CN114804133A - Method for calcining coal-series kaolin at low temperature and application thereof - Google Patents
Method for calcining coal-series kaolin at low temperature and application thereof Download PDFInfo
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- CN114804133A CN114804133A CN202110597417.0A CN202110597417A CN114804133A CN 114804133 A CN114804133 A CN 114804133A CN 202110597417 A CN202110597417 A CN 202110597417A CN 114804133 A CN114804133 A CN 114804133A
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- C01—INORGANIC CHEMISTRY
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- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
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Abstract
The invention relates to the field of kaolin preparation, in particular to a method for calcining coal-series kaolin at low temperature and application thereof, which comprises the following steps: after the coal-series kaolin is crushed, a whitening agent is added, the mixture is heated to 880-950 ℃ in a suspension calciner, and the calcined kaolin is obtained after heat preservation. In the method, the whitening agent accounts for 0.5-5 wt% of the coal-series kaolin, so that the content of iron after calcination can be reduced, the problem of fire resistance grade reduction caused by sodium chloride addition can be avoided, and the kaolin is endowed with good whiteness and fire resistance.
Description
Technical Field
The invention relates to the field of kaolin preparation, in particular to a method for calcining coal-series kaolin at a low temperature and application thereof.
Background
Kaolin is a silicon-aluminium oxide rich in kaolinite mineral phase, and the main chemical component of the Kaolin is SiO 2 And Al 2 O 3 . The main mineral phase of kaolin is kaolinite, and in addition, the kaolin also contains a part of quartz phase. Kaolin is a raw material for preparing geopolymer, and if the geopolymer is directly prepared from the Kaolin, the crystal phase structure is complete, the alkali activation effect is poor, the reaction is difficult, and the strength of the obtained test block is not high. In order to improve the reactivity of kaolin, the kaolin needs to be calcined and activated to destroy the crystal phase structure thereof so as to ensure that the kaolin is enabled to haveChanging from a crystalline phase to an amorphous phase. The influence of the calcination process on the crystal structure of kaolin is crucial. The whiteness is an important index for evaluating the kaolin calcination process, the higher the purity is, the higher the whiteness is, and the existence of metal oxides and organic impurities in the kaolin directly influences the whiteness, so that black spots appear after calcination and the quality of the kaolin is influenced.
CN111533440A discloses a method for producing calcined kaolin for glass fiber, which does not contain additives and saves the process cost, but the whiteness is not ideal and the content of impurity black spots is high.
CN109626385A discloses a method for preparing nano-grade calcined kaolin powder by utilizing coal gangue, wherein sodium chloride is selected as a whitening agent, so that the fire resistance of kaolin is reduced while the whiteness is improved.
CN201410504040A discloses a preparation method of high-whiteness superfine calcined kaolin, which has the heat preservation time of 10-12 hours and serious energy loss during calcination.
Therefore, it is very significant to develop a kaolin calcination process with higher whiteness and shorter holding time under the condition of low addition of the whitening agent.
Disclosure of Invention
The invention provides a method for calcining coal-series kaolin at low temperature, which comprises the steps of crushing the coal-series kaolin, adding a whitening agent, heating to 880-950 ℃ in a suspension calcining furnace, and preserving heat to obtain the calcined kaolin.
As a preferred embodiment, the average particle size after pulverization is not more than 0.05 mm.
As a preferred embodiment, the whitening agent is selected from at least one of sodium salt, magnesium salt, and ammonium salt.
As a preferred embodiment, the whitening agent comprises 0.5 to 5 wt% of the coal-series kaolin.
As a preferred embodiment, the whitening agent comprises a sodium salt.
As a preferred embodiment, the whitening agent further comprises an ammonium salt.
As a preferred embodiment, the weight ratio of the sodium salt to the ammonium salt is 1: (2-4). As a preferable embodiment, in the heating process of the suspension calciner, firstly heating to 720-860 ℃, adding a whitening agent, heating to 880-950 ℃, and preserving heat to obtain the calcined kaolin.
As a preferred embodiment, in the heating process of the suspension calciner, the suspension calciner is heated to 200-400 ℃ and is insulated for 5-8 min, heated to 720-860 ℃ and is insulated for 5-30min, added with a whitening agent, heated to 880-950 ℃ and is insulated for 5-35 min, and calcined kaolin is obtained.
The invention provides an application of calcined kaolin prepared by a method for calcining coal-series kaolin at low temperature in glass fibers or ceramic materials.
Compared with the prior art, the invention has the following beneficial effects:
1. in the method, the whitening agent accounts for 0.5-5 wt% of the coal-series kaolin, so that the content of iron after calcination can be reduced, the problem of fire resistance grade reduction caused by sodium chloride addition can be avoided, and the kaolin is endowed with good whiteness and fire resistance.
2. The method comprises the following steps of mixing sodium chloride and ammonium sulfate in a weight ratio of 1: (2-4) compared with the prior art, the compound preparation reduces the dosage of the whitening agent and improves the whiteness under the condition of low content of the whitening agent.
3. The invention adopts the gas suspension low-temperature calcination technology, is favorable for preparing the kaolin with high reaction activity, and is particularly suitable for preparing glass fiber, daily porcelain, building porcelain, extra-high voltage electric porcelain, alumina ceramic and the like.
4. In the heating process of the suspension decarburization calciner, the suspension decarburization furnace is heated to 720-860 ℃, the whitening agent is added, and then the suspension decarburization calciner is heated to 880-950 ℃, so that the problem of black spots in the calcined kaolin caused by adhesion and agglomeration in the calcining process can be effectively avoided, and the reduction of whiteness is avoided.
5. In the heating process of the suspension dehydroxylation calciner, the suspension dehydroxylation calciner is heated to 200-400 ℃, the temperature is kept for 5-8 min, then the suspension dehydroxylation calciner is heated to 720-860 ℃, the temperature is kept for 5-30min, then the suspension dehydroxylation calciner is heated to 880-950 ℃, the whitening agent is added, the temperature is kept for 5-35 min, and the suspension dehydroxylation calciner is divided into a plurality of partsCompared with the mode of heat preservation for 12 hours in the prior art, the mode of section heating and heat preservation can shorten the heat preservation time and reduce SO 3 The content of (b) improves the energy utilization rate and reduces the generation of side reactions and harmful products.
Detailed Description
In order to solve the above technical problems, a first aspect of the present invention provides a method for low-temperature calcination of coal-based kaolin, comprising: after the coal-series kaolin is crushed, a whitening agent is added, the mixture is heated to 880-950 ℃ in a suspension calciner, and the calcined kaolin is obtained after heat preservation.
As a preferred embodiment, the average particle size after pulverization is not more than 0.05 mm.
Preferably, the average particle size after pulverization is not more than 0.02 mm.
As a preferred embodiment, the whitening agent is selected from at least one of sodium salt, magnesium salt, and ammonium salt.
Preferably, the whitening agent is selected from at least one of sodium chloride, sodium sulfate, sodium sulfite, sodium carbonate, sodium bicarbonate, sodium nitrate, sodium nitrite, sodium acetate, sodium bromide, sodium fluoride, sodium iodide, sodium sulfide, sodium sulfite, sodium hypochlorite, sodium phosphate, sodium phosphite, sodium silicate, magnesium chloride, magnesium carbonate, magnesium bicarbonate, magnesium sulfate, magnesium acetate, magnesium silicate, ammonium sulfate, ammonium chloride, ammonium carbonate, ammonium bicarbonate, ammonium bromide, ammonium carbonate, ammonium phosphate, and ammonium iodide.
Preferably, the whitening agent comprises a sodium salt.
Preferably, the whitening agent further comprises an ammonium salt.
Preferably, the weight ratio of the sodium salt to the ammonium salt is 1: (2-4).
Preferably, the whitening agent accounts for 0.5-5 wt% of the coal-series kaolin.
Coal-based kaolin is a concomitance mineral resource which is most widely distributed in China, but because the whiteness of the kaolin is influenced by carbon, organic matters, iron and other metal impurities, the kaolin is generally required to be whitened by calcination, and generally, the higher the calcination temperature is, the higher the whiteness of the kaolin is, but resource waste and overburning are easily caused, so that a method for improving the whiteness while adopting low-temperature calcination is required to be provided, and the method is used for glass fibers or ceramic materials such as daily china, building porcelain, extra-high voltage electric porcelain, alumina ceramic and the like.
The inventors have surprisingly found that when using sodium and ammonium salts, in particular sodium chloride and ammonium sulphate, it is advantageous to obtain kaolin with a high whiteness at a lower addition and a lower calcination temperature, probably because at the calcination temperature, on the one hand sodium chloride and the like and the alumina in the kaolin give NaAlO 2 And ferric trichloride, which promotes the volatilization of iron, and on the other hand, the kaolin gas generated by the decomposition of ammonium sulfate forms a loose and porous structure, which promotes the permeation of air and the like and the volatilization of residual carbon, iron and the like, thereby obtaining the kaolin with low whiteness and iron content.
In addition, the inventor finds that the addition of sodium chloride is beneficial to the generation of ferric trichloride, but sodium element is also permeated into crystal lattices after the calcination to influence the fire-resistant grade, the reduction of the fire-resistant grade can be avoided by adding the ammonium sulfate with proper dosage to act together with the sodium chloride, the weight ratio of the sodium salt to the ammonium salt needs to be kept at proper ratio, and when the ammonium salt is used alone or the dosage of the ammonium salt is more, the calcination temperature needs to be further increased to more than 1000 ℃, a more loose and porous structure can be formed, so that high whiteness can be obtained.
As a preferable embodiment, in the heating process of the suspension calciner, firstly heating to 720-860 ℃, adding a whitening agent, heating to 880-950 ℃, and preserving heat to obtain the calcined kaolin.
In addition, the inventor finds that the addition time of the whitening agent during the calcination process has an important influence on the appearance and structure of the calcined kaolin, and ammonium sulfate generally begins to decompose at about 235 ℃ and can decompose to generate NH 3 、N 2 、SO 2 And water, but the inventors found that when a brightener of sodium chloride and ammonium sulfate is added at or above the decomposition temperature, the caking and adhesion phenomena of kaolin may be caused, and the whiteness is affected, and at the same time, the kaolin is not easy to be completely calcined, and black impurities and the like are remained.
The reason is probably that more ammonium sulfate is decomposed to generate gas, and simultaneously, part of the ammonium sulfate also has the effect of crystal water, organic matters, alumina and the like in the kaolin, and when the whitening agent is added after 720-860 ℃ and the heating rate is controlled, the sodium chloride, the ammonium sulfate and the like to be melted or melted have the effect, on one hand, the sodium chloride and the alumina have the effect of generating sodium chloride, on the other hand, the ammonium chloride and the like can also be obtained, the volatilization of the ammonium salt and the generation of gas are further promoted, the phenomena of agglomeration and the like are reduced, and the whiteness of the kaolin after low-temperature calcination is further improved.
As a preferred embodiment, in the heating process of the suspension calciner, the suspension calciner is heated to 200-400 ℃ and is insulated for 5-8 min, heated to 720-860 ℃ and is insulated for 5-30min, a whitening agent is added, the suspension calciner is heated to 880-950 ℃ and is insulated for 5-35 min, and calcined kaolin is obtained.
The inventor finds that the improvement of whiteness, iron content and the like is favorably improved when a higher temperature rise rate is adopted and a whitening agent is added, but the further improvement of whiteness and the reduction of sulfur content can be promoted only after the heating is carried out to 880-950 ℃ and a longer heat preservation time is needed, such as 60min, while the inventor finds that the heating is carried out to 880-950 ℃ after the heat preservation is carried out for a period of time at 200-400 ℃ and 720-860 ℃ respectively, the heat preservation and the calcination are favorably shortened, and the energy loss is reduced.
The reason for this is probably that after the temperature is kept at 200-400 ℃ for a period of time, the free water is promoted to be completely removed, then the heat is heated to remove the crystal water, organic matters, element iron, sulfur, iron and the like, and after the temperature is kept at 720-860 ℃ for a period of time, the impurity in the compact structure formed by mineralization in the kaolin can be promoted to be removed, so that the effects of the subsequent brightener and the like in the adding process are reduced, the sulfur is promoted to be removed in a short time, and the high-whiteness product is obtained in a short time at low temperature.
The inventor finds that when the heat preservation time and temperature are not proper, for example, the heat preservation time is 720-860 ℃, the heat preservation time is not reduced, and the sulfur content is not reduced in the subsequent calcining process.
The invention adopts the gas suspension low-temperature calcination technology, takes coal-series kaolin as a raw material, and carries out suspension calcination after crushing the kaolin into proper particle size, thereby being beneficial to preparing the kaolin with better reaction activity, being used for glass fiber to replace the currently used pyrophyllite raw material, and also being used for daily porcelain, building porcelain, ultra-high voltage electric porcelain, alumina ceramic and the like.
The invention provides an application of calcined kaolin prepared by a method for calcining coal-series kaolin at low temperature in glass fibers or ceramic materials.
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
In addition, the starting materials used are all commercially available, unless otherwise specified.
Examples
Example 1
The embodiment provides a method for calcining coal-series kaolin at low temperature, which comprises the following steps: crushing coal series kaolin, adding a whitening agent, heating to 950 ℃ in a suspension calciner, and preserving heat to obtain calcined kaolin.
The average particle size after pulverization was 0.02 mm.
The whitening agent accounts for 0.5 wt% of the coal-series kaolin.
The whitening agent is sodium chloride and ammonium sulfate, and the weight ratio of the whitening agent to the ammonium sulfate is 1: 2, compounding.
In the heating process of the suspension calciner, firstly heating to 400 ℃, preserving heat for 8min, heating to 860 ℃, preserving heat for 30min, heating to 950 ℃, adding a whitening agent, and preserving heat for 35min to obtain the calcined kaolin.
Example 2
The embodiment provides a method for calcining coal-series kaolin at low temperature, which comprises the following steps: crushing coal series kaolin, adding a whitening agent, heating to 880 ℃ in a suspension calciner, and preserving heat to obtain calcined kaolin.
The average particle diameter after pulverization was 0.005 mm.
The whitening agent accounts for 5 wt% of the coal-series kaolin.
The whitening agent is sodium chloride and ammonium sulfate, and the weight ratio of the whitening agent to the ammonium sulfate is 1: 4, compounding.
In the heating process of the suspension calciner, firstly heating to 200 ℃, preserving heat for 5min, then heating to 720 ℃, preserving heat for 5min, then heating to 880 ℃, adding a whitening agent, and preserving heat for 5min to obtain the calcined kaolin.
Example 3
The embodiment provides a method for calcining coal-series kaolin at low temperature, which comprises the following steps: crushing coal series kaolin, adding a whitening agent, heating to 900 ℃ in a suspension calciner, and preserving heat to obtain calcined kaolin.
The average particle diameter after pulverization is 0.01 mm.
The whitening agent accounts for 4 wt% of the coal-series kaolin.
The whitening agent is sodium chloride and ammonium sulfate, and the weight ratio of the whitening agent to the ammonium sulfate is 1: 3, compounding.
In the heating process of the suspension calciner, firstly heating to 260 ℃ and preserving heat for 7min, heating to 830 ℃ and preserving heat for 25min, heating to 900 ℃, adding a whitening agent, and preserving heat for 33min to obtain the calcined kaolin.
Example 4
The embodiment provides a method for calcining coal-series kaolin at low temperature, which comprises the following steps: crushing coal series kaolin, adding a whitening agent, heating to 900 ℃ in a suspension calciner, and preserving heat to obtain calcined kaolin.
The average particle size after pulverization was 0.015 mm.
The whitening agent accounts for 4 wt% of the coal-series kaolin.
The whitening agent is sodium chloride and ammonium sulfate, and the weight ratio of the whitening agent to the ammonium sulfate is 1: 2.5 compounding.
In the heating process of the suspension calciner, firstly heating to 265 ℃, preserving heat for 8min, heating to 840 ℃, preserving heat for 15min, heating to 910 ℃, adding a whitening agent, and preserving heat for 31min to obtain calcined kaolin.
Comparative example 1
The present comparative example provides a method for low-temperature calcination of coal-based kaolin, and the specific implementation manner is the same as that in example 3, except that the average particle size after pulverization is 0.1 mm.
Comparative example 2
This comparative example provides a method for low temperature calcination of coal-based kaolin, the specific embodiment being the same as example 3, except that the whitening agent comprises 10 wt% of the coal-based kaolin.
Comparative example 3
The present comparative example provides a method for low-temperature calcination of coal-based kaolin, which is the same as example 3 in the specific implementation manner, except that the whitening agent is sodium chloride and ammonium sulfate in a weight ratio of 1: 10 to prepare the mixture.
Comparative example 5
The specific implementation mode of the method is the same as that in example 3, except that in the heating process of the suspension calciner, the coal-based kaolin is heated to 260 ℃ and is kept warm for 7min, a whitening agent is added, the coal-based kaolin is heated to 830 ℃ and is kept warm for 40min, the coal-based kaolin is heated to 900 ℃ and is kept warm for 33min, and the calcined kaolin is obtained.
Comparative example 6
The specific implementation mode of the method is the same as that of example 3, except that the coal-based kaolin is heated to 260 ℃ and is kept warm for 20min, heated to 830 ℃ and is kept warm for 10min, added with a whitening agent, heated to 900 ℃ and kept warm for 33min to obtain the calcined kaolin.
Performance testing
Evaluation of kaolin grade: determination of Al with reference to GB/T14565 2 O 3 、Fe 2 O 3 、TiO 2 、SO 3 The content; the 63 μm sieve residue was determined with reference to GB/T14564; the detection result refers to GB/T14563-93, meets TC-0 index in kaolin for ceramics, and is shown in table I.
Evaluation of kaolin whiteness grade: reference is made to GB/T5950, wherein, preferably: > 90%, good: the whiteness is more than or equal to 85% in 90%, and the difference is as follows: less than or equal to 85 percent.
Appearance evaluation of kaolin: observing whether black spots exist inside the crushed calcined kaolin, wherein the black spots are as follows: no black spot, good: slightly black dots, poor: the number of black spots is large.
Kaolin refractoriness evaluation: after calcining at 1780 +/-10 deg.c, the kaolin has stable property and no change.
Watch 1
| Rating evaluation | Whiteness degree | Appearance evaluation | Degree of refractoriness | |
| Example 1 | TC-0 | Superior food | Superior food | Without change |
| Example 2 | TC-0 | Superior food | Superior food | Without change |
| Example 3 | TC-0 | Superior food | Superior food | Without change |
| Example 4 | TC-0 | Superior food | Superior food | Without change |
| Comparative example 1 | TC-2 | Good wine | Good wine | / |
| Comparative example 2 | TC-1 | Good wine | Difference (D) | / |
| Comparative example 3 | TC-2 | Good wine | Difference between | / |
| Comparative example 5 | TC-2 | Difference (D) | Difference (D) | / |
| Comparative example 6 | TC-2 | Good wine | Good wine | / |
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in other forms, and any person skilled in the art may modify or change the technical content of the above disclosure into equivalent embodiments with equivalent changes, but all those simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention still belong to the protection scope of the present invention.
Claims (10)
1. A method for calcining coal-series kaolin at low temperature is characterized in that the coal-series kaolin is crushed, added with a whitening agent, heated to 880-950 ℃ in a suspension calciner, and kept warm to obtain the calcined kaolin.
2. The method for low-temperature calcination of coal-based kaolin as claimed in claim 1, wherein the average particle size after pulverization is not greater than 0.05 mm.
3. The method for low-temperature calcination of coal-based kaolin according to claim 1, wherein the whitening agent is at least one selected from sodium salt, magnesium salt and ammonium salt.
4. The method for low-temperature calcination of coal-series kaolin as claimed in claim 1, wherein the whitening agent is 0.5-5 wt% of the coal-series kaolin.
5. The method for low-temperature calcination of coal-based kaolin as claimed in claim 3, wherein the whitening agent comprises sodium salt.
6. The method for low-temperature calcination of coal-based kaolin as claimed in claim 5, wherein the whitening agent further comprises an ammonium salt.
7. The method for low-temperature calcination of coal-based kaolin as claimed in claim 6, wherein the weight ratio of the sodium salt to the ammonium salt is 1: (2-4).
8. The method for calcining coal-based kaolin at low temperature as claimed in claim 1, wherein in the heating process of the suspension calciner, the calcined kaolin is obtained by heating to 720-860 ℃ first, adding a whitening agent, heating to 880-950 ℃ and preserving heat.
9. The method as claimed in claim 8, wherein in the heating process of the suspension calciner, the coal-based kaolin is heated to 200-400 ℃ and then is insulated for 5-8 min, then heated to 720-860 ℃ and then is insulated for 5-30min, and then added with a whitening agent and heated to 880-950 ℃ and then is insulated for 5-35 min, so as to obtain the calcined kaolin.
10. Use of the calcined kaolin prepared by the method of low temperature calcination of coal-based kaolin according to any one of claims 1 to 9 in glass fibers or ceramic materials.
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| CN111847468A (en) * | 2020-07-29 | 2020-10-30 | 东北大学 | Method for producing high-whiteness calcined kaolin by multi-stage suspension calcination of coal-series kaolin |
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- 2021-05-28 CN CN202110597417.0A patent/CN114804133A/en active Pending
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| CN1125193A (en) * | 1994-12-20 | 1996-06-26 | 陕西省科联新技术开发中心 | Production process for synthesizing high whiteness 4A zeolite using kaolin |
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