CN117756127A - Method for preparing kaolin by adopting oxygen plasma treatment - Google Patents
Method for preparing kaolin by adopting oxygen plasma treatment Download PDFInfo
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- CN117756127A CN117756127A CN202311805094.5A CN202311805094A CN117756127A CN 117756127 A CN117756127 A CN 117756127A CN 202311805094 A CN202311805094 A CN 202311805094A CN 117756127 A CN117756127 A CN 117756127A
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- kaolin
- coal
- oxygen plasma
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- grinding
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 title claims abstract description 172
- 239000005995 Aluminium silicate Substances 0.000 title claims abstract description 170
- 235000012211 aluminium silicate Nutrition 0.000 title claims abstract description 170
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 100
- 239000001301 oxygen Substances 0.000 title claims abstract description 100
- 238000009832 plasma treatment Methods 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 53
- 238000000227 grinding Methods 0.000 claims abstract description 56
- 239000002245 particle Substances 0.000 claims abstract description 43
- 239000003245 coal Substances 0.000 claims abstract description 36
- 239000002994 raw material Substances 0.000 claims abstract description 35
- 206010040844 Skin exfoliation Diseases 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 21
- 238000012216 screening Methods 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 19
- 229910052799 carbon Inorganic materials 0.000 claims description 19
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical group [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 16
- 229910052726 zirconium Inorganic materials 0.000 claims description 16
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 15
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 15
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000004380 ashing Methods 0.000 claims description 7
- 238000003801 milling Methods 0.000 claims description 7
- 238000005086 pumping Methods 0.000 claims description 5
- 239000012159 carrier gas Substances 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 description 26
- 238000005261 decarburization Methods 0.000 description 12
- 230000000694 effects Effects 0.000 description 7
- 229910052500 inorganic mineral Inorganic materials 0.000 description 7
- 239000011707 mineral Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 238000001354 calcination Methods 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 239000003365 glass fiber Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000005188 flotation Methods 0.000 description 4
- 230000005484 gravity Effects 0.000 description 4
- 238000007885 magnetic separation Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 238000004061 bleaching Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000005262 decarbonization Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 229910001447 ferric ion Inorganic materials 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229910052683 pyrite Inorganic materials 0.000 description 1
- 239000011028 pyrite Substances 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 229910021646 siderite Inorganic materials 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005491 wire drawing Methods 0.000 description 1
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- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention provides a method for preparing kaolin by adopting oxygen plasma treatment, which comprises the following steps: (1) The method comprises the steps of sequentially carrying out crushing treatment, grinding and peeling treatment, drying treatment and screening treatment on coal-series kaolin raw materials to obtain coal-series kaolin particles; (2) The coal-based kaolin particles have a vacuum degree of 6×10 ‑1 ～9×10 ‑ 1 And (3) performing oxygen plasma treatment under the condition that the power of the mBar is 45-75W to obtain the kaolin. The method disclosed by the invention is simple to operate, the raw material of the coal-series kaolin is cheap and easy to obtain, the temperature of oxygen plasma treatment is low, and the layered structure of the kaolin Dan Kuangwu contained in the coal-series kaolin is not damaged while decarburizing the raw material of the coal-series kaolin is realized.
Description
Technical Field
The invention relates to the technical field of solid waste resource utilization, in particular to a method for preparing kaolin by adopting oxygen plasma treatment.
Background
The kaolin is a rock, clay and claystone mainly containing clay minerals of Kaolin family, and has chemical formula of Al 2 O 3 ·2SiO 2 ·2H 2 O, pure kaolin is white or light gray, and when impurities are contained, the kaolin is gray or yellowBrown, etc. The modified polypropylene has good plasticity, cohesiveness, insulativity, acid resistance, fire resistance and other excellent physical and chemical properties, and is widely used as a raw material in various fields, such as: ceramic industry, paper industry, refractory material, cement industry, rubber industry, petrochemical industry, medical textile industry, national defense industry, and the like.
The raw materials for preparing the kaolin are natural kaolin ores and coal-series kaolin, and the method mainly comprises gravity separation, magnetic separation, flotation, chemical bleaching, roasting purification and the like. The gravity separation is to remove light organic matters and high-density impurities containing iron, titanium, manganese and other elements by utilizing the density and granularity difference between kaolin and gangue minerals; the magnetic separation is to separate materials by utilizing the attractive force and repulsive force of magnetic substances, and is used for removing weak magnetic dyeing impurities such as hematite, siderite, pyrite, rutile and the like in kaolin; the flotation is to separate minerals by utilizing the differences of physical and chemical properties of the surfaces of the minerals, so that iron-containing, titanium-containing and carbon impurities in the kaolin can be effectively removed; chemical bleaching is to remove ferric ions and oxides thereof by chemical reagents to prepare kaolin; firing is to heat the mineral feedstock in an atmosphere to a temperature below its melting point to cause chemical reaction of the desired components with the furnace gases to convert to the desired composition and morphology to remove carbonaceous impurities from the kaolin. The existing method for preparing kaolin by taking coal-based kaolin as a raw material mainly comprises the steps of gravity separation, magnetic separation, flotation and roasting. Wherein, the carbon impurities in the kaolin cannot be removed by gravity separation and magnetic separation, and chemical agents are added in flotation and chemical bleaching, so that the production cost is increased; firing may destroy the layered structure of the kaolin Dan Kuangwu contained therein.
CN111533440a discloses a method for producing calcined kaolin for glass fiber, which comprises the following steps: crushing and finely crushing kaolin raw materials, grinding the crushed kaolin raw materials into fine powder with the particle size of more than 200 meshes, 2) preheating the ground fine powder in a continuous cyclone preheating system at the preheating temperature of 300-800 ℃, 3) mixing the powder collected from the upper part of a cyclone barrel with the ground powder, preheating the mixture in the cyclone barrel, feeding the cyclone discharged from the lower part of the cyclone barrel into a calcining device for calcining at the calcining temperature of 500-900 ℃ for more than 10 minutes, and cooling the calcined hot powder to obtain the kaolin for glass fibers. According to the production method of the calcined kaolin for the glass fiber, an additive is not needed, the input cost of raw materials is reduced, the COD of the prepared kaolin for the glass fiber is below 300ppm, the mullite phase is extremely small, the components are uniform, the fluctuation of the component content of the product is small, the melting wire drawing of the glass fiber is facilitated, and meanwhile, the continuous and large-scale production is easy to realize in the production process.
CN102730709a discloses a method for preparing calcined kaolin by using coal gangue, which is characterized in that the high-quality calcined kaolin can be prepared by crushing, pelletizing, crushing, washing, drying, adding sulfuric acid solution, naOH solution and drying the coal gangue.
CN104150497a discloses a method for preparing ultra-high whiteness calcined kaolin from full coal gangue. The method calcines the raw materials which are all composed of coal gangue for more than 6 hours at the temperature of 945-955 ℃. The whiteness of the calcined kaolin prepared by the method can reach more than 95, and the abrasion value and the 325 mesh sieve allowance are lower than those of calcined kaolin produced by other methods, thus having high application value.
However, the calcination adopted in the above method for preparing kaolin can destroy the layered structure of the kaolin Dan Kuangwu contained therein, thereby limiting the application of the kaolin.
Disclosure of Invention
In view of the problems existing in the prior art, the invention provides a method for preparing kaolin by adopting oxygen plasma treatment, which adopts cheap and easily available coal-based kaolin raw materials to effectively decarbonize by utilizing the oxygen plasma treatment, can improve the whiteness of the kaolin, and does not damage the layered structure of the kaolin Dan Kuangwu; the method is simple to operate, low in treatment cost and has a large-scale popularization and application prospect.
To achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for preparing kaolin by adopting oxygen plasma treatment, which comprises the following steps:
(1) The method comprises the steps of sequentially carrying out crushing treatment, grinding and peeling treatment, drying treatment and screening treatment on coal-series kaolin raw materials to obtain coal-series kaolin particles;
(2) The coal-based kaolin particles have a vacuum degree of 6×10 -1 ～9×10 -1 And (3) performing oxygen plasma treatment under the condition that the power of the mBar is 45-75W to obtain the kaolin.
The method for preparing the kaolin by using the oxygen plasma treatment adopts the coal-series kaolin with wide sources and low cost as the raw material, and uses the oxygen plasma treatment to prepare the kaolin, so that the carbon in the coal-series kaolin raw material is effectively removed, the operation is simple, the whiteness of the kaolin is greatly improved, and the color is changed from black to grey. The reaction mechanism diagram of the method for preparing kaolin by oxygen plasma treatment in the invention is shown in figure 1. And the temperature of the oxygen plasma treatment is in the range of 50-150 ℃, compared with the method for preparing the kaolin by roasting at the temperature of 1000-1300 ℃ in the prior art, the layered structure of the kaolin Dan Kuangwu is not damaged by low-temperature operation, and the kaolin mineral in the finally obtained kaolin still has the layered structure and has wider application range.
The vacuum degree of the invention is 6 multiplied by 10 -1 ～9×10 -1 The mBar may be, for example, 6×10 -1 mBar、6.5×10 - 1 mBar、7×10 -1 mBar、7.5×10 -1 mBar、8×10 -1 mBar、8.5×10 -1 mBar or 9X 10 -1 mBar, etc., but is not limited to the recited values, and other non-recited values within this range are equally applicable.
The power is 45 to 75W, and may be, for example, 45W, 46W, 50W, 55W, 60W, 65W, 75W, or the like, but is not limited to the values recited, and other values not recited in the numerical range are equally applicable.
The vacuum degree of the oxygen plasma treatment is 6 multiplied by 10 -1 ～9×10 -1 mBar ensures that coal-series kaolin is well decarbonized, has low vacuum degree, less oxygen molecules, less reactive gas active particles and poor decarbonizing effect, and the obtained kaolin has poor quality; when the vacuum degree is high, oxygen molecules are more, the energy loss of electrons in flight is increased, and the reacted gas can be causedThe reduction of the volume active particles, poor decarburization effect of the oxygen plasma coal-based kaolin raw material, low whiteness of the obtained kaolin and limited application range.
The power of the oxygen plasma treatment is 45-75W, when the power is low, the oxygen plasma cannot be well excited, so that the decarburization effect of the coal-series kaolin is poor; when the power is higher, the energy consumption of oxygen plasma treatment is higher, and the economy of preparing kaolin is poorer.
The carbon content of the coal-based kaolin raw material in step (1) is preferably 2 to 15%, and may be, for example, 2%, 4%, 6%, 8%, 10%, 12% or 15%, etc., but is not limited to the values listed, and other values not listed in the range are equally applicable.
The particle size of the coal-based kaolin material after the crushing treatment in the step (1) is preferably 0.25 to 0.85mm, and may be, for example, 0.25mm, 0.30mm, 0.42mm, 0.50mm, 0.60mm, 0.71mm or 0.85mm, etc., but is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned range are applicable.
Preferably, the peeling treatment of step (1) is performed in a peeling machine.
The feeding concentration of the mill stripper is preferably 20 to 40%, for example, 20%, 25%, 30%, 35%, 38% or 40%, but is not limited to the values listed, and other values not listed in the range are equally applicable.
Preferably, grinding aid and grinding medium are added in the grinding treatment in the step (1).
Preferably, the grinding aid is sodium hexametaphosphate, and the addition amount thereof is 1-4%, for example, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 3.8% or 4%, etc., but is not limited to the recited values, and other non-recited values within the range of the recited values are equally applicable.
Preferably, the grinding and stripping medium is zirconium balls, the mass ratio of the material to the zirconium balls is 5:1-1:1, for example, it may be 5:1, 4.5:1, 4:1, 3.8:1, 3.5:1, 3:1, 2.5:1, 2:1 or 1:1, but not limited to the listed values, and other non-listed values in the range of values are equally applicable.
Preferably, the drying treatment of step (1) is performed in a dryer.
The inlet temperature of the dryer is preferably 200 to 300 ℃, and may be 200 ℃, 220 ℃, 240 ℃, 250 ℃, 270 ℃, 290 ℃, 300 ℃, or the like, for example, but the inlet temperature is not limited to the recited values, and other non-recited values within the range are equally applicable;
the outlet temperature is 80 to 180 ℃, and may be, for example, 80 ℃, 100 ℃, 120 ℃, 140 ℃, 150 ℃, 170 ℃, 180 ℃, or the like, but is not limited to the values recited, and other values not recited in the range are equally applicable.
The water content of the coal-based kaolin after the drying treatment is preferably less than 1%, and may be, for example, 0.9%, 0.8%, 0.5%, 0.3%, 0.2%, 0.1%, or 0.05%, but is not limited to the values recited, and other values not recited in the range are equally applicable.
The particle size of the coal-based kaolin particles after the sieving treatment in the step (1) is preferably 0.09 to 0.125mm, and may be, for example, 0.09mm, 0.1mm, 0.15mm, 0.12mm, or 0.125mm, etc., but the present invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value range are equally applicable.
In the invention, the particle size of the coal-series kaolin particles after the screening treatment in the step (1) is preferably 0.09-0.125 mm, so that the coal-series kaolin raw material can be fully contacted with oxygen plasma, and the decarburization efficiency is improved.
Preferably, the oxygen plasma treatment of step (2) is performed in a low temperature oxygen plasma asher.
Preferably, the oxygen plasma treated carrier gas is oxygen.
Preferably, the chamber pressure of the low temperature oxygen plasma asher is from 5×10 -1 To 1X 10 0 mBar。
Preferably, the radio frequency of the oxygen plasma treatment is 13.56MHz.
The ashing time of the oxygen plasma treatment is preferably 4 to 5 hours, and may be, for example, 4 hours, 4.2 hours, 4.4 hours, 4.5 hours, 4.7 hours, 4.9 hours, or 5 hours, etc., but is not limited to the listed values, and other values not listed in the range of the values are equally applicable.
The kaolin preferably has a carbon content of 0.1 to 0.4%, for example, 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, or 0.4%, but is not limited to the recited values, and other non-recited values within the range are equally applicable.
As a preferred technical scheme of the invention, the method comprises the following steps:
(1) Crushing coal-series kaolin raw materials with the carbon content of 2-15%, wherein the particle size is 0.25-0.85 mm, grinding and peeling in a grinding and peeling machine, drying in a dryer, wherein the water content of the coal-series kaolin after the drying is lower than 1%, and screening to obtain coal-series kaolin particles with the particle size of 0.09-0.125 mm;
the feeding concentration of the milling and peeling machine is 20% -40%; grinding aid and grinding and stripping medium are added in the grinding and stripping treatment; the grinding aid is sodium hexametaphosphate, and the addition amount of the sodium hexametaphosphate is 1-4%; the grinding and peeling medium is zirconium balls, and the mass ratio of the materials to the zirconium balls is 5:1-1:1;
the inlet temperature of the dryer is 200-300 ℃, and the outlet temperature of the dryer is 80-180 ℃;
(2) The oxygen plasma treatment is performed in a low temperature oxygen plasma asher; the oxygen plasma treatment is preceded by pumping, carrying oxygen into the chamber, and the pressure of the chamber is from 5 multiplied by 10 -1 To 1X 10 0 mBar, radio frequency power is applied to the whole chamber to excite oxygen molecules;
the coal-based kaolin particles have a radio frequency of 13.56MHz and a vacuum degree of 6X 10 -1 ～9×10 -1 And (3) performing oxygen plasma treatment under the conditions of the mBar power of 45-75W and the ashing time of 4-5 h to obtain the kaolin with the carbon content of 0.1-0.4%.
Compared with the prior art, the invention has at least the following beneficial effects:
the method for preparing the kaolin by adopting the oxygen plasma treatment is simple to operate, the raw materials of the coal-series kaolin are cheap and easy to obtain, the temperature of the oxygen plasma treatment is low, the decarburization of the raw materials of the coal-series kaolin can be well realized, the whiteness of the prepared kaolin is greatly improved, the layered structure of the kaolin Dan Kuangwu contained in the kaolin is not damaged, and the method has a large-scale industrial application prospect.
Drawings
FIG. 1 is a reaction scheme of a method for preparing kaolin by oxygen plasma treatment according to the present invention.
FIG. 2 is an XRD pattern of the bulk coal-based kaolin material of example 1 and the kaolin prepared therefrom.
FIG. 3 is a photograph of a raw material of a large-coal-based kaolin in example 1.
Fig. 4 is a picture of the kaolin prepared in example 1.
FIG. 5 is an XRD pattern of the bulk coal-based kaolin material of comparative example 7 and the calcined kaolin prepared therefrom.
Detailed Description
The technical scheme of the invention is further described below by the specific embodiments with reference to the accompanying drawings.
The present invention will be described in further detail below. The following examples are merely illustrative of the present invention and are not intended to represent or limit the scope of the invention as defined in the claims.
Example 1
The present example provides a method for preparing kaolin using oxygen plasma treatment, the method comprising the steps of:
(1) Crushing a coal-series kaolin raw material with the carbon content of 4%, wherein the particle size is 0.42mm, grinding and stripping in a grinding and stripping machine, drying in a dryer, wherein the water content of the coal-series kaolin after the drying is 0.3%, and screening to obtain coal-series kaolin particles with the particle size of 0.1 mm;
the feeding concentration of the milling and peeling machine is 30%; grinding aid and grinding and stripping medium are added in the grinding and stripping treatment; the grinding aid is sodium hexametaphosphate, and the addition amount of the sodium hexametaphosphate is 1%; the grinding and peeling medium is zirconium balls, and the mass ratio of the materials to the zirconium balls is 2:1;
the inlet temperature of the dryer is 230 ℃, and the outlet temperature of the dryer is 120 ℃;
(2) The oxygen plasma treatment is performed in a low temperature oxygen plasma asher; the oxygen plasma treatment is preceded by pumping, carrying oxygen into the chamber, and the pressure of the chamber is from 5 multiplied by 10 -1 To 1X 10 0 mBar, radio frequency power is applied to the whole chamber to excite oxygen molecules;
the coal-based kaolin particles have a radio frequency of 13.56MHz and a vacuum degree of 7X 10 -1 Oxygen plasma treatment was performed at a power of 60W and an ashing time of 4.5h to obtain kaolin having a carbon content of 0.08%.
The XRD patterns of the raw material of the kaolin of the large coal series and the kaolin prepared by the raw material are shown in figure 2, and it can be seen from figure 2 that the kaolin product obtained after the oxygen plasma treatment is decarbonized and the layered structure of the kaolin Dan Kuangwu is not destroyed.
In this example, a picture of the raw material of the large-coal-based kaolin is shown in fig. 3, and it can be seen from fig. 3 that the color of the raw material of the large-coal-based kaolin is black. The picture of the kaolin prepared in this example is shown in fig. 4, and it can be seen from fig. 4 that the kaolin is off-white in color. Therefore, the method for preparing the kaolin by adopting the oxygen plasma treatment realizes effective decarburization and greatly improves the whiteness of the kaolin.
Example 2
The present example provides a method for preparing kaolin using oxygen plasma treatment, the method comprising the steps of:
(1) Crushing a coal-series kaolin raw material with the carbon content of 10%, wherein the particle size is 0.85mm, grinding and stripping in a grinding and stripping machine, drying in a dryer, wherein the water content of the coal-series kaolin after the drying is 0.1%, and screening to obtain coal-series kaolin particles with the particle size of 0.12 mm;
the feeding concentration of the milling and peeling machine is 20%; grinding aid and grinding and stripping medium are added in the grinding and stripping treatment; the grinding aid is sodium hexametaphosphate, and the addition amount of the sodium hexametaphosphate is 1%; the grinding and peeling medium is zirconium balls, and the mass ratio of the materials to the zirconium balls is 2:1;
the inlet temperature of the dryer is 300 ℃, and the outlet temperature of the dryer is 180 ℃;
(2) The oxygen plasma treatment is performed in a low temperature oxygen plasma asher; the oxygen plasma treatment is preceded by pumping, carrying oxygen into the chamber, and the pressure of the chamber is from 5 multiplied by 10 -1 To 1X 10 0 mBar, radio frequency power is applied to the whole chamber to excite oxygen molecules;
the coal-based kaolin particles have a radio frequency of 13.56MHz and a vacuum degree of 9X 10 -1 Oxygen plasma treatment was performed at 75W power and 5h ashing time to obtain kaolin having 0.2% carbon.
Example 3
The present example provides a method for preparing kaolin using oxygen plasma treatment, the method comprising the steps of:
(1) Crushing a coal-series kaolin raw material with the carbon content of 13%, wherein the particle size is 0.60mm, grinding and stripping in a grinding and stripping machine, drying in a dryer, wherein the water content of the coal-series kaolin after the drying is 0.8%, and screening to obtain coal-series kaolin particles with the particle size of 0.09 mm;
the feeding concentration of the milling and peeling machine is 20% -40%; grinding aid and grinding and stripping medium are added in the grinding and stripping treatment; the grinding aid is sodium hexametaphosphate, and the addition amount of the sodium hexametaphosphate is 1%; the grinding and peeling medium is zirconium balls, and the mass ratio of the materials to the zirconium balls is 2:1;
the inlet temperature of the dryer is 200 ℃, and the outlet temperature of the dryer is 80 ℃;
(2) The oxygen plasma treatment is performed in a low temperature oxygen plasma asher; the oxygen plasma treatment is preceded by pumping, carrying oxygen into the chamber, and the pressure of the chamber is from 5 multiplied by 10 -1 To 1X 10 0 mBar, radio frequency power is applied to the whole chamber to excite oxygen molecules;
the coal-based kaolin particles have a radio frequency of 13.56MHz and a vacuum degree of6×10 -1 Oxygen plasma treatment was performed at a power of 45W and an ashing time of 4h to obtain kaolin having a carbon content of 0.3%.
Comprehensive examples 1-3 show that the method for preparing kaolin by oxygen plasma treatment provided by the invention is simple to operate, has low treatment temperature, can well realize decarbonization of coal-series kaolin raw materials, greatly improves the whiteness of kaolin, does not damage the layered structure of kaolin Dan Kuangwu contained in the kaolin, and has a large-scale industrialized application prospect.
XRF analysis results of the different coal-based kaolin materials of examples 1-3 and the kaolin products prepared therefrom are shown in table 1.
TABLE 1
It can be seen from table 1 that the layered structure of kaolin Dan Kuangwu contained in kaolin was not transformed before and after the oxygen plasma treatment.
Comparative example 1
This comparative example provides a method for preparing kaolin using oxygen plasma treatment except that the oxygen plasma treatment is performed at a vacuum level of 10X 10 -1 Except for mBar, the rest was the same as in example 1.
Comparative example 2
This comparative example provides a method for preparing kaolin using oxygen plasma treatment except that the oxygen plasma treatment is performed at a vacuum level of 5X 10 -1 Except for mBar, the rest was the same as in example 1.
As can be seen from the comprehensive examples 1 and comparative examples 1-2, the oxygen plasma treatment in comparative example 1 has lower vacuum degree, less oxygen molecules, less reactive gas active particles, poor decarburization effect and poor quality of the obtained kaolin; in comparative example 2, the oxygen plasma treatment has higher vacuum degree, more oxygen molecules and increased electron energy loss in flight, which can lead to the reduction of reactive gas active particles, poor decarburization effect of oxygen plasma coal-based kaolin raw materials, lower whiteness of the obtained kaolin and limited application range.
Comparative example 3
This comparative example provides a method for preparing kaolin using oxygen plasma treatment, which is the same as example 1 except that the power of the oxygen plasma treatment is 40W.
Comparative example 4
This comparative example provides a method for preparing kaolin using oxygen plasma treatment, which is the same as example 1 except that the power of the oxygen plasma treatment is 80W.
As can be seen from the comprehensive examples 1 and comparative examples 3 to 4, the oxygen plasma treatment power in comparative example 3 is lower, and oxygen plasma cannot be well excited, so that the decarburization effect of the coal-based kaolin is poor, and the whiteness of the obtained kaolin is lower; the oxygen plasma treatment in comparative example 4 was higher in power, and although it did not greatly affect decarburization of the coal-based kaolin, the higher power resulted in higher energy consumption and poor economical production of kaolin.
Comparative example 5
This comparative example provides a method for preparing kaolin using oxygen plasma treatment, which is the same as example 1 except that the time of oxygen plasma treatment is 2 hours.
Comparative example 6
This comparative example provides a method for preparing kaolin using oxygen plasma treatment, which is the same as example 1 except that the time of the oxygen plasma treatment is 7 hours.
As can be seen from the combination of examples 1 and comparative examples 5 to 6, the oxygen plasma treatment time in comparative example 5 is short, the decarburization is not complete, and the decarburization effect is poor; the oxygen plasma treatment in comparative example 6 was longer, and although it did not have a great influence on decarburization of the coal-based kaolin, the longer time resulted in higher energy consumption and poor economical production of kaolin.
The carbon content of the coal-based kaolin and kaolin products in comparative examples 1 to 6 are shown in Table 2.
TABLE 2
Comparative example 7
This comparative example provides a method of preparing kaolin comprising the steps of:
(1) Crushing a large-size coal-series kaolin raw material with the carbon content of 4%, wherein the particle size is 0.85mm, grinding and peeling in a grinding and peeling machine, drying in a dryer, wherein the water content of the coal-series kaolin after the drying is 0.1%, and screening to obtain coal-series kaolin particles with the particle size of 0.09 mm;
the feeding concentration of the milling and peeling machine is 20%; grinding aid and grinding and stripping medium are added in the grinding and stripping treatment; the grinding aid is sodium hexametaphosphate, and the addition amount of the sodium hexametaphosphate is 1%; the grinding and peeling medium is zirconium balls, and the mass ratio of the materials to the zirconium balls is 2:1;
the inlet temperature of the dryer is 300 ℃, and the outlet temperature of the dryer is 180 ℃;
(2) The coal-series kaolin particles are placed in a muffle furnace, the furnace temperature is controlled at 1000 ℃ for calcining for 2 hours, natural annealing is carried out, and the kaolin is obtained after cooling at normal temperature.
The XRD patterns of the raw material bulk coal-based kaolin and the prepared kaolin in this comparative example are shown in FIG. 5. As can be seen from fig. 5, the higher calcination temperature breaks down the layered structure of the kaolinite mineral contained in the kaolin, and mineral transformation occurs, resulting in reduced performance of the kaolin.
The applicant declares that the above is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that are easily conceivable within the technical scope of the present invention disclosed by the present invention fall within the scope of the present invention and the disclosure.
Claims (10)
1. A method for preparing kaolin using oxygen plasma treatment, said method comprising the steps of:
(1) The method comprises the steps of sequentially carrying out crushing treatment, grinding and peeling treatment, drying treatment and screening treatment on coal-series kaolin raw materials to obtain coal-series kaolin particles;
(2) The coal-based kaolin particles have a vacuum degree of 6×10 -1 ～9×10 -1 And (3) performing oxygen plasma treatment under the condition that the power of the mBar is 45-75W to obtain the kaolin.
2. The method of claim 1, wherein the coal-based kaolin feedstock of step (1) has a carbon content of 2 to 15%;
preferably, the particle size of the crushed coal-based kaolin raw material is 0.25-0.85 mm.
3. The method of claim 1 or 2, wherein the abrasive stripping process of step (1) is performed in an abrasive stripper;
preferably, the feeding concentration of the milling and peeling machine is 20-40%.
4. A method according to any one of claims 1 to 3, wherein grinding aid and grinding medium are added to the grinding treatment of step (1);
preferably, the grinding aid is sodium hexametaphosphate, and the addition amount of the sodium hexametaphosphate is 1-4%;
preferably, the grinding and stripping medium is zirconium balls, and the mass ratio of the material to the zirconium balls is 5:1-1:1.
5. The method according to any one of claims 1 to 4, wherein the drying treatment of step (1) is performed in a dryer;
preferably, the inlet temperature of the dryer is 200-300 ℃, and the outlet temperature is 80-180 ℃;
preferably, the water content of the coal-based kaolin after the drying treatment is less than 1%.
6. The method according to any one of claims 1 to 5, wherein the particle size of the coal-based kaolin particles after the sieving treatment in step (1) is 0.09 to 0.125mm.
7. The method according to any one of claims 1 to 6, wherein the oxygen plasma treatment of step (2) is performed in a low temperature oxygen plasma asher;
preferably, the oxygen plasma treated carrier gas is oxygen;
preferably, the chamber pressure of the low temperature oxygen plasma asher is from 5×10 -1 To 1X 10 0 mBar。
8. The method according to any one of claims 1 to 7, wherein the radio frequency of the oxygen plasma treatment of step (2) is 13.56MHz;
preferably, the ashing time of the oxygen plasma treatment is 4 to 5 hours.
9. The method according to any one of claims 1 to 8, wherein the kaolin of step (2) has a carbon content of 0.1 to 0.4%.
10. The method according to any one of claims 1 to 9, characterized in that it comprises the steps of:
(1) Crushing coal-series kaolin raw materials with the carbon content of 2-15%, wherein the particle size is 0.25-0.85 mm, grinding and peeling in a grinding and peeling machine, drying in a dryer, wherein the water content of the coal-series kaolin after the drying is lower than 1%, and screening to obtain coal-series kaolin particles with the particle size of 0.09-0.125 mm;
the feeding concentration of the milling and peeling machine is 20-40%; grinding aid and grinding and stripping medium are added in the grinding and stripping treatment; the grinding aid is sodium hexametaphosphate, and the addition amount of the sodium hexametaphosphate is 1-4%; the grinding and peeling medium is zirconium balls, and the mass ratio of the materials to the zirconium balls is 5:1-1:1; the inlet temperature of the dryer is 200-300 ℃, and the outlet temperature of the dryer is 80-180 ℃;
(2) The oxygen plasma treatment is performed in a low temperature oxygen plasma asher; the oxygen plasma treatment is preceded by pumping, carrying oxygen into the chamber, and the pressure of the chamber is from 5 multiplied by 10 -1 To 1X 10 0 mBar, radio frequency power is applied to the whole chamber to excite oxygen molecules;
the coal-based kaolin particles have a radio frequency of 13.56MHz and a vacuum degree of 6X 10 -1 ～9×10 -1 And (3) performing oxygen plasma treatment under the conditions of the mBar power of 45-75W and the ashing time of 4-5 h to obtain the kaolin with the carbon content of 0.1-0.4%.
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