CN114790005A - Preparation method and production device of high-transparency silicon dioxide - Google Patents

Preparation method and production device of high-transparency silicon dioxide Download PDF

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Publication number
CN114790005A
CN114790005A CN202210158258.9A CN202210158258A CN114790005A CN 114790005 A CN114790005 A CN 114790005A CN 202210158258 A CN202210158258 A CN 202210158258A CN 114790005 A CN114790005 A CN 114790005A
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Prior art keywords
silicon dioxide
sodium silicate
reaction kettle
preparing
silicate solution
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张起森
游昌贵
叶志威
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FUJIAN SANMING JUFENG CHEMICAL CO LTD
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FUJIAN SANMING JUFENG CHEMICAL CO LTD
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Priority to CN202210158258.9A priority Critical patent/CN114790005A/en
Publication of CN114790005A publication Critical patent/CN114790005A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C01B33/187Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
    • C01B33/193Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D25/00Filters formed by clamping together several filtering elements or parts of such elements
    • B01D25/12Filter presses, i.e. of the plate or plate and frame type
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention relates to the technical field of silicon dioxide production, in particular to a preparation method and a production device of high-transparency silicon dioxide, which comprises the following steps of S1: preparing a sodium silicate solution; s2: preparing seed crystals; s3: preparing slurry; s4: obtaining silicon dioxide: the invention is characterized in that when the high-transparency silicon dioxide is prepared, a surfactant is added in the preparation process of the slurry, namely the surfactant is used as a modifier for modification, precipitated silicon dioxide is obtained by controlling the pH value and the reaction temperature in the reaction process, the transparency of the dried and screened silicon dioxide is obviously improved, meanwhile, warm water is added into a reaction kettle before the preparation is started, and crystal seeds and diluted sodium silicate are simultaneously dripped, so that the reaction speed between the crystal seeds, the diluted sodium silicate and other reaction liquids can be improved, the preparation efficiency of the whole preparation process is improved, and the production speed is improved.

Description

Preparation method and production device of high-transparency silicon dioxide
Technical Field
The invention relates to the technical field of silicon dioxide production, in particular to a preparation method and a production device of high-transparency silicon dioxide.
Background
Silica is a generic term for white powdery X-ray amorphous silicic acid and silicate products, mainly precipitated silica, fumed silica, ultrafine silica gel, and the like. Silica is a porous substance, the composition of which can be SiO 2 ·nH 2 O represents, wherein nH 2 O exists in the form of surface hydroxyl, can be dissolved in caustic alkali and hydrofluoric acid, but is not dissolved in water, solvent and acid (except hydrofluoric acid), and has the characteristics of high temperature resistance and good electrical insulation.
The transparency of the silicon dioxide prepared by the existing high-transparency silicon dioxide preparation process is not ideal enough, and the production efficiency is low. To this end, we provide a method for preparing silica having high transparency and an apparatus for producing the same to solve the above problems.
Disclosure of Invention
The present invention is directed to a method for preparing silica having high transparency and an apparatus for manufacturing the same to solve the above-mentioned problems.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of high-transparency silicon dioxide comprises the following steps:
s1: preparing a sodium silicate solution: adding solid sodium silicate and deionized water into a first reaction kettle, and stirring for 30-50 min at constant pressure and constant temperature to obtain a dilute sodium silicate solution;
s2: preparing seed crystal: adding a quantitative diluted sodium silicate solution into a second reaction kettle, dropwise adding a sulfuric acid solution into the second reaction kettle while stirring until the pH of the mixed solution reaches 7-8, and then sealing and preserving at constant temperature for 2 hours to obtain seed crystals;
s3: preparing slurry: adding warm water into a third reaction kettle, then dropwise adding a quantitative seed crystal and a dilute sodium silicate solution in a constant temperature environment, controlling the pH to be 8-10 in the process when the seed crystal is dropwise added, and stirring for 30-50 min to obtain a first solution; standing at constant temperature for 20min, adding surfactant into the first solution, stirring for 20min, wherein the volume ratio of the surfactant to the seed crystal is 0.01:1, adding sulfuric acid solution until the pH value is 5-6, and stirring for 30min to obtain slurry;
s4: obtaining silicon dioxide: and naturally cooling the slurry to room temperature, and carrying out spray drying after filter pressing, crushing and washing to obtain the high-transparency silicon dioxide.
Preferably, the surfactant is one or a mixture of fatty alcohol-polyoxyethylene ether, gamma-chloropropyltrimethoxysilane and polyoxyethylene sorbitan fatty acid ester.
Preferably, the constant pressure in step S1 is controlled to be 150-200cm Hg, and the constant temperature is 40-60 ℃.
Preferably, the temperature of the warm water in the step S3 is 60-70 ℃, and the constant temperature is controlled to be 60-70 ℃.
A production device of high-transparency silicon dioxide comprises a first reaction kettle, a second reaction kettle, a third reaction kettle, a filter press, a crusher, an ultrasonic cleaner and a spray dryer;
the first reaction kettle is used for preparing a dilute sodium silicate solution;
the second reaction kettle is used for preparing crystal seeds;
the third reaction kettle is used for preparing slurry and allowing the slurry to stand for precipitation;
the filter press is used for sequentially carrying out filter pressing on the slurry after standing and precipitating to obtain solid silicon dioxide;
the crusher is used for crushing solid silicon dioxide to obtain granular silicon dioxide
The ultrasonic cleaning machine is used for carrying out ultrasonic cleaning on the silicon dioxide particles;
the spray dryer is used for carrying out spray drying treatment on the granular silicon dioxide to obtain a dried finished product silicon dioxide.
Preferably, the device also comprises a dilute sodium silicate solution storage tank and a seed crystal storage tank, wherein the dilute sodium silicate solution storage tank and the seed crystal storage tank are constant-temperature and constant-pressure storage tanks;
the dilute sodium silicate solution storage tank is used for storing the prepared dilute sodium silicate solution;
the seed crystal storage tank is used for storing the prepared seed crystal.
Preferably, the filter press comprises a shell with an opening at the top, a conical funnel is installed between the side walls of the inner cavity of the shell, the opening at the bottom of the conical funnel is communicated with a square discharging pipe, the bottom of the square discharging pipe is provided with an openable material blocking mechanism, the position, close to the material blocking mechanism, of the side wall of the square discharging pipe is communicated with a water discharging pipe, one end of the water discharging pipe penetrates through the left side wall of the shell, a filter pressing mechanism is rotatably connected between the side walls of the inner cavity of the shell and is positioned above the conical funnel, the right side wall of the shell is fixedly connected with an electric cabinet, and a driving mechanism matched with the material blocking mechanism and the filter pressing mechanism is arranged in the electric cabinet;
the filter pressing mechanism comprises two hollow rotating shafts, the two rotating shafts symmetrically rotate on the left side wall and the right side wall of an inner cavity of the shell, two connecting rods are symmetrically and fixedly connected to the outer wall of each rotating shaft, a fixed shaft is connected between the two oppositely-arranged connecting rods, a plurality of groups of pressing plates are slidably connected between the two fixed shafts, the pressing plate on the leftmost side is fixedly connected with the rotating shaft on the left side, sliding blocks are symmetrically arranged on two opposite sides of the pressing plates, the sliding blocks are slidably connected with the fixed shafts, and filter screens are arranged on three side surfaces between the pressing plates in each group;
the driving mechanism comprises an electric cylinder, and the telescopic end of the electric cylinder penetrates through the right side wall of the shell and is rotationally connected with the middle part of the rightmost pressing plate.
Preferably, the stock stop includes the gate-shaped frame, the gate-shaped frame is installed in square row material bottom of the tube portion, the spout has all been seted up on three lateral walls of gate-shaped frame, relative two of setting sliding connection has the striker plate between the spout, striker plate inner chamber middle part threaded connection has the lead screw, lead screw one end runs through casing right side wall and is connected with actuating mechanism.
Preferably, actuating mechanism still includes driving motor, driving motor output outer wall rigid coupling has the double flute action wheel, is located the right side the right-hand member of axis of rotation run through the casing lateral wall and the rigid coupling has the first from the driving wheel, lead screw outer wall rigid coupling has the second from the driving wheel, the double flute action wheel is connected with the first transmission belt transmission from all between driving wheel and the second from the driving wheel.
Preferably, the inner cavity of the shell is provided with a conveyor belt feeding mechanism, the conveyor belt feeding mechanism is located below the material blocking mechanism, one end of the conveyor belt feeding mechanism penetrates through the left side wall of the shell, and the left side wall of the shell is provided with a discharge port matched with the conveyor belt feeding mechanism.
Compared with the prior art, the invention has the beneficial effects that:
when the high-transparency silicon dioxide is prepared, the surfactant is added in the preparation process of the slurry, namely the surfactant is used as the modifier for modification, the precipitated silicon dioxide is obtained by controlling the pH value and the reaction temperature in the reaction process, the transparency of the silicon dioxide obtained after drying and screening is obviously improved, meanwhile, warm water is added into a reaction kettle before the preparation is started, and the seed crystal and the dilute sodium silicate are simultaneously dripped, so that the reaction speed between the seed crystal, the dilute sodium silicate and other reaction liquids can be improved, the preparation efficiency of the whole preparation process is improved, and the production speed is improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the description below are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic process flow diagram of the present invention;
FIG. 2 is a schematic view of the flow line structure of the apparatus of the present invention;
FIG. 3 is a schematic view showing the structure of a filter press according to the present invention;
FIG. 4 is a schematic front cross-sectional view of FIG. 3;
FIG. 5 is a schematic top view of the structure of FIG. 3;
FIG. 6 is a schematic view of the filter press mechanism of the filter press according to the present invention;
FIG. 7 is a schematic top view of the structure of FIG. 6;
FIG. 8 is an enlarged view of the structure at A in FIG. 7;
FIG. 9 is a schematic structural view of a conical hopper and its connecting mechanism in the filter press according to the present invention;
fig. 10 is a sectional view of the structure of fig. 9.
In the drawings, the reference numbers indicate the following list of parts:
1. a first reaction kettle;
2. a second reaction kettle;
3. a third reaction kettle;
4. a filter press; 41. a housing; 42. a conical funnel; 43. a square discharge pipe; 44. a material stop mechanism; 441. a gate frame; 442. a chute; 443. a striker plate; 444. a screw rod; 45. a drain pipe; 451. a water pump; 46. a filter pressing mechanism; 461. a rotating shaft; 462. a connecting rod; 463. a fixed shaft; 464. pressing a plate; 4641. a connecting shaft; 465. a slider; 466. filtering with a screen; 467. connecting sleeves; 47. an electric cabinet; 48. a drive mechanism; 481. an electric cylinder; 4811. rotating the base; 482. a drive motor; 483. a double-groove driving wheel; 484. a first driven wheel; 485. a second driven wheel; 486. a drive belt; 49. a conveyor belt feeding mechanism;
5. a crusher;
6. an ultrasonic cleaning machine;
7. a spray dryer;
8. a dilute sodium silicate solution storage tank;
9. a seed crystal storage tank.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-10, the technical solution provided by the present invention is as follows:
referring to fig. 1:
a preparation method of high-transparency silicon dioxide comprises the following steps:
s1: preparing a sodium silicate solution: adding solid sodium silicate and deionized water into a first reaction kettle, and stirring for 30-50 min at constant pressure and constant temperature to obtain a dilute sodium silicate solution;
s2: preparing seed crystals: adding a certain amount of dilute sodium silicate solution into a second reaction kettle, dropwise adding a sulfuric acid solution into the second reaction kettle while stirring until the pH of the mixed solution reaches 7-8, and then sealing and preserving at constant temperature for 2 hours to obtain seed crystals;
s3: preparing slurry: adding warm water into a third reaction kettle, then dropwise adding a quantitative seed crystal and a dilute sodium silicate solution at the same time in a constant temperature environment until the seed crystal is completely dropwise added, controlling the pH to be 8-10 in the process, and simultaneously stirring for 30-50 min to obtain a first solution; standing at constant temperature for 20min, adding surfactant into the first solution, stirring for 20min, wherein the volume ratio of the surfactant to the seed crystal is 0.01:1, adding sulfuric acid solution until the pH is 5-6, and stirring for 30min to obtain slurry;
s4: obtaining silicon dioxide: and naturally cooling the slurry to room temperature, carrying out filter pressing, crushing, washing and spray drying to obtain the high-transparency silicon dioxide.
Specifically, the surfactant is one or a mixture of fatty alcohol-polyoxyethylene ether, gamma-chloropropyltrimethoxysilane and polyoxyethylene sorbitan fatty acid ester.
Specifically, in the step S1, the constant pressure is controlled to be 150-200cm Hg, and the constant temperature is controlled to be 40-60 ℃.
Specifically, the temperature of the warm water in the step S3 is 60-70 ℃, and the constant temperature is controlled to be 60-70 ℃.
Referring to FIGS. 2-10:
a production device of high-transparency silicon dioxide comprises a first reaction kettle 1, a second reaction kettle 2, a third reaction kettle 3, a filter press 4, a crusher 5, an ultrasonic cleaner 6 and a spray dryer 7;
the first reaction kettle 1 is used for preparing a dilute sodium silicate solution;
the second reaction kettle 2 is used for preparing seed crystals;
the third reaction kettle 3 is used for preparing slurry and standing the slurry for precipitation;
the filter press 4 is used for sequentially carrying out filter pressing on the slurry after standing and precipitating to obtain solid silicon dioxide;
the crusher 5 is used for crushing the solid silicon dioxide to obtain granular silicon dioxide
The ultrasonic cleaning machine 6 is used for carrying out ultrasonic cleaning on the silicon dioxide particles;
the spray dryer 7 is used for performing spray drying treatment on the granular silicon dioxide to obtain dried finished silicon dioxide.
Specifically, the device also comprises a dilute sodium silicate solution storage tank 8 and a seed crystal storage tank 9, wherein the dilute sodium silicate solution storage tank 8 and the seed crystal storage tank 9 are constant-temperature and constant-pressure storage tanks;
the dilute sodium silicate solution storage tank 8 is used for storing the prepared dilute sodium silicate solution;
the seed storage tank 9 is used for storing the prepared seed.
Specifically, the filter press 4 comprises a shell 41 with an opening at the top, a conical funnel 42 is installed between the side walls of the inner cavity of the shell 41, the opening at the bottom of the conical funnel 42 is communicated with a square discharging pipe 43, the bottom of the square discharging pipe 43 is provided with an openable stop mechanism 44, the side wall of the square discharging pipe 43 close to the stop mechanism 44 is communicated with a drain pipe 45, one end of the drain pipe 45 penetrates through the left side wall of the shell 41, a filter press mechanism 46 is rotatably connected between the side walls of the inner cavity of the shell 41, the filter press mechanism 46 is positioned above the conical funnel 42, the right side wall of the shell 41 is fixedly connected with an electric cabinet 47, a driving mechanism 48 which is mutually matched with the stop mechanism 44 and the filter press mechanism 46 is arranged in the electric cabinet 47, the stop mechanism can stop the bottom of the square discharging pipe in the filter press process, so that slurry obtained by filter press can be discharged along the drain pipe, after filter press is completed, the stop mechanism is opened, so that the silicon dioxide obtained by filter pressing can be discharged along the bottom of the square discharge pipe, thereby realizing solid-liquid separation;
the filter pressing mechanism 46 comprises two hollow rotating shafts 461, the two rotating shafts 461 symmetrically rotate on the left side wall and the right side wall of the inner cavity of the shell 41, two connecting rods 462 are symmetrically fixedly connected to the outer wall of the rotating shaft 461, a fixing shaft 463 is connected between the two oppositely arranged connecting rods 462, a plurality of groups of pressing plates 464 are slidably connected between the two fixing shafts 463, the pressing plate 464 on the leftmost side is fixedly connected with the rotating shaft 461 on the left side, sliding blocks 465 are symmetrically arranged on the opposite sides of the pressing plates 464, the sliding blocks 465 are slidably connected with the fixing shafts 463, and a filter screen 466 is arranged on three side surfaces between each group of pressing plates 464;
actuating mechanism 48 includes electric cylinder 481, and electric cylinder 481 stretches out and draws back the end and runs through casing 41 right side wall and rotate with the clamp plate 464 middle part on rightmost side and be connected, and electric cylinder can promote the multiunit clamp plate and slide, and then extrudees each other between the multiunit clamp plate for the thick liquid can be discharged along the filter screen fast, thereby the high-efficient solid-liquid separation who realizes the thick liquid.
Specifically, striker 44 includes door type frame 441, door type frame 441 is installed in square row material pipe 43 bottom, spout 442 has all been seted up on three side inner walls of door type frame 441, sliding connection has striker plate 443 between two relative spout 442 that set up, striker plate 443 inner chamber middle part threaded connection has lead screw 444, lead screw 444 one end runs through casing 41 right side wall and is connected with actuating mechanism 48, the lead screw rotates and can drives the striker plate and slide along the spout of door type frame, thereby realize that the automation of square row material pipe is opened, and then discharge silica.
Concretely, actuating mechanism 48 still includes driving motor 482, driving motor 482 output outer wall rigid coupling has double flute action wheel 483, the right-hand member that is located the axis of rotation 461 on right side runs through casing 41 lateral wall and rigid coupling has first from driving wheel 484, lead screw 444 outer wall rigid coupling has the second from driving wheel 485, double flute action wheel 483 and first from all being connected through the transmission of driving belt 486 between driving wheel 484 and the second from driving wheel 485, can drive the upset of filter-pressing mechanism and the stock stop simultaneously through setting up a set of driving motor and open, thereby can effectually avoid the silica material to pile up on the stock stop, also greatly reduced the cost of equipment.
Specifically, the inner cavity of the shell 41 is provided with the conveyor belt feeding mechanism 49, the conveyor belt feeding mechanism 49 is located below the material blocking mechanism 44, one end of the conveyor belt feeding mechanism 49 penetrates through the left side wall of the shell 41, the left side wall of the shell 41 is provided with a discharge hole matched with the conveyor belt feeding mechanism 49, and the conveyor belt feeding mechanism is arranged to enable silica subjected to filter pressing to be rapidly conveyed to the next procedure after the filter pressing is completed, so that the production efficiency is improved.
The first embodiment is as follows:
a preparation method of high-transparency silicon dioxide comprises the following steps:
s1: preparing a sodium silicate solution: adding solid sodium silicate and deionized water into a first reaction kettle, stirring at constant pressure and constant temperature for 30min to obtain a dilute sodium silicate solution, wherein the constant pressure is 150cm Hg, and the constant temperature is 40 ℃;
s2: preparing seed crystal: adding a certain amount of dilute sodium silicate solution into a second reaction kettle, dropwise adding a sulfuric acid solution into the second reaction kettle while stirring until the pH of the mixed solution reaches 7, and then sealing and preserving at constant temperature for 2 hours to obtain seed crystals;
s3: preparing slurry: adding warm water into a third reaction kettle, then dropwise adding a quantitative seed crystal and a dilute sodium silicate solution at the same time in a constant temperature environment until the seed crystal is completely dropwise added, controlling the pH to be 8 in the process, and stirring for 30min at the same time to obtain a first solution; keeping the temperature and standing for 20min, adding a surfactant into the first solution, stirring for 20min, wherein the surfactant is fatty alcohol-polyoxyethylene ether, the volume ratio of the surfactant to the seed crystal is 0.01:1, then adding a sulfuric acid solution until the pH is 5, and stirring for 30min to obtain a slurry, wherein the temperature of warm water is 60-70 ℃, and the constant temperature is controlled to be 60-70 ℃;
s4: obtaining silicon dioxide: and naturally cooling the slurry to room temperature, carrying out filter pressing, crushing, washing and spray drying to obtain the high-transparency silicon dioxide.
The second embodiment:
a preparation method of high-transparency silicon dioxide comprises the following steps:
s1: preparing a sodium silicate solution: adding solid sodium silicate and deionized water into a first reaction kettle, and stirring for 50min at constant pressure and constant temperature to obtain a dilute sodium silicate solution, wherein the constant pressure is 200cm Hg, and the constant temperature is 60 ℃;
s2: preparing seed crystal: adding a quantitative diluted sodium silicate solution into a second reaction kettle, dropwise adding a sulfuric acid solution into the second reaction kettle while stirring until the pH value of the mixed solution reaches 8, and then sealing and preserving at a constant temperature for 2 hours to obtain seed crystals;
s3: preparing slurry: adding warm water into a third reaction kettle, then dropwise adding a quantitative seed crystal and a dilute sodium silicate solution at the same time in a constant temperature environment until the seed crystal is completely dropwise added, controlling the pH to be 10 in the process, and stirring for 30min at the same time to obtain a first solution; keeping the constant temperature and standing for 20min, adding a surfactant into the first solution, stirring for 20min, wherein the surfactant is fatty alcohol-polyoxyethylene ether, the volume ratio of the surfactant to the seed crystal is 0.01:1, then adding a sulfuric acid solution until the pH value is 6, and stirring for 30min to obtain a slurry, wherein the temperature of warm water is 60-70 ℃, and the constant temperature is controlled to be 60-70 ℃;
s4: obtaining silicon dioxide: and naturally cooling the slurry to room temperature, carrying out filter pressing, crushing, washing and spray drying to obtain the high-transparency silicon dioxide.
Example three:
when the device is used for producing silicon dioxide, dilute sodium silicate solution, crystal seeds and slurry are prepared through a first reaction kettle 1, a second reaction kettle 2 and a third reaction kettle 3 respectively, and the prepared dilute sodium silicate solution and the prepared crystal seeds can be stored by a dilute sodium silicate solution storage tank 8 and a crystal seed storage tank 9 respectively;
after the slurry preparation is finished and the slurry is kept stand for a period of time, the slurry is poured between each group of pressing plates 464 of the filter pressing mechanism 46, then, the electric cylinder 481 is started, the electric cylinder 481 pushes the rightmost pressing plate 464 to slide along the fixed shaft 463, so that the pressing plates 464 are pressed against each other, and in order to improve the filter pressing effect of the pressing plates 464, the pressing block protrusions are respectively arranged on the side surfaces of the pressing plates 464, which are close to each other, in a staggered manner, so that the liquid in the slurry is discharged from the through holes of the filter screen 466, and is discharged into a square discharging pipe 43 through a conical funnel 42, and is blocked by a material blocking mechanism 44, so that the slurry can be discharged through the drain pipe 45, and the drain pipe 45 can be used by additionally installing a water pump 451 on the side wall of the square discharge pipe 43, the water inlet of the water pump 451 is connected with the water inlet pipe and extends into the square discharging pipe 43, and the water outlet pipe 45 is communicated with the water outlet of the water pump 451, so that the water discharging effect and efficiency in the square discharging pipe 43 can be improved;
after filter pressing is completed, the electric cylinder 481 is retracted to adjust the distance between the pressing plates 464, the driving motor 482 is started, the driving motor 482 rotates to drive the double-groove driving wheel 483 to rotate and respectively drive the rotating shaft 461 and the screw rod 444 to rotate through the transmission belt 486, the rotating shaft 461 rotates the whole filter pressing mechanism 46 to turn over, so that the opening of the filter pressing mechanism 46 faces downwards, silica in the filter pressing mechanism 46 is discharged and falls into the conical funnel 42, and in order to fully discharge the silica, the electric cylinder 481 can be started again in a reciprocating mode (the electric cylinder 481 is rotatably connected with the pressing plates 464 through the rotating seat 4811), so that the electric cylinder 481 can drive the pressing plates 464 to slide in a reciprocating mode, vibration force is generated, and the silica is discharged quickly; meanwhile, the screw rod 444 rotates to drive the material baffle 443 to slide along the sliding groove 442, so that the opening of the square discharging pipe 43 is opened, the silicon dioxide is rapidly discharged from the square discharging pipe 43 and falls onto the conveyor belt feeding mechanism 49 for rapid conveying, and the filter pressing operation of the silicon dioxide is realized;
the silicon dioxide after filter pressing separation sequentially enters a crusher 5, an ultrasonic cleaner 6 and a spray dryer 7 to be crushed, cleaned and dried sequentially, and finally finished silicon dioxide is obtained;
example four:
this example was used on the basis of example three:
the pressure plate 464 and the filter screen 466 can be detached for cleaning or replacement by the detachable connection between the leftmost pressure plate 464 and the left rotating shaft 461, between the fixed shaft 463 and the connecting rod 462, and between the electric cylinder 481 and the rightmost pressure plate 464 in the filter pressing mechanism 4;
wherein, the outer wall of the left rotating shaft 461 is connected with a connecting sleeve 467 through a screw thread, the side wall of the leftmost pressing plate 464 is fixedly connected with a connecting shaft 4641 which is matched with the connecting sleeve 467, and the outer wall of the connecting shaft 4641 is provided with an external thread (as shown in fig. 8); while the detachable structure between the fixed shaft 463 and the connecting rod 462 and between the electric cylinder 481 and the rightmost pressing plate 464 may refer to the structure between the leftmost pressing plate 464 and the left rotating shaft 461, which will not be described in detail.
In the description of the present invention, it is to be understood that the terms "coaxial", "bottom", "one end", "top", "middle", "other end", "upper", "one side", "top", "inner", "front", "center", "both ends", and the like, indicate orientations or positional relationships based on the drawings, and are only for convenience of description and simplicity of description, and do not indicate or imply that the referred device or element must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
In the present invention, unless otherwise explicitly stated or limited, the terms "mounted," "disposed," "connected," "fixed," "screwed" and the like are to be understood broadly, for example, as being fixedly connected, detachably connected, or integrated; can be mechanically or electrically connected; the terms may be directly connected or indirectly connected through an intermediate, and may be communication between two elements or interaction relationship between two elements, unless otherwise specifically limited, and the specific meaning of the terms in the present invention will be understood by those skilled in the art according to specific situations.
Although embodiments of the present invention have been shown and described, it would be appreciated by those skilled in the art that changes may be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the claims and their equivalents.

Claims (10)

1. A method for preparing high-transparency silicon dioxide is characterized by comprising the following steps: the method comprises the following steps:
s1: preparing a sodium silicate solution: adding solid sodium silicate and deionized water into a first reaction kettle, and stirring at constant pressure and constant temperature for 30-50 min to obtain a dilute sodium silicate solution;
s2: preparing seed crystals: adding a quantitative diluted sodium silicate solution into a second reaction kettle, dropwise adding a sulfuric acid solution into the second reaction kettle while stirring until the pH of the mixed solution reaches 7-8, and then sealing and preserving at constant temperature for 2 hours to obtain seed crystals;
s3: preparing slurry: adding warm water into a third reaction kettle, then dropwise adding a quantitative seed crystal and a dilute sodium silicate solution in a constant temperature environment, controlling the pH to be 8-10 in the process when the seed crystal is dropwise added, and stirring for 30-50 min to obtain a first solution; standing at constant temperature for 20min, adding surfactant into the first solution, stirring for 20min, wherein the volume ratio of the surfactant to the seed crystal is 0.01:1, adding sulfuric acid solution until the pH value is 5-6, and stirring for 30min to obtain slurry;
s4: obtaining silicon dioxide: and naturally cooling the slurry to room temperature, and carrying out spray drying after filter pressing, crushing and washing to obtain the high-transparency silicon dioxide.
2. A method for preparing silica having high transparency and an apparatus for manufacturing the same according to claim 1, wherein: the surfactant is one or a mixture of fatty alcohol-polyoxyethylene ether, gamma-chloropropyltrimethoxysilane and polyoxyethylene sorbitan fatty acid ester.
3. The method for preparing silica having high transparency and the apparatus for manufacturing the same according to claim 1, wherein: in the step S1, the constant pressure is controlled to be 150-200cm Hg, and the constant temperature is controlled to be 40-60 ℃.
4. The method for preparing silica having high transparency and the apparatus for manufacturing the same according to claim 1, wherein: the temperature of the warm water in the step S3 is 60-70 ℃, and the constant temperature is controlled to be 60-70 ℃.
5. A production apparatus for the high-transparency silica according to any one of claims 1 to 4, characterized in that: the production device comprises a first reaction kettle (1), a second reaction kettle (2), a third reaction kettle (3), a filter press (4), a crusher (5), an ultrasonic cleaning machine (6) and a spray dryer (7);
the first reaction kettle (1) is used for preparing a dilute sodium silicate solution;
the second reaction kettle (2) is used for preparing seed crystals;
the third reaction kettle (3) is used for preparing slurry and allowing the slurry to stand for precipitation;
the filter press (4) is used for sequentially carrying out filter pressing on the slurry after standing and precipitating to obtain solid silicon dioxide;
the crusher (5) is used for crushing solid silicon dioxide to obtain granular silicon dioxide, and the ultrasonic cleaning machine (6) is used for carrying out ultrasonic cleaning on silicon dioxide granules;
and the spray dryer (7) is used for carrying out spray drying treatment on the granular silicon dioxide to obtain dried finished silicon dioxide.
6. The apparatus for manufacturing silica having high transparency according to claim 5, wherein: the device also comprises a dilute sodium silicate solution storage tank (8) and a seed crystal storage tank (9), wherein the dilute sodium silicate solution storage tank (8) and the seed crystal storage tank (9) are constant-temperature and constant-pressure storage tanks;
the dilute sodium silicate solution storage tank (8) is used for storing the prepared dilute sodium silicate solution;
the seed crystal storage tank (9) is used for storing the prepared seed crystal.
7. The apparatus for manufacturing silica having high transparency according to claim 5, wherein: the filter press (4) comprises a shell (41) with an opening at the top, a conical funnel (42) is arranged between the side walls of the inner cavity of the shell (41), the bottom opening of the conical funnel (42) is communicated with a square discharge pipe (43), the bottom of the square discharge pipe (43) is provided with an openable material blocking mechanism (44), a drain pipe (45) is communicated with the side wall of the square discharging pipe (43) close to the stock stop (44), one end of the drain pipe (45) penetrates through the left side wall of the shell (41), a filter pressing mechanism (46) is rotatably connected between the side walls of the inner cavity of the shell (41), and the filter pressing mechanism (46) is positioned above the conical funnel (42), the right side wall of the shell (41) is fixedly connected with an electric cabinet (47), a driving mechanism (48) which is mutually matched with the material blocking mechanism (44) and the filter pressing mechanism (46) is arranged in the electric cabinet (47);
the filter pressing mechanism (46) comprises two hollow rotating shafts (461), the two rotating shafts (461) symmetrically rotate on the left side wall and the right side wall of an inner cavity of the shell (41), two connecting rods (462) are symmetrically and fixedly connected to the outer wall of each rotating shaft (461), a fixing shaft (463) is connected between the two oppositely-arranged connecting rods (462), a plurality of groups of pressing plates (464) are slidably connected between the two fixing shafts (463), the pressing plate (464) on the leftmost side is fixedly connected with the rotating shaft (461) on the left side, sliding blocks (465) are symmetrically arranged on the two opposite sides of each pressing plate (464), the sliding blocks (465) are slidably connected with the fixing shafts (463), and filter screens (466) are arranged on three side surfaces between each group of the pressing plates (464);
the driving mechanism (48) comprises an electric cylinder (481), and the telescopic end of the electric cylinder (481) penetrates through the right side wall of the shell (41) and is rotatably connected with the middle part of the rightmost pressing plate (464).
8. The apparatus for manufacturing silica having high transparency according to claim 7, wherein: stop member (44) are including door type frame (441), install in square row material pipe (43) bottom door type frame (441), spout (442) have all been seted up on three side inner walls of door type frame (441), two of relative setting sliding connection has striker plate (443) between spout (442), striker plate (443) inner chamber middle part threaded connection has lead screw (444), lead screw (444) one end is run through casing (41) right side wall and is connected with actuating mechanism (48).
9. The apparatus for manufacturing silica having high transparency according to claim 8, wherein: actuating mechanism (48) still include driving motor (482), driving motor (482) output end outer wall rigid coupling has double flute action wheel (483), is located the right side the right-hand member of axis of rotation (461) run through casing (41) lateral wall and rigid coupling have first follow driving wheel (484), lead screw (444) outer wall rigid coupling has the second to follow driving wheel (485), double flute action wheel (483) and first follow driving wheel (484) and second are all connected through driving belt (486) transmission between driving wheel (485).
10. The apparatus for producing silica having high transparency according to claim 7 or 9, wherein: casing (41) inner chamber is provided with conveyer belt feeding mechanism (49), and conveyer belt feeding mechanism (49) are located stock stop (44) below, the one end of conveyer belt feeding mechanism (49) runs through casing (41) left side wall, casing (41) left side wall is provided with the discharge gate of mutually supporting with conveyer belt feeding mechanism (49).
CN202210158258.9A 2022-02-21 2022-02-21 Preparation method and production device of high-transparency silicon dioxide Pending CN114790005A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115417415A (en) * 2022-10-14 2022-12-02 金三江(肇庆)硅材料股份有限公司 Silicon dioxide for high-transparency silicone rubber and preparation method and application thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115417415A (en) * 2022-10-14 2022-12-02 金三江(肇庆)硅材料股份有限公司 Silicon dioxide for high-transparency silicone rubber and preparation method and application thereof

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