated caco3 composite described in claim 1, its feature exists
In, in step B, calcium sulfate addition after purification is 12.5.0-30.0g/L, and the addition of magnesium salt is 15.0-50.0g/L, weak base
In property solution, the concentration of alkalescence material is 30.0-100.0g/L, and hydrothermal temperature is 150.0-180.0 DEG C, and the response time is
8.0-24.0 hour.
5., according to the preparation method of a kind of fusiform magnesium carbonate coated caco3 composite described in claim 1, its feature exists
In, magnesium salt refers to magnesium acetate.
6., according to the preparation method of a kind of fusiform magnesium carbonate coated caco3 composite described in claim 1, its feature exists
In, in weakly alkaline solution, alkalescence material is carbamide.
7., according to the preparation method of a kind of fusiform magnesium carbonate coated caco3 composite described in claim 1, its feature exists
In, in step C, washing refers to that the composite filter cake being filtrated to get adds ethanol filtered at room temperature drip washing, or be filtrated to get compound
Material filter cake 55.0-85.0 DEG C adds ethanol filtered at room temperature drip washing after drying.
8., according to the preparation method of a kind of fusiform magnesium carbonate coated caco3 composite described in claim 1, its feature exists
In, step D is dried and refers to that washed composite filter cake obtains fusiform carbon for 4.0-8.0 hour through 55.0-85.0 DEG C of drying
Acid magnesium coated caco3 composite.
9. the fusiform magnesium carbonate coated caco3 composite prepared according to the method described in any one of claim 1-8.
10. the fusiform magnesium carbonate coated caco3 composite prepared according to the method described in any one of claim 1-8,
It is characterized in that, surface is to be assembled by nanometer sheet.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20100024686A1 (en) * | 2007-06-28 | 2010-02-04 | Brent Constantz | Rocks and aggregate, and methods of making and using the same |
| US20100158786A1 (en) * | 2007-06-28 | 2010-06-24 | Constantz Brent R | Desalination methods and systems that include carbonate compound precipitation |
| CN102583483A (en) * | 2012-02-22 | 2012-07-18 | 常州碳酸钙有限公司 | Preparation method of micrometer spindle composite nano-calcium carbonate |
| CN104302594A (en) * | 2012-03-22 | 2015-01-21 | 勒瓦研究开发股份有限公司 | Mineral composition made from a mixed solid phase of calcium and magnesium carbonates, method of preparing same and use thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100024686A1 (en) * | 2007-06-28 | 2010-02-04 | Brent Constantz | Rocks and aggregate, and methods of making and using the same |
| US20100158786A1 (en) * | 2007-06-28 | 2010-06-24 | Constantz Brent R | Desalination methods and systems that include carbonate compound precipitation |
| CN102583483A (en) * | 2012-02-22 | 2012-07-18 | 常州碳酸钙有限公司 | Preparation method of micrometer spindle composite nano-calcium carbonate |
| CN104302594A (en) * | 2012-03-22 | 2015-01-21 | 勒瓦研究开发股份有限公司 | Mineral composition made from a mixed solid phase of calcium and magnesium carbonates, method of preparing same and use thereof |
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