CN103288096B - A kind of calcining coal-series kaolinite method reducing calcining temperature - Google Patents
A kind of calcining coal-series kaolinite method reducing calcining temperature Download PDFInfo
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- 238000001354 calcination Methods 0.000 title claims abstract description 85
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- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 24
- 238000005119 centrifugation Methods 0.000 claims abstract description 24
- 238000004513 sizing Methods 0.000 claims abstract description 24
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- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 claims description 17
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- 230000009257 reactivity Effects 0.000 claims description 11
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims description 8
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 2
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- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
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- 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
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention belongs to coal series kaolin rock field of comprehensive utilization, be specifically related to a kind of calcining coal-series kaolinite method reducing calcining temperature, described method for calcinating comprises the following steps: pulverized by coal series kaolin rock; Coal series kaolin rock after pulverizing is mixed with water and sylvite, obtains intercalated compound slurry; Described intercalated compound slurry carries out centrifugation, obtains intercalated compound sizing and intercalant solution; Described intercalated compound sizing is put into calcining furnace, is warming up to 350-450 DEG C, after constant temperature 2-2.5h, then be warming up to 600-700 DEG C and constant temperature 0.5-1h; Washing, filtration; Coal series kaolin rock after filtering is made slurry again, carries out spraying dry, obtain finished product superfine calcined kaolin.Method for calcinating provided by the invention reduces energy consumption, and the kaolinite after calcining has higher activity.
Description
Technical field
The invention belongs to coal series kaolin rock field of comprehensive utilization, be specifically related to a kind of calcining coal-series kaolinite method reducing calcining temperature.
Background technology
Coal series kaolin rock is mainly present in roof and floor and the coal seam dirt band in coal seam, with coal symbiosis, abundant kaolinite resource is had in China's coal stratum, it has verified prospective reserves up to more than 180 hundred million tons, be that China accounts for one of nonmetal mineral resource of reserves and quality double dominant, and there is huge development and utilization value.Generally extraction can be attached while seam mining.In the past, the resource of these preciousnesses was often taken as spoil and discarded, and not only wasted resource, land occupation, but also seriously contaminate environment.In order to fully carry out the comprehensive utilization of coal resources, developing a circular economy, in the recent decade, having started the upsurge of one exploitation coal series kaolin rock in China's coal-mine district.The coal field big and small coal series kaolin rock processing enterprise setting up more than 50 families at present in provinces such as China Shanxi, Inner Mongol, Henan, Shandong, Hebei, national accumulation annual production reaches 60-80 ten thousand tons.
Coal series kaolin rock, because contained kaolinite purity is high, crystallization degree good, form of flake crystal is complete, become the main production raw material of producing high grade kaolinite product, particularly calcined ultrafine kaolin, in great demand, coal gangue (coal series kaolin rock) can be made to have a sudden rise in social status, produce huge economic benefit simultaneously.Calcined coal kaolin is compared with common kaolin, whiteness is high, fine size, there is better insulativity and oil absorbency, and refractoriness improves, specific surface area significantly increases, and therefore, calcined coal kaolin has been widely used in the fields such as rubber, plastics, cable, paint, coating, papermaking, pottery, enamel, refractory materials, weaving, cement, automobile, chemistry, environmental protection, agricultural.
Calcining is a key link of coal series kaolin rock deep process technology, and be in fact also kaolinic a kind of modification mode, its main purpose is: (1) removes organic carbonaceous with other impure mineral to improve whiteness; (2) moisture content contained by kaolinite, hydroxyl is removed to improve void volume and the chemical reactivity of calcination product; (3) improve its physical and chemical performance, meet various application demand.Current different types of kaolin product is very high to the requirement of whiteness, if coal series kaolin rock impurity component fails to be completely removed, can not ensure whiteness and the quality of product, does not just reach industry needs.So the calcining temperature that present coal series kaolin rock is general makes it calcine removing impurity completely up to about 1000 DEG C, improve whiteness, to reach industry needs.
Be that raw material is prepared in high whiteness calcined kaolin technique with coal series kaolin rock, calcined kaolin can be divided into according to calcining temperature: 600-1000 DEG C, low temperature calcination; 1000-1200 DEG C, middle temperature calcining; Be greater than 1200 DEG C, high-temperature calcination three types.Low temperature calcination Product Activity is high, for the synthesis of the functional materials of molecular sieve, aluminium salt chemical engineering plastics, rubber.The selection of optimum calcinating temperature, different from the difference of the origin cause of formation of raw material, granularity, working method, purposes.
The method for calcinating of current coal series kaolin rock is comparatively single, mainly contains " calcine after grind " and " grind after calcine " two kinds of techniques.But " calcine after grind " technique cannot solve the calcining agglomeration of product, product granularity fluctuation is larger, " grind after calcine " technique cannot ensure the whiteness of product, the product stability of these two kinds of explained hereafter and bad adaptability, tooling cost is relatively high, the quality of product and whiteness all can not be guaranteed, and the gas that simultaneously discharge of carbonic acid gas and calcining add Thermal release in calcination process causes very large pollution to environment.This shows that reduction and the reduction Carbon emission of calcining coal-series kaolinite temperature have important practical significance for raising coal series kaolin rock class and protection of the environment.
Application number is the patent of CN99116119.X, describes a kind of calcining coal-series kaolinite working method.The bulk coal series kaolin rock come in mine is processed into 800 order-3500 object ultrafine powders through pulverizing removal of impurities.In the whiteness of 700-960 DEG C or 1050-1250 DEG C calcining at the extremely strong active substance of the adsorptive power of 88-97.
Application number be CN01141668.8 patent describes a kind of production method of wet ultra-fine calcined kaolin.Kaolin ore is broken into powder, then powder is mixed with water and be made into raw material and starch, be delivered in flash drying equipment after raw material slurry is worn into superfine slurry and carry out drying, preheating in drying process in preheating zone and the calcining of calcining zone, then in cooling zone, namely complete kaolinic calcining after cooling, finally carry out breaing up making finished product.
Application number is that the one that patent discloses of CN03125386.5 utilizes coal gangue to do raw material to prepare superfine calcined kaolin method.After being less than the coal gangue powder of 45 μm and urea mixing with granularity, add in ball mill or vibration mill, then the intercalated compound of dry grinding inserts in calcining furnace, 600 DEG C of constant temperature 0.5 hour is warming up to the heat-up rate of 5 DEG C/min, reheat to 850-900 DEG C, constant temperature 1 hour, break up after burnt powder cooling, obtain 90% granularity and be less than 2 μm, and the ultra tiny calcined kaolin that whiteness is greater than 90%.
Application number is the patent of CN200810047547.1, describe a kind of calcination kleit preparation method, Coaseries kaolin is crushed to 800-1250 order, add dispersion agent after classification and be made into the ore pulp that concentration is 42-45%, the granularity being ground to 80% with machine for cutting charge into pieces is less than 2 μm, dilution ore pulp to concentration is utilize hydroclone classification after 20-40%, dehydrates, breaks up, calcines, breaks up depolymerization, classification obtains the calcined kaolin products that whiteness is greater than 90% after overflowing concentrate through row.
The method energy consumption that above-mentioned patent adopts is all higher, and kaolinic crystalline form is difficult to remain intact, and kaolinic activity fails to ensure, pollution on the environment is serious in addition.Not yet find at present can reduce energy consumption and the method for calcinating that can improve Coaseries kaolin activity.
Summary of the invention
The object of the present invention is to provide a kind of calcining coal-series kaolinite method reducing calcining temperature, this method reduce energy consumption, alleviate calcining coal series kaolin rock to the pollution of environment, the coal series kaolin rock after calcining has higher activity.
In order to realize foregoing invention object, adopt following technical scheme:
Reduce a calcining coal-series kaolinite method for calcining temperature, comprise the following steps:
(1) coal series kaolin rock is pulverized;
(2) coal series kaolin rock after pulverizing is mixed with water and sylvite, obtain intercalated compound slurry; Described sylvite be selected from Potassium ethanoate, Potassium monofluoride, Repone K, Potassium Bromide, potassiumiodide one or more;
(3) described intercalated compound slurry carries out centrifugation, obtains intercalated compound sizing and intercalant solution;
(4) described intercalated compound sizing is put into calcining furnace, be warming up to 350-450 DEG C, after constant temperature 2-2.5h, then be warming up to 600-700 DEG C and constant temperature 0.5-1h;
(5) wash, filter;
(6) coal series kaolin rock after filtration is made slurry again, carry out spraying dry, obtain finished product high reactivity superfine calcined kaolin.
In calcining coal-series kaolinite process, a large amount of eliminating hydroxide about 550 DEG C time and be converted into metakaolinite, and be continued until about 950 DEG C, about 990 DEG C time, mineral lattice is destroyed, and recrystallization forms the release that cenotype causes energy, generates mullite.Kaolinite dehydroxylation makes lattice form room, and add the activity of kaolinite, the recrystallization under high temperature destroys the activity of kaolinite.The present invention adopts sylvite to carry out intercalation processing before being calcined, has slackened the reactive force between kaolinite synusia, makes its thermomechanical property generation great variety, dehydroxylation temperature declines to a great extent, calcining temperature declines to a great extent, and improves the kaolinic activity after calcining, reduces energy consumption.Organic impurity contained in coal series kaolin rock also can be separated by intercalation processing in intercalation process simultaneously, be separated together with intercalant solution through centrifugation again, the discharge to carbonic acid gas is reduced, to reduce environmental pollution in calcination process below.In addition, intercalation processing can stop kaolinite recrystallization at high temperature, avoids the destruction of high temperature to kaolinite activity.
Described coal series kaolin rock is preferably coal gangue.
In described step (1), preferably coal series kaolin rock is crushed to 200-325 order.
Described sylvite is preferably Potassium ethanoate.
In described step (2), the mass ratio of described coal series kaolin rock and water is 1: 1 ~ 5, and the mass ratio of described coal series kaolin rock and sylvite is 1: 0.05 ~ 0.30; Preferably, the mass ratio of described coal series kaolin rock and water is 1: 3 ~ 5, described coal series kaolin rock and sylvite mass ratio be 1: 0.15 ~ 0.2.
In described step (2): described mixing is by coal series kaolin rock, sylvite, water, puts into steel basin, stir after 10 ~ 60 minutes and leave standstill 6 ~ 40h, obtain Kaolinite/organic Intercalation Compounds.Can be coal series kaolin rock, sylvite puts into together with water, after also sylvite and water can being mixed, then add coal series kaolin rock.Intercalation process can carry out removal of impurities to Coaseries kaolin further.
In described step (3), the rotating speed of centrifugation is that 3000 ~ 5000r/ divides, and the time of centrifugation is 5 ~ 15 minutes.The sylvite intercalator obtained after centrifugation can reclaim to be reused.
The present invention has considered calcining temperature, temperature rise rate and the constant temperature time Different Effects to physicochemical properties such as calcined kaolin activity, whiteness, radius-thickness ratio, crystal formations, thus determines best calcining process.In described step (4), be warming up to 350-450 DEG C with 5-15 DEG C/min, after constant temperature 2-2.5h; 600-700 DEG C is warming up to and constant temperature 0.5-1h again with 2 ~ 5 DEG C/min; Preferred: to be warming up to 350-450 DEG C with 10 ~ 15 DEG C/min; 600-700 DEG C is warming up to again with 5 DEG C/min; Most preferred: 10 DEG C/min or 15 DEG C/min are warming up to 350-450 DEG C.
In described step (5), bath water amount is 1 ~ 2 times of coal series kaolin rock weight.
In described finished product high reactivity superfine calcined kaolin, hexagonal flake kaolin crystal accounts for 20-50%, particle diameter D97≤2 μm of finished product superfine calcined kaolin, and finished product superfine calcined kaolin wafer thickness is less than 200nm, and whiteness is higher than 90%.
Compared with prior art, the invention has the beneficial effects as follows:
(1) reduce the temperature of dehydroxylation, improve kaolinic activity
Calcining process of the present invention is owing to taking sylvite intercalation processing in advance, some compounds are made to enter in the middle of kaolinite crystal layer, slacken the reactive force between kaolinite synusia, kaolinite dehydroxylation temperature is declined, and calcining temperature declines to a great extent, and in calcination process, the temperature of dehydroxylation have dropped 100 ~ 150 DEG C, therefore in calcination process, under cryogenic can eliminating hydroxide completely, and avoid the recrystallization of high temperature, improve kaolinic activity.
(2) energy consumption is reduced
Hydrated potassium ion can be formed at interlayer after intercalated molecule sylvite and silicate mixing, be convenient to the hydroxyl between silicate layer is sloughed at a lower temperature, reduce calcining temperature, thus reduce energy consumption, energy-conservation more than 30%.
(3) improve whiteness
Calcining process of the present invention is owing to taking sylvite intercalation processing in advance, some compounds are made to enter in the middle of kaolinite crystal layer, the organic matter being attached to kaolinite surface is separated, and the organic matter departed from after a few hours leave standstill just swims in intercalant solution surface.After centrifugation, organic impurity is separated, and be conducive to the raising of kaolin whiteness after low temperature calcination, whiteness is increased to more than 90%; The discharge of carbonic acid gas in calcination process can be reduced simultaneously, alleviate the pollution to environment.
(4) larger radius-thickness ratio is kept
The stripping of the kaolinite crystal layer after sylvite intercalation, can form the very thin lamella that 100 ~ 200nm is thick, and keep large kaolinite radius-thickness ratio, the radius-thickness ratio of finished product kaolin crystal is between 10: 1 ~ 30: 1.
(5) kaolinic crystal formation keeps better
Calcining process of the present invention is comparatively light to the destructiveness of kaolin crystal, can keep relatively complete kaolinite crystalline form.
(6) simple to operate, low production cost, calcines effective.
Embodiment
Below in conjunction with embodiment, the present invention is described in more detail; but it is not thereby limiting the invention; under the prerequisite not departing from design philosophy of the present invention, the various changes and modifications that those skilled in the art make technical scheme of the present invention, all belong to protection scope of the present invention.
Embodiment 1
Drop into steel basin with water together with Potassium ethanoate after being pulverized by coal series kaolin rock, mix, obtain intercalated compound slurry; Intercalated compound slurry is carried out centrifugation, obtains intercalated compound sizing and intercalant solution; Intercalated compound sizing is put into calcining furnace, is warming up to 350 DEG C, after constant temperature 2h, then be warming up to 600 DEG C and constant temperature 1h.The coal series kaolin rock taken out after calcining carries out washing, filtering, and the coal series kaolin rock after filtering is made slurry again, carries out spraying dry, obtain finished product high reactivity superfine calcined kaolin.In finished product kaolinite, hexagonal flake kaolin crystal accounts for 20%, particle diameter D97=2 μm, and wafer thickness is less than 200nm, whiteness 90%.
Embodiment 2
Drop into steel basin with water together with Repone K after being pulverized by coal series kaolin rock, mix, obtain intercalated compound slurry; Intercalated compound slurry is carried out centrifugation, obtains intercalated compound sizing and intercalant solution; Intercalated compound sizing is put into calcining furnace, is warming up to 450 DEG C, after constant temperature 2.5h, then be warming up to 700 DEG C and constant temperature 0.5h.The coal series kaolin rock taken out after calcining carries out washing, filtering, and the coal series kaolin rock after filtering is made slurry again, carries out spraying dry, obtain finished product calcined kaolin.In finished product kaolinite, hexagonal flake kaolin crystal accounts for 30%, particle diameter D97=2 μm, and wafer thickness is less than 200nm, whiteness 91%.
Embodiment 3
Drop into steel basin with water together with Potassium Bromide after being pulverized by coal series kaolin rock, mix, obtain intercalated compound slurry, wherein the mass ratio of coal series kaolin rock and water is 1: 5, and the mass ratio of coal series kaolin rock and Potassium Bromide is 1: 0.30.Intercalated compound slurry is carried out centrifugation, obtains intercalated compound sizing and intercalant solution; Intercalated compound sizing is put into calcining furnace, is warming up to 350 DEG C, after constant temperature 2.5h, then be warming up to 600 DEG C and constant temperature 0.5h.The coal series kaolin rock taken out after calcining carries out washing, filtering, and the coal series kaolin rock after filtering is made slurry again, carries out spraying dry, obtain finished product calcined kaolin.In finished product kaolinite, hexagonal flake kaolin crystal accounts for 30%, particle diameter D97=1.9 μm, and wafer thickness is less than 200nm, whiteness 90%.
Embodiment 4
Drop into steel basin with water together with Potassium ethanoate after being pulverized by coal series kaolin rock, mix, obtain intercalated compound slurry, wherein the mass ratio of coal series kaolin rock and water is 1: 1, and the mass ratio of coal series kaolin rock and Potassium ethanoate is 1: 0.05.Intercalated compound slurry is carried out centrifugation, obtains intercalated compound sizing and intercalant solution; Intercalated compound sizing is put into calcining furnace, is warming up to 450 DEG C, after constant temperature 2h, then be warming up to 700 DEG C and constant temperature 1h.The coal series kaolin rock taken out after calcining carries out washing, filtering, and the coal series kaolin rock after filtering is made slurry again, carries out spraying dry, obtain finished product calcined kaolin.In finished product kaolinite, hexagonal flake kaolin crystal accounts for 25%, particle diameter D97=2 μm, and wafer thickness is less than 200nm, whiteness 92%.
Embodiment 5
Pulverize coal gangue to 325 orders, and drop into steel basin with water together with Potassium ethanoate, mix, obtain intercalated compound slurry, wherein the mass ratio of coal gangue and water is 1: 5, and the mass ratio of coal gangue and Potassium ethanoate is 1: 0.25.Intercalated compound slurry is carried out centrifugation 15 minutes, the rotating speed of centrifugation is that 3000r/ divides, and obtains intercalated compound sizing and intercalant solution.Intercalated compound sizing is put into calcining furnace, is warming up to 350 DEG C with 5 DEG C/min, after constant temperature 2.5h; 600 DEG C are warming up to and constant temperature 0.5h again with 5 DEG C/min.The coal gangue taken out after calcining washs, and bath water amount is 1 times of coal series kaolin rock weight, filters, and the coal gangue after filtering is made 45% slurry again, carries out spraying dry, obtain finished product high reactivity superfine calcined kaolin.In finished product, hexagonal flake kaolin crystal accounts for 40%, particle diameter D97=1.8 μm, and wafer thickness is less than 180nm, whiteness 90%.
Embodiment 6
Coal series kaolin rock is crushed to 200 orders, and drops into steel basin with water together with Potassium ethanoate, mix, obtain intercalated compound slurry, wherein the mass ratio of coal series kaolin rock and water is 1: 4, and the mass ratio of coal series kaolin rock and Potassium ethanoate is 1: 0.20.Intercalated compound slurry is carried out centrifugation 5 minutes, the rotating speed of centrifugation is that 5000r/ divides, and obtains intercalated compound sizing and intercalant solution.Intercalated compound sizing is put into calcining furnace, is warming up to 400 DEG C with 10 DEG C/min, after constant temperature 2h; 650 DEG C are warming up to and constant temperature 0.5h again with 2 DEG C/min.The coal series kaolin rock taken out after calcining washs, and bath water amount is 1 times of coal series kaolin rock weight, filters, and the coal series kaolin rock after filtering is made 45% slurry again, carries out spraying dry, obtain finished product high reactivity superfine calcined kaolin.In finished product, hexagonal flake kaolin crystal accounts for 50%, particle diameter D97=1.7 μm, and wafer thickness is less than 150nm, whiteness 92%.
Embodiment 7
Coal series kaolin rock is crushed to 325 orders, and drops into steel basin with water together with Potassium ethanoate, mix, obtain intercalated compound slurry, wherein the mass ratio of coal series kaolin rock and water is 1: 3, and the mass ratio of coal series kaolin rock and Potassium ethanoate is 1: 0.15.Intercalated compound slurry is carried out centrifugation 15 minutes, the rotating speed of centrifugation is that 3000r/ divides, and obtains intercalated compound sizing and intercalant solution.Intercalated compound sizing is put into calcining furnace, is warming up to 450 DEG C with 15 DEG C/min, after constant temperature 2.5h; 700 DEG C are warming up to and constant temperature 1h again with 5 DEG C/min.The coal series kaolin rock taken out after calcining washs, and bath water amount is 2 times of coal series kaolin rock weight, filters, and the coal series kaolin rock after filtering is made 45% slurry again, carries out spraying dry, obtain finished product high reactivity superfine calcined kaolin.In finished product, hexagonal flake kaolin crystal accounts for 50%, particle diameter D97=1.5 μm, and wafer thickness is less than 150nm, whiteness 94%.
Embodiment 8
Coal series kaolin rock is crushed to 325 orders, and drop into steel basin with water together with Potassium ethanoate, stir after 10 minutes and leave standstill 6h, obtain intercalated compound slurry, wherein the mass ratio of coal series kaolin rock and water is 1: 3, and the mass ratio of coal series kaolin rock and Potassium ethanoate is 1: 0.15.Intercalated compound slurry is carried out centrifugation 15 minutes, the rotating speed of centrifugation is that 3000r/ divides, and obtains intercalated compound sizing and intercalant solution.Intercalated compound sizing is put into calcining furnace, is warming up to 450 DEG C with 15 DEG C/min, after constant temperature 2.5h; 700 DEG C are warming up to and constant temperature 1h again with 5 DEG C/min.The coal series kaolin rock taken out after calcining washs, and bath water amount is 2 times of coal series kaolin rock weight, filters, and the coal series kaolin rock after filtering is made 50% slurry again, carries out spraying dry, obtain finished product high reactivity superfine calcined kaolin.In finished product, hexagonal flake kaolin crystal accounts for 50%, particle diameter D97=1.5 μm, and wafer thickness is less than 160nm, whiteness 93%.
Embodiment 9
Coal series kaolin rock is crushed to 250 orders, and drop into steel basin with water together with Potassium ethanoate, stir after 60 minutes and leave standstill 40h, obtain intercalated compound slurry, wherein the mass ratio of coal series kaolin rock and water is 1: 3, and the mass ratio of coal series kaolin rock and Potassium ethanoate is 1: 0.15.Intercalated compound slurry is carried out centrifugation 15 minutes, the rotating speed of centrifugation is that 3000r/ divides, and obtains intercalated compound sizing and intercalant solution.Intercalated compound sizing is put into calcining furnace, is warming up to 450 DEG C with 15 DEG C/min, after constant temperature 2.5h; 700 DEG C are warming up to and constant temperature 1h again with 5 DEG C/min.The coal series kaolin rock taken out after calcining washs, and bath water amount is 2 times of coal series kaolin rock weight, filters, and the coal series kaolin rock after filtering is made 40% slurry again, carries out spraying dry, obtain finished product high reactivity superfine calcined kaolin.In finished product, hexagonal flake kaolin crystal accounts for 50%, particle diameter D97=1.6 μm, and wafer thickness is less than 160nm, and whiteness is 94%.
Experimental example 1
This experimental example has investigated the impact of calcining process on Coaseries kaolin activity, and the three kinds of samples investigated all react under identical experiment condition.
Sample 1 is the product prepared according to the embodiment of the present invention 1;
Sample 2 is the product prepared according to the embodiment 1 of patent CN03125386.5;
Sample 3 is the product prepared according to the embodiment 1 of patent CN01141668.8;
The activity of coal series kaolin rock is higher, and its speed of reaction is faster.The reaction product of Coaseries kaolin and alkali lye is the NaAlO of solubility
2and Na
2siO
3, this experimental example compares the activity of three kinds of samples by the speed of reaction investigating three kinds of samples.
Sample thief 1, sample 2, each 5g of sample 3, in three beakers, add the NaOH liquid 20ml of 15% respectively under 85 DEG C of conditions, react 10 minutes under induction stirring, filter, and weigh the quality of filter residue after three example reactions.The filter residue of sample 1 is 1.9g, and the filter residue of sample 1 is 2.4g, and the filter residue of sample 1 is 2.6g.
Conclusion: the filter residue quality of sample 1 is minimum, the speed of its reaction is maximum, active maximum.
The product of other embodiment of the present invention also has the experimental result similar with sample 1, because length limit, does not enumerate at this.
Claims (9)
1. reduce a calcining coal-series kaolinite method for calcining temperature, it is characterized in that, comprise the following steps:
(1) coal series kaolin rock is pulverized;
(2) coal series kaolin rock after pulverizing is mixed with water and sylvite, obtain intercalated compound slurry; Described sylvite be selected from Potassium ethanoate, Potassium monofluoride, Repone K, Potassium Bromide, potassiumiodide one or more; The mass ratio of described coal series kaolin rock and water is 1:1 ~ 5, and the mass ratio of described coal series kaolin rock and sylvite is 1:0.05 ~ 0.30;
(3) described intercalated compound slurry carries out centrifugation, obtains intercalated compound sizing and intercalant solution;
(4) described intercalated compound sizing is put into calcining furnace, be warming up to 350-450 DEG C, after constant temperature 2-2.5h, then be warming up to 600-700 DEG C and constant temperature 0.5-1h;
(5) wash, filter;
(6) coal series kaolin rock after filtration is made slurry again, carries out spraying dry, obtain finished product high reactivity superfine calcined kaolin,
Wherein, the mixing described in step (2) coal series kaolin rock, sylvite and water is stirred after 10-60 minute to leave standstill 6-40 hour.
2. method for calcinating according to claim 1, is characterized in that, described coal series kaolin rock is coal gangue.
3. method for calcinating according to claim 1, is characterized in that, in described step (1), coal series kaolin rock is crushed to 200-325 order.
4. method for calcinating according to claim 1, is characterized in that, described sylvite is Potassium ethanoate.
5. method for calcinating according to claim 1, is characterized in that, the mass ratio of described coal series kaolin rock and water is 1:3 ~ 5, and the mass ratio of described coal series kaolin rock and sylvite is 1:0.15 ~ 0.2.
6. method for calcinating according to claim 1, is characterized in that, in described step (3), the rotating speed of centrifugation is that 3000 ~ 5000r/ divides, and the time of centrifugation is 5 ~ 15 minutes.
7. method for calcinating according to claim 1, is characterized in that, in described step (4), is warming up to 350-450 DEG C with 5-15 DEG C/min, after constant temperature 2-2.5h; 600-700 DEG C is warming up to and constant temperature 0.5-1h again with 2 ~ 5 DEG C/min.
8. method for calcinating according to claim 7, is characterized in that, in described step (4), is warming up to 350-450 DEG C with 10 ~ 15 DEG C/min; 600-700 DEG C is warming up to again with 5 DEG C/min.
9. method for calcinating according to claim 1, it is characterized in that, in described finished product high reactivity superfine calcined kaolin, hexagonal flake kaolin crystal accounts for 20-50%, particle diameter D97≤2 μm of finished product superfine calcined kaolin, finished product superfine calcined kaolin wafer thickness is less than 200nm, and whiteness is higher than 90%.
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| CN103613296B (en) * | 2013-12-04 | 2015-09-09 | 重庆大学 | A kind of low temperature calcination intercalation kaolin soil prepares the method for alkali-activated carbonatite gelling material |
| CN110577225B (en) * | 2019-09-23 | 2022-07-08 | 山西金宇科林科技有限公司 | Preparation method of high-whiteness calcined kaolin with ultrahigh oil absorption |
| CN112516984A (en) * | 2020-12-23 | 2021-03-19 | 山西晋坤矿产品股份有限公司 | Method for preparing high-activity petroleum catalytic cracking catalyst by utilizing coal gangue |
| CN114261969A (en) * | 2021-12-25 | 2022-04-01 | 太原科技大学 | Preparation method of coal-series kaolin with high oil absorption |
| CN114436276B (en) * | 2022-01-20 | 2023-10-27 | 中国地质大学（武汉） | Method for rapidly extracting useful elements from aluminosilicate-containing minerals |
| CN114572990A (en) * | 2022-03-15 | 2022-06-03 | 太原理工大学 | Preparation method of calcined kaolin with high oil absorption value |
| CN114849654B (en) * | 2022-05-13 | 2023-03-17 | 成都理工大学 | Preparation method and adsorption application of oxalic acid intercalation expanded kaolin |
| CN115159580B (en) * | 2022-05-31 | 2023-05-12 | 中国矿业大学(北京) | Method for preparing jarosite by using coal gangue |
| CN115259146B (en) * | 2022-07-15 | 2023-05-02 | 中国矿业大学(北京) | Catalytic anthracite graphitization method |
| CN115449349B (en) * | 2022-08-19 | 2024-04-19 | 中国地质大学（武汉） | Carbon-coated aluminosilicate nano-sheet-based heat storage material and preparation method thereof |
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| CN1522959A (en) * | 2003-09-04 | 2004-08-25 | 湖北省葛店开发区地大创新材料有限公 | Method for preparing ultra-fine calcined kaolin by dry process using gangue as material |
| CN101293659A (en) * | 2007-04-24 | 2008-10-29 | 郑州大学 | Method for crystallization synthesis of L zeolite molecular sieve with kleit in situ |
| CN101746768A (en) * | 2009-12-29 | 2010-06-23 | 中国矿业大学(北京) | Coal-series hard kaolinite stripping method capable of keeping crystal form of kaolinite |
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| CN1522959A (en) * | 2003-09-04 | 2004-08-25 | 湖北省葛店开发区地大创新材料有限公 | Method for preparing ultra-fine calcined kaolin by dry process using gangue as material |
| CN101293659A (en) * | 2007-04-24 | 2008-10-29 | 郑州大学 | Method for crystallization synthesis of L zeolite molecular sieve with kleit in situ |
| CN101746768A (en) * | 2009-12-29 | 2010-06-23 | 中国矿业大学(北京) | Coal-series hard kaolinite stripping method capable of keeping crystal form of kaolinite |
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