CN111072035B - Complete equipment for producing sodium-free silica sol by incineration of silicon-containing ash and recycling treatment - Google Patents
Complete equipment for producing sodium-free silica sol by incineration of silicon-containing ash and recycling treatment Download PDFInfo
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- CN111072035B CN111072035B CN202010047033.7A CN202010047033A CN111072035B CN 111072035 B CN111072035 B CN 111072035B CN 202010047033 A CN202010047033 A CN 202010047033A CN 111072035 B CN111072035 B CN 111072035B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/141—Preparation of hydrosols or aqueous dispersions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/146—After-treatment of sols
- C01B33/148—Concentration; Drying; Dehydration; Stabilisation; Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/146—After-treatment of sols
- C01B33/148—Concentration; Drying; Dehydration; Stabilisation; Purification
- C01B33/1485—Stabilisation, e.g. prevention of gelling; Purification
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Abstract
The invention discloses complete equipment for producing sodium-free silica sol by recycling treatment of incineration of siliceous ash, which comprises an ash storage tank, a high-speed shearing and activating machine, a heating and pressurizing digestion tank, a first sulfuric acid storage tank, a centrifugal machine, a centrifugal liquid tank, a centrifugal material tank, a single screw pump conveyor, a silica sol reaction tank, a catalyst storage tank, a second sulfuric acid storage tank, salt bath circulation heating equipment, a discharge tank, a filter, a slag filtering tank, a liquid filtering tank, an evaporation and concentration unit, a cooler, a metering filling machine and a silica sol product storage tank. The invention directly uses sulfuric acid and catalyst to react the pretreated and impurity-removed incineration siliceous dust to generate sodium-free silica sol, and compared with the traditional method for producing silica sol by using sodium silicate as raw material and industrial silicon as raw material, the invention has the advantages of simple process flow, no sodium, good product quality, low cost and large production scale superior to the silica sol produced by the traditional method.
Description
Technical Field
The invention relates to the field of comprehensive utilization of solid waste (including hazardous waste) of incineration of siliceous ash residue recycling treatment, in particular to the field of sodium-free silica sol preparation, and in particular relates to complete equipment for producing sodium-free silica sol by incineration of siliceous ash residue recycling treatment.
Background
The traditional incineration of the siliceous ash slag does not belong to the hazardous waste mainly for manufacturing cement, bricks, building blocks and other building materials, belongs to the hazardous waste, is used for solidifying heavy metals together with a cross-linking agent, is used for landfill treatment after cement solidification, or is also used for landfill treatment after glass melting, and belongs to harmless treatment. It is also added to cement as an ingredient in an amount of not more than 15% by weight for firing the cement. Belongs to a low added value treatment method.
The raw material required by the traditional silica sol production is sodium silicate (also called water glass and sodium silicate), and the alkaline silica sol is obtained by adopting an ion exchange resin to remove most sodium after dilution and then concentrating the sodium. In addition, sodium in sodium silicate is neutralized with sulfuric acid to form sodium sulfate, and the sodium sulfate is separated by solvent extraction and then concentrated to obtain silica sol. Still another method is to dissolve metallic silicon in water and neutralize it with ammonia, which is particularly costly although sodium-free. (Manual of chemical products, inorganic chemical products P465-P468)
The solid waste of burning silicon ash slag is used as raw material, the impurity Fe, al, ca, mg, K, na is dissolved out with sulfuric acid, and then the silicon sol is prepared by high-temperature high-pressure catalytic reduction method. The sodium-free silica sol has the advantages of improving the product quality, using waste as raw materials, along with low cost and low selling price, and widening the application field of the silica sol.
Disclosure of Invention
The traditional theory holds that only metal silicon and sodium silicate are used as raw materials, but no report is made on the production of the silica sol by the reaction of sulfuric acid and a catalyst with silicon dioxide, namely 2018.4 of the third volume of science publishers of the division of silicon and germanium in the book of inorganic chemistry.
The invention breaks the forbidden zone, and the pure silicon dioxide after the silicon-containing ash slag is subjected to high-speed shearing mechanochemical activation on the basis of incineration thermal activation and cold activation in the water or normal-temperature air conveying process is subjected to high-temperature high-pressure catalytic reduction reaction with sulfuric acid after further loosening the bonding bonds of the silicon and other components and then carrying out pretreatment with sulfuric acid to remove other impurities Fe, ae, ca, mg, K, na; wherein two hydrogen ions dissociated in water attack oxygen atoms in the silica to form a molecule of water, irreversible. The sulfate radical is reduced to sulfide ion under the action of catalyst and reacts with silicon to form silica sol of mixed silica disulfide and silica.
The chemical reaction formula is as follows: single type
H 2 SO 4 →2H + +SO 4 ＝ SO 4 2- +2M→S 2- +2M + ·O 2
SiO 2 +4H + +S 2- →2H 2 O+SiS 2
Also have partial reaction to form SiO 2 、SiS 2 Mixed silica sol
SiO 2 +4H + +2S 2- →2H 2 O+SiS 2 ·SiO 2
M + Metal oxide catalysts in the substate such as FeO, mnO, cuO in the lower substate, and the like.
The invention is an original innovation theoretical principle innovation and a technical process innovation.
The invention aims to solve the following technical problems:
1. solves the problem of low added value of the traditional cement and building material utilization of the burnt siliceous ash, and realizes high-value utilization.
2. The method solves the problems that the traditional method for producing the sodium-containing silica sol by using sodium silicate as a raw material has poorer quality than the sodium-free silica sol, has complex production process, high cost, low yield and high selling price, and limits the application range of the silica sol.
3. The traditional sodium-free silica sol uses metallic silicon as a raw material and is neutralized by ammonia, but the cost is extremely high, and the sodium-free silica sol can only be used in special occasions, so that the application range of the sodium-free silica sol is limited.
The technical problems to be solved by the invention can be realized by the following technical scheme:
a complete set of equipment for producing sodium-free silica sol by incinerating siliceous ash comprises an ash storage tank, a high-speed shearing activator, a heating and pressurizing digestion tank, a first sulfuric acid storage tank, a centrifuge, a centrifugal liquid tank, a centrifugal material tank, a single screw pump conveyor, a silica sol reaction tank, a catalyst storage tank, a second sulfuric acid storage tank, a salt bath circulation heating device, a discharging tank, a filter, a slag filtering tank, a liquid filtering tank, an evaporation concentration unit, a cooler, a metering filling machine and a silica sol product storage tank; the outlet of the ash storage tank is connected with the inlet of the high-speed shearing and activating machine, the outlet of the high-speed shearing and activating machine is connected with one inlet of the heating and pressurizing digestion tank, and the other inlet of the heating and pressurizing digestion tank is connected with the outlet of the first sulfuric acid storage tank; the outlet of the heating and pressurizing digestion tank is connected with the inlet of the centrifugal machine, the centrifugal liquid phase outlet of the centrifugal machine is connected with the inlet of the centrifugal liquid tank, the centrifugal solid phase outlet of the centrifugal machine is connected with the inlet of the centrifugal tank, and the outlet of the centrifugal tank is connected with the inlet of the single screw pump conveyor;
two inlets of the silica sol reaction tank are respectively connected with an outlet of the catalyst storage tank and an outlet of the single-screw pump conveyor, and an outlet and an inlet of a heating coil in the silica sol reaction tank are respectively connected with an inlet and an outlet of the salt bath circulation heating equipment; the outlet of the silica sol reaction tank is connected with the inlet of the discharging tank; the outlet of the discharge tank is connected with the inlet of the filter, and the filter residue outlet and the filtrate outlet of the filter are respectively connected with the inlet of the slag filtering tank and the inlet of the filtrate tank;
the outlet of the filtrate tank is connected with the inlet of the evaporation concentration unit, the water outlet of the evaporation concentration unit is connected with the cooler, the product outlet of the evaporation concentration unit is connected with the inlet of the metering filling machine, and the outlet of the metering filling machine is connected with the silica sol product storage tank;
the incineration siliceous ash in the ash storage tank enters the high-speed shearing activator for treatment and then enters the heating and pressurizing digestion tank to be activated with sulfuric acid from the first sulfuric acid storage tank, and the activated incineration siliceous ash is obtained after non-silicon impurity components are removed; centrifugally separating the activated incineration siliceous dust slag by a centrifugal machine, enabling centrifugally separated centrifugal liquid phase to enter a centrifugal liquid tank for standby, and enabling centrifugally separated centrifugal solid phase to enter the centrifugal liquid tank;
the centrifugal solid phase in the centrifugal liquid tank enters the silica sol reaction tank through the single screw pump conveyor, and together with sulfuric acid from the second sulfuric acid storage tank and catalyst from the catalyst storage tank, silica sol reaction is carried out in the silica sol reaction tank to obtain crude silica sol solution, a heat source in the silica sol reaction tank is from a coil in the silica sol reaction tank, and heat of the coil in the silica sol reaction tank is from the salt bath circulation heating equipment;
the crude silica sol solution enters the discharging tank, the crude silica sol solution in the discharging tank is filtered by a filter, filtered filter residues enter the residue filtering tank for additional treatment, and filtered filtrate enters the filtrate tank; the filtrate in the filtrate tank is sent into the evaporation concentration unit for evaporation concentration; and cooling and recycling the evaporated and concentrated water by a cooler, and enabling the evaporated and concentrated silica sol product to enter the silica sol product storage tank through the metering canning machine for warehousing.
Compared with the traditional method, the sodium-free silica sol produced by the innovative method has the following advantages:
1. the raw materials used in the innovative method are incineration of the siliceous ash and the sulfuric acid and the reduction catalyst; one or two of ferrous oxide, manganous oxide, cuprous oxide and the like are cheaper than the traditional method which adopts raw materials of anion-cation exchange resin and sodium silicate (water glass). The sulfuric acid is consumed completely to become a component part of the silica sol, so that the product yield and the product quality are increased.
2. The inventive method does not need to dilute in a large proportion in the traditional method, and concentrate in a large proportion after removing sodium by using ion exchange resin or sulfuric acid. Only a certain concentration of sulfuric acid is used for low-temperature low-pressure pretreatment to dissolve out impurities, then high-temperature high-pressure catalytic reduction reaction is carried out, and the concentration and dehydration ratio is not large. The difference in energy consumption is not too great. The energy consumption of the invention is slightly higher than that of the traditional method, but the comprehensive cost is low.
3. The product of the invention is sodium-free silica sol, and solves the problem of extremely high production cost of producing sodium-free silica sol by using traditional metallic silicon as a raw material. The traditional sodium-free silica sol uses industrial metal silicon as a main raw material, the ton price exceeds ten thousand yuan, the cost is too high, the sodium-free silica sol can only be used as an adhesive in special occasions of the electronic industry, and the application range of the sodium-free silica sol is seriously influenced due to the small dosage.
4. The low-cost sodium-free silica sol solves the problem of small application area of the high-cost sodium-free silica sol, can be widely applied to anti-corrosion materials and waterproof materials, is used for making artificial stone and excellent adhesive by utilizing waste stone and powder, is used as a water-soluble silica fertilizer with wide application in agriculture, can increase the yield and quality of agricultural products, lightens the damage of plant diseases and insect pests and reduces the application of chemical pesticides.
Drawings
FIG. 1 is a schematic diagram of an apparatus for producing sodium-free silica sol by recycling incineration of silica-containing ash.
FIG. 2 is a process flow diagram of an apparatus for producing sodium-free silica sol by utilizing incineration of silica-containing ash as a resource.
Detailed Description
The invention will be further described with reference to the accompanying drawings and examples.
Referring to fig. 1, the complete equipment for producing sodium-free silica sol by recycling treatment of incineration of siliceous ash residues is shown in the drawing and comprises an ash residue storage tank 1, a high-speed shearing and activating machine 2, a heating and pressurizing digestion tank 3, a first sulfuric acid storage tank 4, a centrifugal machine 5, a centrifugal liquid tank 6, a centrifugal material tank 7, a single screw pump conveyor 8, a silica sol reaction tank 9, a catalyst storage tank 10, a second sulfuric acid storage tank 11, a salt bath circulation heating device 12, a material discharging tank 13, a filter 14, a slag filtering tank 15, a liquid filtering tank 16, an evaporation and concentration unit 17, a cooler 18, a metering filling machine 19 and a silica sol product storage tank 20.
The outlet of the ash storage tank 1 is connected with the inlet of the high-speed shearing activator 2, the outlet of the high-speed shearing activator 2 is connected with one inlet of the heating and pressurizing digestion tank 3, and the other inlet of the heating and pressurizing digestion tank 3 is connected with the outlet of the first sulfuric acid storage tank 4; the outlet of the heating and pressurizing digestion tank 3 is connected with the inlet of a centrifugal machine 5, the centrifugal liquid phase outlet of the centrifugal machine 5 is connected with the inlet of a centrifugal liquid tank 6, the centrifugal solid phase outlet of the centrifugal machine 5 is connected with the inlet of a centrifugal material tank 7, and the outlet of the centrifugal material tank 7 is connected with the inlet of a single screw pump conveyor 8;
two inlets of the silica sol reaction tank 9 are respectively connected with an outlet of the catalyst storage tank 10 and an outlet of the single screw pump conveyor 8, and an outlet and an inlet of a heating coil in the silica sol reaction tank 9 are respectively connected with an inlet and an outlet of the salt bath circulation heating equipment 12; the outlet of the silica sol reaction tank 9 is connected with the inlet of the discharge tank 13; the outlet of the discharge tank 13 is connected with the inlet of the filter 14, and the filter residue outlet and the filtrate outlet of the filter 14 are respectively connected with the inlet of the slag filtering tank 15 and the inlet of the filtrate tank 16;
the outlet of the filtrate tank 16 is connected with the inlet of the evaporation and concentration unit 17, the water outlet of the evaporation and concentration unit 17 is connected with the cooler 18, the product outlet of the evaporation and concentration unit 17 is connected with the inlet of the metering and filling machine 19, and the outlet of the metering and filling machine 19 is connected with the silica sol product storage tank 20.
The invention sends the burned silicon-containing ash in the ash storage tank 1 into the high-speed shearing and activating machine 2 for high-speed shearing and activating treatment, and the revolution of the high-speed shearing and activating machine 2 is 5000 rpm.
Then the burned silica-containing ash slag treated by the high-speed shearing and activating machine 2 is sent into a heating and pressurizing digestion tank 3, sulfuric acid in a first sulfuric acid storage tank 4 is added into the heating and pressurizing digestion tank 3 to perform heating and pressurizing digestion of iron, aluminum, calcium, magnesium, potassium, sodium and other trace metal impurity components, and then the mixture is sent into a centrifugal machine 5 for centrifugal separation.
And delivering the centrifugal liquid phase impurities centrifugally separated by the centrifugal machine 5 into a centrifugal liquid tank 6 for further treatment. The centrifugal solid phase centrifugally separated by the centrifugal machine 5 is activated burned silicon-containing ash slag, and is sent into a centrifugal charging bucket 7
The mass percentage concentration of sulfuric acid used for heating and pressurizing dissolution in the heating and pressurizing dissolution tank 3 is 20%, the solid-liquid ratio is 1:3, the pressure is controlled at 0.5Mpa, and the dissolution time is 3h.
The activated incineration silica-containing ash slag in the centrifugal charging bucket 7 is sent into a silica sol reproduction tank 9 through a single screw pump conveyor 8, and is reacted with sulfuric acid sent from a second sulfuric acid storage tank 11 and catalyst sent from a catalyst storage tank 10 together. The addition of the catalyst in the silica sol reaction is 2 per mill of the activated silica dry basis for burning the silica ash containing silicon ash, the mass percentage concentration of the added sulfuric acid is 30 percent, the addition is 3 times of the weight of the activated silica dry basis for burning the silica ash containing silicon ash, the temperature of cyclic heating and indirect heating by using a salt bath is controlled at 350 ℃, the reaction temperature of the silica sol is controlled at 250 ℃, the pressure is controlled at 2.5Mpa, and the dissolution time is 2h. The heat source in the silica sol reaction tank 9 comes from a salt bath circulation heating device 12.
The crude silica sol solution after the reaction is sent into a discharge tank 13 and then is filtered by a filter 14, the filter medium of the filter 14 is polyvinylidene fluoride fiber, and the filtering speed is 5m/h. The filtering period is 15h, and the water quantity is backwashedIs 1m 3 /m 3 Min. After filtration, the residue impurities are sent into a residue filtering tank 15 for further treatment. The filtrate, i.e. the silica sol solution, is sent into a filtrate tank 16 and then into an evaporation and concentration unit 17 for vacuum evaporation and concentration, and the concentration of the concentrated silica sol is 30 percent, and the concentration of the concentrated silica sol and other indexes completely meet the chemical industry standard HG/T2521-2008 acidic industrial silica sol standard. (B) A & lt- & gt. The concentration of the concentrated silica sol is measured by a measuring filling machine 19 and then is sent into a silica sol product storage tank 20, and the water after vacuum evaporation and concentration is sent into a cooler 18 for cooling and recycling.
The above examples are provided to further illustrate the present invention, but should not be construed as limiting the scope of the invention, and the conditions in the examples may be further modified according to specific conditions, and simple modifications to the method of the present invention under the premise of the inventive concept are all within the scope of the invention claimed.
Claims (1)
1. The complete equipment for producing the sodium-free silica sol by the resource treatment of burning the siliceous ash is characterized by comprising an ash storage tank, a high-speed shearing and activating machine, a heating and pressurizing digestion tank, a first sulfuric acid storage tank, a centrifugal machine, a centrifugal liquid tank, a centrifugal material tank, a single screw pump conveyor, a silica sol reaction tank, a catalyst storage tank, a second sulfuric acid storage tank, a salt bath circulation heating device, a discharge tank, a filter, a slag filtering tank, a liquid filtering tank, an evaporation and concentration unit, a cooler, a metering filling machine and a silica sol product storage tank; the outlet of the ash storage tank is connected with the inlet of the high-speed shearing and activating machine, the outlet of the high-speed shearing and activating machine is connected with one inlet of the heating and pressurizing digestion tank, and the other inlet of the heating and pressurizing digestion tank is connected with the outlet of the first sulfuric acid storage tank; the outlet of the heating and pressurizing digestion tank is connected with the inlet of the centrifugal machine, the centrifugal liquid phase outlet of the centrifugal machine is connected with the inlet of the centrifugal liquid tank, the centrifugal solid phase outlet of the centrifugal machine is connected with the inlet of the centrifugal material tank, and the outlet of the centrifugal material tank is connected with the inlet of the single screw pump conveyor;
two inlets of the silica sol reaction tank are respectively connected with an outlet of the catalyst storage tank and an outlet of the single-screw pump conveyor, and an outlet and an inlet of a heating coil in the silica sol reaction tank are respectively connected with an inlet and an outlet of the salt bath circulation heating equipment; the outlet of the silica sol reaction tank is connected with the inlet of the discharging tank; the outlet of the discharge tank is connected with the inlet of the filter, and the filter residue outlet and the filtrate outlet of the filter are respectively connected with the inlet of the slag filtering tank and the inlet of the filtrate tank;
the outlet of the filtrate tank is connected with the inlet of the evaporation concentration unit, the water outlet of the evaporation concentration unit is connected with the cooler, the product outlet of the evaporation concentration unit is connected with the inlet of the metering filling machine, and the outlet of the metering filling machine is connected with the silica sol product storage tank;
the incineration siliceous ash in the ash storage tank enters the high-speed shearing activator for treatment and then enters the heating and pressurizing digestion tank to be activated with sulfuric acid from the first sulfuric acid storage tank, and the activated incineration siliceous ash is obtained after non-silicon impurity components are removed; centrifugally separating the activated incineration siliceous dust slag by a centrifugal machine, enabling centrifugally separated centrifugal liquid phase to enter a centrifugal liquid tank for standby, and enabling centrifugally separated centrifugal solid phase to enter the centrifugal charging bucket;
the centrifugal solid phase in the centrifugal charging bucket enters the silica sol reaction tank through the single screw pump conveyor, and is subjected to silica sol reaction in the silica sol reaction tank together with sulfuric acid from the second sulfuric acid storage tank and a catalyst from the catalyst storage tank to obtain a crude silica sol solution, a heat source in the silica sol reaction tank is from a coil in the silica sol reaction tank, and heat of the coil in the silica sol reaction tank is from the salt bath circulation heating equipment; wherein the catalyst in the catalyst storage tank is selected from FeO, mnO, cuO;
the crude silica sol solution enters the discharging tank, the crude silica sol solution in the discharging tank is filtered by a filter, filtered filter residues enter the residue filtering tank for additional treatment, and filtered filtrate enters the filtrate tank; the filtrate in the filtrate tank is sent into the evaporation concentration unit for evaporation concentration;
and cooling and recycling the evaporated and concentrated water by a cooler, and enabling the evaporated and concentrated silica sol product to enter the silica sol product storage tank through the metering filling machine for storage.
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| 纪萍.以天然硅灰石制备稳定硅溶胶.辽宁化工.2000,第29卷(第29期),141-142页，第145页. * |
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