CN1281820A - Technological process for producing aluminium salt and silicate by using coal gangue - Google Patents
Technological process for producing aluminium salt and silicate by using coal gangue Download PDFInfo
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Abstract
the production process of aluminium salt and silicate by utilizing coal gangue is characterized by that is adopts the processes of alkali fusion, hydrolysis, carbonization, causticization and correspondent acid solving and alkali solving processes to obtain high-yield aluminium hydroxide and silicic acid, and can develop them into various aluminium salts and silicates with different specification. Said invented causticization process can recover and circularly use the caustic soda being in alkali fusion. Said invented technological line is reasonable, additional value of product is high, and said invented product can be used in the fields of environmental protection, paper-making, petroleum chemical and rubber and plastic industries.
Description
A process for producing aluminium salt and silicate by using coal gangue.
The invention relates to a method for chemical development and utilization of aluminosilicate minerals (coal gangue, clay, kaolin, bauxite, yellow sand and fly ash), in particular to a processmethod for producing aluminum salt and silicate by utilizing coal gangue.
According to the technical scheme that Feng Shi is called in inorganic salt industry journal of No. 4 of 1995, No. 22-24 pages of coal gangue for preparing aluminum salt and white carbon black (comparison document 1), the discharge amount of coal gangue in China reaches more than 22 hundred million tons, the discharge amount of coal gangue occupies about 1.3 hundred million tons, the discharge amount of coal gangue occupies about 1 thousand mu each year, chemical products are extracted from industrial waste coal gangue, waste is changed into wealth, the environment is improved to all countries in the world, more important industrial policy in China is provided, the coal gangue is basically composed of aluminosilicate, oxide containing a small amount of iron, calcium, titanium and the like, the content of each component varies from place to place, mainly silicon dioxide and aluminum trioxide account for 75-98% in total, the silicon dioxide component accounts for more than 50%, the comparison document 1 adopts acid leaching coal gangue and aluminum trioxide component therein to react with aluminum oxide to generate aluminum salt, ammonium salt is then added with ammonium salt, another more main component in coal gangue is not utilized, only as aluminum oxide, only the tail ammonium sulfate is used as an activator, the tail of aluminum sulfate, the tail sulfate is added, the tail of aluminum sulfate, the tail sulfate is added, the tail sulfate is added, the tail sulfate, the aluminum sulfate, the tail sulfate is added, the tail sulfate, the aluminum sulfate, the tail sulfate, the aluminum chloride, the tail sulfate is added, the tail sulfate, the tail of aluminum oxide, the aluminum chloride, the tail sulfate, the aluminum oxide, the tail sulfate is added, the aluminum oxide, the tail sulfate, the tail of aluminum oxide, the tail of aluminum oxide, the tail of.
The invention aims to improve the development and utilization method of coal gangue, so that the coal gangue has high resource utilization rate, flexible product types, low production cost and no secondary pollution.
The purpose of the invention is realized as follows: the invention relates to a process for producing aluminum salt and silicate by using coal gangue, which is characterized in that the aluminum salt and silicate and precipitated calcium carbonate are produced by adopting the processes of alkali fusion, hydrolysis, carbonization and causticization: (1) crushing coal gangue, roasting to remove carbon, activating, heating a water reservoir by flue gas generated by roasting and flue gas of a coal-fired furnace for heating other process sections below, drying a product, and washing to obtain carbon dioxide gas for later use; (2) mixing the roasted and decarbonized coal gangue powder with a circulating caustic soda (sodium hydroxide) solution, and then carrying out alkali fusion process treatment; (3) hydrolyzing the clinker treated by the alkali fusion process, performing filter pressing, and washing with hot water in a water reservoir heated by the flue gas to obtain a filter cake, namely aluminum hydroxide; (4) carrying out carbonization process treatment on the filtrate obtained by pressure filtration after alkali fusion-hydrolysis process treatment by using the obtained carbon dioxide gas, carrying out pressure filtration, and washing by using hot water in a water reservoir to obtain a filter cake, namely silicic acid; (5) causticizing the filtrate obtained by the alkali fusion-hydrolysis-carbonization process with lime (calcium oxide) obtained by reacting the quicklime (calcium oxide) with water, and then carrying out filter pressing to obtain a filtrate which is a caustic soda (sodium hydroxide) solution, concentrating the filtrate and then circularly returning the concentrated solution to the alkali fusion process section for use; (6) washing the filter cake obtained by the alkali fusion, hydrolysis, carbonization and causticization processes with hot water in a water reservoir to obtain calcium carbonate, and drying the obtained flue gas by using the waste heat to obtain precipitated calcium carbonate; (7) carrying out different acid dissolution processes on the aluminum hydroxide obtained by alkali fusion-hydrolysis to obtain corresponding aluminum salt; (8) and (3) carrying out different alkali dissolution process treatments on the silicic acid obtained by the alkali dissolution-hydrolysis-carbonization process to obtain the corresponding silicate.
FIG. 1 is a schematic view of the production process of the present invention.
With reference to fig. 1, the object of the invention is further achieved in that:
the raw materials in figure 1 refer to aluminosilicate minerals of different producing areas, such as coal gangue with aluminum oxide content not limited to be more than 35%, low-grade bauxite with aluminum-silicon ratio not limited, waste fly ash of thermal power plants, kaolin, clay and yellow sand. As long as the main components in the minerals are silicon dioxide and aluminum oxide, the main components can be used as raw materials in the implementation of the invention, and the coal gangue is coal mine waste polluting the environment, the coal gangue is preferably used as the raw material in the invention, the raw material in figure 1 is required to be crushed to the granularity of 80-120 meshes before being roasted, the roasting achieves the purposes of removing carbon and activating the raw material coal gangue, the carbonremoval and the activation are carried out in a reverberatory furnace or a fluidized bed furnace with the furnace temperature of 600 and 750 ℃, and combustible components in the coal gangue are utilized while the carbon removal and the activation are carried out, and the reaction activity is improved. The waste heat of the flue gas is used for heating hot water for washing in the water storage device for each subsequent process section, drying products needing heating and drying in the subsequent process section, and then washing to obtain carbon dioxide gas needed by the subsequent carbonization process section. In the alkali fusion process in the figure 1, the coal gangue powder after being roasted and decarbonized and activated and caustic soda (sodium hydroxide) are mixed according to the mass ratio of 1: 1.2-1.3 (according to the test result of coal gangue samples), the caustic soda is prepared into solution with the content of 50 percent and is uniformly mixed with the coal gangue powder, the mixture is carried out in an alkali fusion pot with the temperature of 400-plus-500 ℃, the reaction product is moved into a reaction disc when being viscous, and the reaction product is placed into a kiln with the temperature of 500-plus-600 ℃ to be baked into offwhite powdery clinker; in the hydrolysis process treatment in fig. 1, the clinker is put into a hydrolysis tank with hot water at 80 ℃ while the clinker is hot, after the clinker is sufficiently hydrolyzed, filter pressing is carried out, the clinker is washed with the hot water at 60-80 ℃ in the water reservoir until the pH value is 7-8, a filter cake is aluminum hydroxide, and the filtrate is sent to the next stage of carbonization process treatment; the carbonization process treatment in FIG. 1 is to carbonize the carbon dioxide gas obtained by washing the filtrate and flue gas in an absorption tower, the pH at the carbonization end point is approximately equal to 9, filter pressing is carried out, the filtrate is washed by hot water with the temperature of 60-80 ℃ in the water storage device until the pH is approximately equal to 7, the filter cake is silicic acid, and the filtrate is sent to the next stage of causticization process treatment; in the causticizing process shown in figure 1, the filtrate obtained by the carbonizing process and calcium hydroxide emulsion with the concentration of 13 Be' are causticized in a causticizing barrel with a stirrer, calcium carbonate produced by causticizing is sent to an oven to Be dried by the residual heat of flue gas when being washed by hot water with the temperature of 60-80 ℃ in a water storage device until the pH value is approximately equal to 7, so that precipitated calcium carbonate products are obtained, and caustic soda (sodium hydroxide) dilute solution generated by causticizing is sent to an evaporating pot to Be concentrated to a solution with the content of 50% and then sent to an alkali fusion process section for recycling. In fig. 1, the aluminum hydroxide is treated by acid dissolution process, different acid dissolution can be adopted, and corresponding aluminum salt is obtained by conventional process, and the following are selected in implementation: 1. adding 60 percent sulfuric acid with a certain proportion in an acid dissolving tank, stirring for reaction, performing filter pressing to obtain rough aluminum sulfate, performing a conventional purification process, and crystallizing to obtain crystalline aluminum sulfate which is one of aluminum salts; 2. adding hydrochloric acid with the concentration of 20% into the acid solution tank, stirring the solution to react, performing filter pressing to obtain rough aluminum chloride, purifying the rough aluminum chloride, and crystallizing the rough aluminum chloride to obtain crystalline aluminum chloride of aluminum salt II. Continuously heating the crystallized aluminum chloride at 170-180 ℃ to decompose and polymerize the crystallized aluminum chloride, thereby producing polyaluminum chloride; 3. adding a nitric acid solution with the content of 30% into an acid dissolving tank, stirring for reaction, completely dissolving an aluminum hydroxide filter cake, performing filter pressing to obtain crude aluminum nitrate, and performing conventional purification and crystallization processes to obtain crystalline aluminum nitrate of aluminum salt III; 4. adding 25% hydrofluoric acid solution into the acid solution tank, stirring for reaction, and filtering, purifying and crystallizing to obtain aluminum salt-IV crystal aluminum fluoride; 5. adding 32% phosphoric acid, controlling the temperature at 110 ℃, stirring in an acid dissolving tank, and obtaining the aluminum salt penta-powder aluminum dihydrogen phosphate through conventional processes of filtering, purifying and spray drying. In the figure 1, different alkali dissolution processes are carried out on silicic acid to obtain corresponding silicate, and the following steps are adopted in the implementation: 1. adding caustic soda (sodium hydroxide) with the purity of 98 percent, performing in an alkali dissolving tank with hot water at the temperature of 60-80 ℃ to completely dissolve filter-cake-shaped silicic acid, performing filter pressing to obtain filtrate which is a sodium silicate solution, concentrating the solution by an evaporating pot, and then obtaining crystalline sodium silicate which is one of silicates by a conventional crystallization process, wherein a filter cake is aluminum hydroxide and can be sent to the acid dissolution process section for producing aluminum salt; 2. putting potassium hydroxide with the purity of 98 percent into an alkali dissolving tank, heating to 80 ℃ to completely dissolve the filter cake-shaped silicic acid, and obtaining potassium silicate of silicate II through conventional filtration and concentration; 3. adding aluminum hydroxide with the purity of 96 percent, fully and uniformly mixing, heating to 100 ℃ to fully react, and obtaining the aluminosilicate of the silicate after conventional filtration, washing, drying and crushing. Adding aluminum hydroxide and corresponding alkali in required proportion into cleaned silicic acid, mixing uniformly, heating at 100 deg.C for complete reaction, crystallizing, filtering, washing, drying, molding, and activating to obtain the molecular sieve with required specification and model. 4. Adding mixed solution of caustic soda and caustic potash (sodium hydroxide and potassium hydroxide) into the cleaned silicic acid, heating to 80 deg.C for complete reaction, filtering, and concentrating to obtain sodium potassium silicate tetrahydrate. 5. Adding 60 ℃ hot water into the washed silicic acid, fully stirring to form silica sol again, precipitating for 48 hours, and then processing and manufacturing according to various different silica gel production modes to obtain the silica gels with various specifications. The washed silicic acid is dried to obtain precipitated white carbon black, the precipitated white carbon black is classified and processed to obtain white carbon black with various specifications, compared with the production process of the tailings white carbon black in the reference, the method does not need to add an activating agent for modification reaction, and has high purity and good quality.
The following is the chemistry in each process flow in figure 1:
alkali fusion:
hydrolysis:
carbonizing:
causticizing:
acid dissolution:
alkali dissolution:
in the figure 1, the flue gas not only collects the flue gas generated in the process of roasting coal gangue, but also collects the flue gas of all the coal-fired furnaces needing to be heated in other process sections, firstly heats hot water in a water reservoir for each process section, then utilizes the waste heat of an oven for drying calcium carbonate in a causticization process section, and obtains carbon dioxide gas required by a carbonization process section through water washing, thereby improving the energy utilization rate.
The invention has the following effects after practical trial: 1. the resource utilization rate of coal gangue and similar aluminosilicate minerals is high, and compared with the references 1, 2 and 3, the alumina component accounting for 30-40% is utilized, and the silicon dioxide component accounting for 50-60% is utilized; 2. because the aluminum hydroxide is obtained by the alkali fusion-hydrolysis process and the silicic acid is obtained by the carbonization process, the aluminum salt and silicate products with various types and specifications and capable of meeting the market requirements can be obtained by the known acid fusion and alkali fusion processes, and the aluminum salt and silicate products with high added value can be easily obtained in commerce by applying the method disclosed by the invention, so that the product with high market competitiveness can be easily selected; 3. compared with the methods for developing and utilizing coal gangue in the comparison documents 1, 2 and 3, on one hand, because the resource utilization rate is high, the components of aluminum oxide and silicon dichloride are developed and utilized, on the other hand, the process flow is simple and the yield is high, and in addition, the energy utilization rate of flue gas and waste heat is high as described above, and the process lines of alkali fusion, hydrolysis, carbonization and causticization are reasonable, the caustic soda in the alkali fusion process is recycled and recycled in the causticization process, and the carbon dioxide gas obtained after the flue gas is washed by water is reasonably used in the carbonization, so the cost of the obtained aluminum hydroxide and silicic acid is greatly reduced compared with the production cost of other domestic and foreign process methods; 4. compared with the reference documents 1, 2 and 3, the flue gas in the process of the invention is sealed and recycled, so that volatile toxic and harmful gas is not generated, the washing water for cleaning the flue gas and the washing hot water in each process section are both treated and recycled slightly, the utilization rate of coal gangue resources is high, and no solid waste is generated, so that the implementation of the invention does not cause secondary pollution to the environment.
The aluminum salt, silicate and precipitated calcium carbonate products obtained by the implementation of the invention, and white carbon black, silica gel and other products directly obtained from silicic acidand aluminum hydroxide can be flexibly selected according to market changes and adjustment of industrial policies in the types and specifications, and the products can be used in the industries of environmental protection, rubber, plastics, papermaking, printing and dyeing, daily chemical detergents, petroleum, fire fighting, paint, coating, tanning, metallurgy, glass and medicine.
Claims (13)
1. A process for producing aluminum salt and silicate by using coal gangue is characterized in that the process for producing aluminum salt, silicate and precipitated calcium carbonate by adopting alkali fusion, hydrolysis, carbonization and causticization is as follows:
(1) crushing coal gangue, roasting to remove carbon, activating, heating flue gas generated by roasting and flue gas generated by a coal-fired furnace for heating other process sections below, heating a water reservoir, and washing to obtain carbon dioxide gas for later use;
(2) mixing the roasted and decarbonized and activated coal gangue powder with circulating caustic soda (sodium hydroxide) solution, and then carrying out alkali fusion process treatment;
(3) hydrolyzing the clinker treated by the alkali fusion process, then performing filter pressing, and washing with hot water in a water reservoir heated by the flue gas to obtain a filter cake, namely aluminum hydroxide;
(4) performing carbonization treatment on the filtrate obtained by pressure filtration after alkali fusion-hydrolysis treatment by using the obtained carbon dioxide gas, performing pressure filtration, and washing by using hot water in the water reservoir to obtain a filter cake, namely silicic acid;
(5) causticizing the filtrate obtained by the alkali fusion-hydrolysis-carbonization process by lime (calcium oxide) and water to obtain lime milk (calcium hydroxide), then carrying out filter pressing, washing by hot water in the obtained water reservoir, concentrating the filtrate, and circularly returning the concentrated filtrate to the alkali fusion process section for use;
(6) drying the filter cake obtained by the alkali fusion, hydrolysis, carbonization and causticization processes by the waste heat of the obtained flue gas to obtain precipitated calcium carbonate;
(7) carrying out different acid dissolution processes on the aluminum hydroxide obtained by the alkali fusion-hydrolysis process to obtain corresponding aluminum salt;
(8) and (3) carrying out different alkali dissolution processes on the silicic acid obtained by the alkali fusion-hydrolysis-carbonization processes to obtain the corresponding silicate.
2. The method according to claim 1, characterized in that the pulverized particle size of the coal gangue before roasting and carbon removal is 80-120 mesh.
3. The method as claimed in claim 1 or 2, wherein the calcination, carbon removal and activation of the coal gangue are performed in a reverberatory furnace or a fluidized bed furnace at a furnace temperature of 600 ℃ and 750 ℃.
4. The method as claimed in claim 1, wherein the alkali fusion process comprises the steps of mixing the coal gangue powder subjected to carbon removal and activation by roasting with sodium hydroxide (sodium hydroxide) according to a mass ratio of 1: 1.2-1.3 (according to the test result of a coal gangue sample), preparing a solution with the content of 50% by using the sodium hydroxide, uniformly mixing the solution with the coal gangue powder, reacting in an alkali fusion pot at the temperature of 400 ℃ and 500 ℃, moving the reaction material into a reaction disc when the reaction material is viscous, and baking in a kiln at the temperature of 500 ℃ and 600 ℃ until the reaction material is gray powdery clinker.
5. The method according to claim 1, characterized in that the hydrolysis process treatment is to put the clinker after the alkali fusion treatment into a hydrolysis tank at 80 ℃ while the clinker is hot, filter-press the clinker after sufficient hydrolysis, wash the clinker with hot water at 60-80 ℃ in the water reservoir until the pH is 7-8, the filter cake is aluminum hydroxide, and send the filtrate to the next stage of carbonization process treatment.
6. The method according to claim 1, characterized in that the carbonization process treatment is to carbonize the filtrate obtained by pressure filtration after alkali fusion-hydrolysis process treatment and carbon dioxide gas obtained by flue gas water washing in an absorption tower, the pH at the carbonization end point is approximately equal to 9, pressure filtration is carried out, the filtrate is washed by hot water of the water reservoir at 60-80 ℃ until the pH is approximately equal to 6-7, the filter cake is silicic acid, and the filtrate is sent to the next stage of causticization process treatment.
7. The method according to claim 1, characterized in that the causticizing process treatment is carried out by causticizing the filtrate obtained by alkali fusion-hydrolysis-carbonization process treatment and calcium hydroxide emulsion with concentration of 13 Be' in a causticizing barrel with a stirrer, washing the calcium carbonate generated by causticizing in hot water of 60-80 ℃ in the water storage device until the pH value isapproximately equal to 7, drying the calcium carbonate in an oven by using the residual heat of flue gas, concentrating the sodium hydroxide diluted solution generated by causticizing in an evaporating pot to 50% solution, and then sending the solution to the alkali fusion process section for recycling.
8. The method according to claim 1, characterized in that one of said different acid dissolution processes on the aluminium hydroxide is to add a proportional amount of skipped sulphuric acid in an acid dissolution tank with stirring, to obtain crude aluminium sulphate by pressure filtration, to obtain further purification and to obtain crystalline aluminium sulphate, one of the aluminium salts, by a crystallization process.
9. The method according to claim 1, characterized in that one of the different alkali dissolution processes performed on the silicic acid is to put caustic soda (sodium hydroxide) with a purity of 98%, to be performed in an alkali dissolution tank with hot water at 60-80 ℃ to completely dissolve the silicic acid in the form of filter cake, to obtain a filter cake of aluminum hydroxide and a filtrate of sodium silicate solution by pressure filtration, to be concentrated by an evaporator, to obtain crystalline sodium silicate, which is one of the silicates, by a crystallization process, and to use the filter cake of aluminum hydroxide in the acid dissolution process section.
10. The method according to claim 1, characterized in that the second different acid dissolution process for aluminum hydroxide is to add hydrochloric acid with a concentration of 20% in the acid dissolution tank and stir, filter press to obtain crude aluminum chloride, purify, and crystallize to obtain crystalline aluminum chloride of the second aluminum salt.
11. The method of claim 1, wherein the second of the different alkali dissolution processes for silicic acid is to add potassium hydroxide with 98% purity into an alkali dissolution tank, heat the tank to 80 ℃ to dissolve all the silicic acid in the form of filter cake, filter and concentrate the solution to obtain potassium silicate of the second silicate.
12. The method of claim 1, wherein the third step of subjecting the aluminum hydroxide to different acid dissolution processes is to add a nitric acid solution with a content of 30% and stir the solution in an acid dissolution tank to completely dissolve the cake-shaped aluminum hydroxide, filter-press the solution to obtain crude aluminum nitrate, and purify and crystallize the crude aluminum nitrate to obtain the crystalline aluminum nitrate of the third aluminum salt.
13. The method of claim 1, characterized in that the third step of subjecting silicic acid to different alkali dissolution processes is to add aluminum hydroxide with a purity of 96% and mix them thoroughly, heat it to 100 ℃ for sufficient reaction, filter, wash, dry and pulverize to obtain aluminosilicate silicate.
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| GB2453799A (en) * | 2007-10-16 | 2009-04-22 | Christopher Strevens | A chemical method of extracting aluminium and iron from soil, rock and clay |
| CN101857253B (en) * | 2009-04-09 | 2012-06-06 | 刘庆玲 | Process for producing aluminium hydroxide, silicic acid and sodium carbonate by utilizing fly ash |
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