CN209974312U - System for utilize hydrogen chloride gas leaching silicate ore preparation superfine silicon dioxide - Google Patents
System for utilize hydrogen chloride gas leaching silicate ore preparation superfine silicon dioxide Download PDFInfo
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Abstract
The utility model discloses a system for utilize hydrogen chloride gas leaching silicate ore preparation superfine silicon dioxide. In the system, a circulating material outlet of the stirring kettle is communicated with a liquid inlet of the ejector through a circulating pipeline; the liquid outlet of the ejector is communicated with the circulating material inlet of the stirring kettle; a material outlet of the ore raw material feeding device is communicated with a circulating pipeline; a circulating pump is arranged on the circulating pipeline; and a circulating material outlet of the stirring kettle is communicated with the liquid-solid separation device. The utility model discloses utilize hydrogen chloride gas to leach system of silicate ore preparation superfine silicon dioxide, provide the industrialization feasible scheme that continuous leaching silicate ore prepared silica, through selecting for use the ejector moreover, adopt hydrogen chloride gas directly to dissolve the mode in silicate circulation thick liquids, owing to the high concentration of thick liquid in the ejector, high dispersibility and the high concentration hydrochloric acid solution initial contact have improved the dissolution efficiency of ore and the utilization ratio of hydrochloric acid greatly moreover.
Description
Technical Field
The utility model relates to a system for utilize hydrogen chloride gas leaching silicate ore preparation superfine silicon dioxide.
Background
Superfine SiO2The composite material has the characteristics of large specific surface area, porosity, high temperature resistance, strong electrical insulation, good reinforcing effect, no combustion and the like, and is widely applied to the fields of coatings, plastics, medicine, biology, papermaking, rubber, agriculture, chemical industry, national defense, machinery and the like. Superfine SiO2The production process is more, and only a gas phase method and a precipitation method are divided from a basic principle. The precipitation method is a method generally adopted in the current industrial production due to simple process, stable production condition, lower cost and high yield, and the current precipitation method is divided into a traditional precipitation method and a novel precipitation method, the novel precipitation method is also called as a dissociation method. Depending on the raw materials used, they can be classified into non-metal mineral methods, gramineous plant methods, byproduct recovery methods, and the like.
The separation method using non-metal ore as raw material is roughly divided into two methods, one is to use sodium hydroxide solution to leach raw material to obtain sodium silicate solution, then use hydrochloric acid to acidify the sodium silicate solution to obtain superfine SiO2One is to directly leach the raw material by hydrochloric acid solution or mixed acid solution to obtain superfine SiO2. However, most of the research currently stays in the experimental research stage, and the leaching reaction of silicate ore and acid is slow, high-temperature and strong acid environment is required, and high-concentration hydrochloric acid volatilizes at high temperature.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing an utilize hydrogen chloride gas leaching silicate ore deposit preparation superfine silicon dioxide's system, the utility model discloses a gaseous direct dissolved mode of HCl, acid concentration is high, active strong, and solution heat can be for leaching the process heat supply.
The utility model relates to an ultra-fine silica refers to the particle diameter and is 10 ~ 15 mu m's silica.
The utility model provides a system for preparing superfine silicon dioxide by leaching silicate ores with hydrogen chloride gas, which comprises an ore raw material feeding device, an ejector, a stirring kettle and a liquid-solid separation device;
the ejector is provided with a liquid inlet, a liquid outlet and a gas inlet;
a circulating material outlet of the stirring kettle is communicated with a liquid inlet of the ejector through a circulating pipeline;
the liquid outlet of the ejector is communicated with the circulating material inlet of the stirring kettle;
the material outlet of the ore raw material feeding device is communicated with the circulating pipeline;
a circulating pump is arranged on the circulating pipeline;
and a circulating material outlet of the stirring kettle is communicated with the liquid-solid separation device.
In the system, the joint of the material outlet of the ore raw material feeding device and the circulating pipeline is close to one end of the ejector.
In the system, the stirring kettle comprises at least one circulating material inlet, at least one circulating material outlet and at least one discharging opening.
In the system, the ore raw material feeding device comprises a powder quantitative conveying device;
the powder quantitative conveying device is communicated with the circulating pipeline through a feeding pipe;
the powder quantitative conveying device adds raw material powder of silicate ore into the circulating pipeline through the feeding pipe and mixes the raw material powder with materials in the circulating pipeline.
In the system, the ore raw material feeding device also comprises a premixing tank communicated with the powder quantitative conveying device;
the slurry outlet and the slurry inlet of the premixing tank are respectively communicated with the ejector and the circulating pipeline;
part of materials in the circulating pipeline are introduced into the premixing tank through the circulating pump to be premixed with the added silicate ore powder; and the premixed slurry is input into the ejector through the slurry outlet.
In the system, a steam outlet is arranged on the stirring kettle and is used for discharging vaporized water vapor and a small amount of unreacted hydrogen chloride gas;
preferably, the steam outlet is communicated with the circulating pipeline through a cooling water pipeline, and the cooling water pipeline is provided with a heat exchanger for condensing the steam and a small amount of unreacted hydrogen chloride gas and returning the condensed steam and a small amount of unreacted hydrogen chloride gas to the ejector, and meanwhile, part of reaction heat can be removed to keep the reaction temperature stable.
In the system, the liquid-solid separation device can be a settling separator, a hydrocyclone, a centrifuge or a filtering separator.
Utilize the system preparation when superfine silica, can include following step:
the silicate ore powder is mixed with the circulating liquid conveyed by the circulating pipeline through the ore raw material feeding device and then pumped into the ejector at a high speed; the hydrogen chloride gas is sucked into the ejector through the gas inlet on the ejector and dissolved in the circulating liquid, and the silicon dioxide is obtained through the reaction of hydrochloric acid and the silicate ore; the reaction is carried out in the ejector, the circulating pipeline and the stirring kettle in sequence (initial contact reaction is carried out in the ejector, and then reaction liquid enters the circulating pipeline and the stirring kettle for further reaction);
the circulating liquid is a slurry formed by the silicate ore and water (at the beginning of reaction) or a reaction liquid formed by the hydrochloric acid and the silicate ore after reaction.
The above method utilizes the following objects for part of the material circulation: firstly, part of circulating materials flow through the ejector, negative pressure is formed in the ejector, hydrogen chloride gas is sucked in, and therefore the hydrogen chloride gas can be pressurized without using a compressor; secondly, unreacted calcium silicate in the recycled materials is quickly reacted with hydrogen chloride in the ejector and a pipeline behind the ejector, the concentration of the hydrogen chloride is high, the mixing in the pipeline is quick, and the reaction rate is high.
The utility model discloses utilize the venturi effect form the negative pressure in the ejector to inhale hydrogen chloride gas extremely in the ejector and then react with the silicate ore, leach silica.
In the above preparation method, the silicate ore may be at least one of feldspar (orthoclase, plagioclase, paraphrate), mica, olivine, garnet, andalusite, agalmatolite, pyroxene, amphibole, wollastonite, talc, kaolinite, chlorite, and serpentine;
the particle size of the powder of the silicate ore is not less than 50 meshes and is screened based on Taylor standard;
SiO in the silicate ore2The mass content of (A) is not less than 40%;
the difference between the pressure of the hydrogen chloride gas at the gas inlet of the ejector and the pressure in the stirring kettle is not more than the maximum vacuum degree which can be reached by the ejector, such as 3.3 kPa;
the reaction temperature in the stirred tank can be 70-120 ℃;
the volume flow ratio of the circulating liquid to the hydrogen chloride gas in the ejector can be 2-3.5: 1.
In the preparation method, the continuous preparation of the superfine silicon dioxide can be realized by continuously adding the powder of the silicate ore into the ejector;
the specific operation is as follows: hydrogen chloride gas is sucked into the ejector through the gas inlet on the ejector and dissolved in the circulating liquid, and is subjected to primary reaction with silicate mineral powder in the circulating liquid, and then the reaction liquid enters the stirring kettle for further reaction; a part of the slurry in the stirring kettle is discharged into the liquid-solid separation device to be subjected to solid-liquid separation to obtain superfine silicon dioxide, and a part of the slurry enters the circulating pipeline through the circulating pump to be circulated;
the molar ratio of the hydrogen chloride gas to the silicate ore can be 2-3: 1, wherein the amount of the silicate ore is SiO2And (6) counting.
In the preparation method, the powder of the silicate ore is directly added into the stirring kettle to form slurry with water; the slurry is input into the ejector through the circulating pipeline; dissolving the hydrogen chloride gas sucked into the ejector into the slurry, and reacting hydrochloric acid with the silicate ore to obtain silicon dioxide, thereby realizing the batch preparation of the superfine silicon dioxide;
the molar ratio of the hydrogen chloride gas to the silicate ore is 2-2.5: 1, wherein the amount of the silicate ore is SiO2And (6) counting.
The principle of the utility model is that the silicate ore is leached under the existence of hydrochloric acid, so that soluble chloride salt is formed in leaching solution. The reaction mechanism of mineral leaching is a multiphase reaction that occurs at the interface of two phases, solid and liquid, the leaching process is divided into two stages: the first stage is leaching of the mineral surface; the second stage is capillary diffusion leaching. The leaching reaction speed of the former is high, and the time is short; the latter has slow reaction speed and long reaction time.
The utility model discloses utilize hydrogen chloride gas to leach system of silicate ore preparation superfine silicon dioxide, the industrialization feasible scheme of continuous leaching silicate ore preparation silica is provided, and through selecting for use the ejector, adopt the direct mode of dissolving in silicate circulation thick liquids of hydrogen chloride gas, hydrogen chloride gas and circulation thick liquids form in short time after contacting and are close saturated hydrochloric acid solution, it goes on more easily to make the leaching reaction, dissolve the advantage that heat can be for leaching the process heat supply simultaneously, and because the high concentration of thick liquids in the ejector, high dispersibility and high concentration hydrochloric acid solution initial contact, the dissolution efficiency of ore and the utilization ratio of hydrochloric acid have been improved greatly.
Drawings
FIG. 1 is a schematic diagram of a system for leaching silicate ore to prepare ultra-fine silica by using hydrogen chloride gas according to embodiment 1 of the present invention.
FIG. 2 is a second schematic diagram of the system for preparing ultra-fine silica by leaching silicate ore with hydrogen chloride gas according to the embodiment of the present invention.
The respective symbols in the figure are as follows:
the device comprises a dust remover 1, a storage tank 2, a powder quantitative conveying device 3, an ejector 4, a circulating pump 5, a slurry pump 5', a stirring kettle 6, a liquid-solid separation device 7, a circulating pipeline 8, a heat exchanger 9 and a cooling water pipeline 10.
Detailed Description
The present invention will be further described with reference to the accompanying drawings, but the present invention is not limited to the following embodiments.
Examples 1,
Fig. 1 is a schematic diagram of a preparation system according to a first embodiment of the present invention, which includes an ore raw material feeding device, an ejector 4, a stirring kettle 6 and a liquid-solid separation device 7. The ore raw material feeding device comprises a dust remover 1, a material storage tank 2 and a powder quantitative conveying device 3 which are connected in sequence; the ejector 4 is provided with a liquid inlet (not shown), a liquid outlet (not shown) and a gas inlet (not shown); a circulating pipeline 8 is communicated between the liquid inlet of the ejector 4 and the discharge port of the stirring kettle 6, and the liquid outlet of the ejector 4 is communicated with the circulating material inlet of the stirring kettle 6; the quantitative powder conveying device 3 feeds raw material powder of silicate ore into the circulating pipeline 8 through a feeding pipe and mixes the raw material powder with the material in the circulating pipeline 8. The discharge port of the stirring kettle 6 is communicated with the liquid-solid separation device 7; the circulating pipeline 8 is provided with a circulating pump 5 for pumping circulating liquid.
In the preparation system of the utility model, the stirring kettle 6 is provided with a steam outlet (not shown) for discharging vaporized steam and a small amount of unreacted hydrogen chloride gas. The steam outlet is communicated with a circulating pipeline 8 through a cooling water pipeline 10, a heat exchanger 9 is arranged on the cooling water pipeline 10 and used for condensing the steam and a small amount of unreacted hydrogen chloride gas and then returning the condensed steam and a small amount of unreacted hydrogen chloride gas to the ejector 4, meanwhile, partial reaction heat can be removed, and the reaction temperature is kept stable.
The utility model discloses in the preparation system, liquid-solid separator 7 can be sedimentation separator, hydrocyclone, centrifuge or filtering separator.
The utility model discloses the working process of preparation system of first embodiment does: by adopting continuous operation, the ore raw material powder conveyed to the material storage tank 2 is continuously added into a circulating pipeline 8 through a powder quantitative conveying device 3 and is mixed with circulating liquid to form slurry, the slurry is injected into an ejector 4 at a high speed, negative pressure is formed in the ejector by utilizing the Venturi effect, hydrogen chloride gas is sucked and subjected to primary contact reaction, then the reaction liquid enters a stirring kettle 6 for further reaction, one part of the slurry after the reaction of the stirring kettle is discharged into a solid-liquid separation device 7 for solid-liquid separation operation, and the other part of the slurry is pumped into the circulating pipeline 8 as circulating liquid through a circulating pump 5.
As a specific example, the effective ingredient of the ore raw material powder is selected to be CaSiO3The reaction temperature of the stirring kettle is 120 ℃, the temperature of hydrogen chloride gas is 250 ℃, the molar flow rate of the hydrogen chloride gas and CaSiO3The molar flow ratio of (1) is 2:1, and the material balance and heat balance data obtained by Aspen simulation are shown in Table 1.
TABLE 1 Material balance and Heat balance data
As a specific example, the silicate mineral of this example is wollastonite, which originates from Jiangxi and has a high height, a particle size of 200 mesh (based on Taylor standard screening), and an average mineral composition as shown in Table 2:
TABLE 2 mean mineral composition of wollastonite (%)
As a specific example, the storage tank has a volume of 4m3The powder quantitative conveying device selects a screw feeder, and the volume of the stirring kettle is 4m3The rotating speed is 30rpm, the adding amount of the wollastonite powder is 110kg/h, the adding amount of the water is 880kg/h, and the flow of the hydrogen chloride is controlled to be 45m3H (the molar ratio of hydrogen chloride gas to wollastonite powder is 2:1, wherein the amount of the wollastonite powder is SiO2Metering), setting the temperature of the stirring kettle at 80 ℃, the retention time at 2h, the circulation flow at 100kg/h, further washing, filtering and drying settled solid slag to obtain superfine SiO2The technical index is shown in Table 3.
TABLE 3 superfine SiO prepared from wollastonite ore powder2Technical index
| Silica% | 95 |
| Heating to reduce weight% | 5.8 |
| Reduction on ignition% | 5.1 |
| DBP absorption/ml/g | 2.98 |
| BET specific surface area/m2/g | 198 |
| pH | 6.4 |
| Average particle diameter/um | 10.5 |
| Iron/ppm | 180 |
As a specific example, the silicate ore of this example is serpentine, which is from hengyo, having a particle size of 200 mesh (based on taylor standard sieve), and an average mineral composition as shown in table 4:
TABLE 4 average mineral composition of serpentine (%)
As a specific example, the storage tank has a volume of 4m3The powder quantitative conveying device selects a screw feeder, and the volume of the stirring kettle is 4m3The rotating speed is 30rpm, the adding amount of the serpentine powder is 91kg/h, the adding amount of the water is 880kg/h, and the flow rate of the hydrogen chloride is controlled to be 45m3The mol ratio of hydrogen chloride gas to serpentine powder is 2:1, wherein the amount of serpentine powder is SiO2Metering), setting the temperature of the stirring kettle at 120 ℃, the retention time at 2h, the circulation flow at 100kg/h, further washing, filtering, drying and crushing the settled solid slag to obtain superfine SiO2The technical index is shown in Table 5.
TABLE 5 superfine SiO prepared from serpentine mineral powder2Technical index
Examples 2,
Fig. 2 is a schematic view of a preparation system according to a second embodiment of the present invention, which has a structure substantially the same as that of the system shown in fig. 1, except that: the ore raw material feeding device also comprises a premixing tank 11 communicated with the powder quantitative conveying device 3, a slurry outlet and a slurry inlet of the premixing tank 11 are respectively communicated with the ejector 4 and the circulating pipeline 8, and part of materials in the circulating pipeline 8 are introduced into the premixing tank 11 through the circulating pump 5 to be premixed with the added silicate ore powder; the premixed slurry is input into the ejector 4 through the slurry outlet. A slurry pump 5' is arranged on a pipeline of the premixing tank 11 communicated with the ejector 4.
The utility model discloses the working process of preparation system of second embodiment does: by adopting continuous operation, the ore raw material powder conveyed to the storage tank 2 is continuously added into a premixing tank 11 through a powder quantitative conveying device 3, the ore raw material powder is uniformly stirred and mixed with a certain amount of water in the premixing tank 11 to form slurry, the slurry is injected into an ejector 4 through a slurry pump 5' at a high speed, negative pressure is formed in the ejector by utilizing the Venturi effect, hydrogen chloride gas is sucked and subjected to preliminary contact reaction, then the reaction liquid enters a stirring kettle 6 for further reaction, one part of the slurry after the reaction of the stirring kettle is discharged into a liquid-solid separation device 7 for solid-liquid separation operation, and the other part of the slurry is taken as circulating liquid and is pumped into the premixing tank 11 through a circulating pipeline 8 by a circulating pump 5.
As a specific example, the silicate mineral of this example is wollastonite which originates from Jiangxi province and has a particle size of 200 meshes (based on Taylor standard sieve), and the average mineral composition is as shown in Table 2,
as a specific example, the storage tank has a volume of 4m3The powder quantitative conveying device selects a screw feeder, and the volume of the premixing tank is 3m3The volume of the stirring kettle is 4m3The rotating speed is 30rpm, the adding amount of the wollastonite powder is 110kg/h, the adding amount of the water is 880kg/h, and the flow of the hydrogen chloride is controlled to be 45m3H (the molar ratio of hydrogen chloride gas to wollastonite powder is 2:1, wherein the amount of the wollastonite powder is SiO2Metering), setting the temperature of the stirring kettle at 80 ℃, the retention time at 2h, the circulation flow at 100kg/h, further washing, filtering and drying settled solid slag to obtain superfine SiO2The technical index is shown in Table 6.
TABLE 6 superfine SiO prepared from wollastonite ore powder2Technical index
As a specific example, the silicate minerals of this example are also wollastonite from Jiangxi high, having a particle size of 200 mesh (based on Taylor standard sieve), and an average mineral composition as in Table 2,
as a specific example, 110kg of wollastonite powder was charged into a stirred tank, 880kg of water was added, and the flow rate of hydrogen chloride was controlled to 45m by a batch operation3H (molar ratio of hydrogen chloride gas to wollastonite powder is 2:1, wherein wollastoniteThe amount of the powder is SiO2Metering), setting the temperature of the stirring kettle at 80 ℃, the reaction time at 1h, the circulation flow at 100kg/h, further washing, filtering and drying settled solid slag to obtain superfine SiO2The technical index is shown in Table 7.
TABLE 7 ultrafine SiO prepared by batch operation2Technical index
| Silica% | 95.5 |
| Heating to reduce weight% | 5.72 |
| Reduction on ignition% | 5.19 |
| DBP absorption/ml/g | 2.95 |
| BET specific surface area/m2/g | 189 |
| pH | 6.4 |
| Average particle diameter/um | 14.1 |
| Iron/ppm | 180 |
It should be noted that, according to the general knowledge of those skilled in the art, the decomposition reactor and the regeneration reactor are also provided with corresponding temperature, liquid level, etc. measurement, control system and corresponding valves, which are not shown in the drawings, and this does not indicate that the process of the present invention does not include these conventional designs. The adjustment of the feed rate of the raw materials in the present invention based on the conversion and material balance is also a conventional design of the general knowledge of the skilled person in the art, and is not described one by one in the present invention, which does not mean that the process of the present invention does not include such a conventional design.
Claims (6)
1. A system for preparing superfine silicon dioxide by leaching silicate ores by using hydrogen chloride gas comprises an ore raw material feeding device, an ejector, a stirring kettle and a liquid-solid separation device;
the ejector is provided with a liquid inlet, a liquid outlet and a gas inlet;
a circulating material outlet of the stirring kettle is communicated with a liquid inlet of the ejector through a circulating pipeline;
the liquid outlet of the ejector is communicated with the circulating material inlet of the stirring kettle;
the material outlet of the ore raw material feeding device is communicated with the circulating pipeline;
a circulating pump is arranged on the circulating pipeline;
and a circulating material outlet of the stirring kettle is communicated with the liquid-solid separation device.
2. The system of claim 1, wherein: the ore raw material feeding device comprises a powder quantitative conveying device;
the powder quantitative conveying device is communicated with the circulating pipeline through a section of feeding pipe.
3. The system of claim 2, wherein: the ore raw material feeding device also comprises a premixing tank communicated with the powder quantitative conveying device;
and the slurry outlet and the slurry inlet of the premixing tank are respectively communicated with the ejector and the circulating pipeline.
4. The system according to any one of claims 1-3, wherein: and a steam outlet is arranged on the stirring kettle.
5. The system of claim 4, wherein: the steam outlet is communicated with the circulating pipeline through a cooling water pipeline, and a heat exchanger is arranged on the cooling water pipeline.
6. The system according to any one of claims 1-3, wherein: the liquid-solid separation device is a settling separator, a hydrocyclone, a centrifuge or a filtering separator.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109850911A (en) * | 2019-04-08 | 2019-06-07 | 原初科技（北京）有限公司 | A kind of system and method preparing superfine silicon dioxide using hydrogen chloride gas leaching silicate mine |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109850911A (en) * | 2019-04-08 | 2019-06-07 | 原初科技（北京）有限公司 | A kind of system and method preparing superfine silicon dioxide using hydrogen chloride gas leaching silicate mine |
| CN109850911B (en) * | 2019-04-08 | 2023-11-28 | 原初科技（北京）有限公司 | System and method for preparing ultrafine silicon dioxide by leaching silicate ore by using hydrogen chloride gas |
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