CN213895215U - Device for synthesizing mesoporous silica by using silicon-containing waste - Google Patents

Device for synthesizing mesoporous silica by using silicon-containing waste Download PDF

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Publication number
CN213895215U
CN213895215U CN202022485949.9U CN202022485949U CN213895215U CN 213895215 U CN213895215 U CN 213895215U CN 202022485949 U CN202022485949 U CN 202022485949U CN 213895215 U CN213895215 U CN 213895215U
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mixing
box
reaction box
silicon
temperature control
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CN202022485949.9U
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章萍
蔡悦
彭港
张凌杰
相明雪
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Jiangxi Bluestar Xinghuo Silicone Co Ltd
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Jiangxi Bluestar Xinghuo Silicone Co Ltd
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Abstract

The utility model discloses a device for synthesizing mesoporous silica by using silicon-containing waste, which comprises a mixing reaction box, a mixing stirring box, a temperature control reaction box and a muffle furnace, wherein the mixing reaction box, the mixing stirring box and the temperature control reaction box are sequentially connected, and the connection part is provided with a control valve; the top of the mixing reaction box is provided with a NaOH feed port and a silicon-containing waste feed port, and an electric stirrer I is arranged in the mixing reaction box; the top of the mixing and stirring box is connected with the mixing and reacting box, the mixing and stirring box is provided with a template agent adding port, and an electric stirrer II and an HCl adding rod are arranged in the mixing and stirring box; the top of the temperature control reaction box is connected with the mixing and stirring box, an electric heating plate is arranged on the inner wall of the temperature control reaction box, and a water outlet and a discharge hole are formed in the bottom of the temperature control reaction box. The utility model discloses a set up mixed reaction box, mixed agitator tank, accuse temperature reaction box, muffle furnace equipment, integrated the step of former process flow, retrench the process design, reduce because the waste of the silicon source that reaction process leads to, improve the utilization ratio of silicon source.

Description

Device for synthesizing mesoporous silica by using silicon-containing waste
Technical Field
The utility model belongs to the technical field of the discarded object utilization, concretely relates to utilize device of siliceous discarded object synthesis mesoporous silica.
Background
In recent years, with the rapid development of industry and agriculture, a large amount of silicon-containing wastes are generated, the industrial wastes mainly comprise organic silicon factory waste residues, fly ash, power plant bottom ash, mine tailings, coal gasification fine residues, blast furnace slag, copper ore slag and the like, the agricultural wastes mainly comprise rice husk carbon, rice husk ash, sugarcane ash, grass ash and the like, the generated wastes need to be subjected to timely resource treatment, and random accumulation can cause environmental pollution. The existing treatment method comprises the treatment of burning or preparing cement to generate white carbon black and the like, but the problems of low treatment efficiency, low utilization degree of a silicon source, low industrial value of a generated product and the like exist, so that the resource utilization of the silicon source extraction from industrial and agricultural wastes is an urgent problem to be solved in the modern industrial and agricultural development.
At present, industrial and agricultural silicon-containing wastes are converted into mesoporous silica materials which can be applied to catalysis and petrochemical industry. Firstly, extracting a silicon source in waste by using an alkali liquor dissolving method, then generating a mesoporous silicon dioxide material through hydrothermal liquid crystal reaction with a template agent, and finally calcining to remove the template agent. The traditional reaction process is complicated in process, and the silicon source extraction efficiency is not high. Therefore, optimizing the reaction steps and equipment to improve the efficiency of extracting silicon source is a current concern.
SUMMERY OF THE UTILITY MODEL
To not enough and a difficult problem among the prior art, the utility model aims at providing an utilize device of silicon-containing discarded object synthesis mesoporous silica, the utility model discloses silicon in with the silicon-containing discarded object in mixing the reaction box is extracted, again in mixing agitator tank and accuse temperature reaction box with template agent hydrothermal reaction, through control solution pH, mesoporous silica appearance and specific surface area are controlled to reaction temperature and time, calcine in the muffle furnace at last and remove template agent, obtain the mesoporous silica material of ideal.
The utility model discloses a following technical scheme realizes:
a device for synthesizing mesoporous silica by using silicon-containing waste comprises a mixing reaction box, a mixing stirring box, a temperature control reaction box and a muffle furnace, wherein the mixing reaction box, the mixing stirring box and the temperature control reaction box are sequentially connected, and a control valve is arranged at the connection part;
the mixing reaction box is used for fully mixing the silicon-containing waste with NaOH alkali liquor to generate sodium silicate solution, the top of the mixing reaction box is provided with a NaOH feeding port and a silicon-containing waste feeding port, and an electric stirrer I is arranged in the mixing reaction box;
the mixing and stirring box is used for uniformly mixing the sodium silicate solution extracted by the mixing and reaction box with the template agent and the like, the top of the mixing and stirring box is connected with the mixing and reaction box, the mixing and stirring box is provided with a template agent adding port, and an electric stirrer II and an HCl adding rod are arranged in the mixing and stirring box;
the temperature control reaction box is used for reacting the uniformly mixed template agent with a sodium silicate solution to generate a mesoporous silica material, the top of the temperature control reaction box is connected with the mixing and stirring box, an electric heating plate is arranged on the inner wall of the temperature control reaction box, and the bottom of the temperature control reaction box is provided with a water outlet and a discharge hole;
and the muffle furnace is used for calcining the reaction product of the temperature control reaction box so as to remove the template agent in the reaction product.
Furthermore, the tail end of the mixing reaction box is provided with a waste residue outlet, and an automatic slag pusher is arranged in the mixing reaction box.
Further, a pH measuring device is arranged in the mixing and stirring box.
Furthermore, a thermometer is arranged in the temperature control reaction box.
Further, an HCl adding rate regulator is arranged on the HCl adding rod and is associated with the pH measuring device.
Compared with the prior art, the utility model discloses beneficial effect includes:
(1) the utility model discloses a set up equipment such as mixed reaction box, mixed agitator tank, accuse temperature reaction box, muffle furnace, integrated the step of former process flow, retrench process design, reduce because the waste of the silicon source that reaction process leads to, improve the utilization ratio of silicon source.
(2) The utility model discloses compare in the past be used for burning or making applications such as cement with the siliceous discarded object, higher to the utilization ratio of silicon source, gained result industrial value is higher, the resource utilization discarded object.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
Illustration of the drawings: 1-a mixing reaction box, 101-a NaOH feeding hole, 102-a silicon-containing waste feeding hole, 103-an electric stirrer I, 104-an automatic slag pusher, 105-a waste slag discharging hole, 2-a mixing stirring box, 201-a template agent feeding hole, 202-an electric stirrer II, 203-a pH measuring device, 204-an HCl feeding rod, 205-an HCl feeding rate regulator, a 3-temperature control reaction box, 301-a thermometer, 302-an electric heating plate, 303-a water outlet, 304-a discharging hole and a 4-muffle furnace.
In the description of the present invention, the terms "center", "upper", "lower", "inner", "outer", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplification of the description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "I", "II", "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted", "connected" and "connected" are to be interpreted broadly, and may be, for example, fixedly connected, detachably connected, integrally connected; can be mechanical connection and electrical connection; may be directly connected, indirectly connected through intervening agents, or may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood to be specific to those skilled in the art.
Detailed Description
The present invention will be further described with reference to the accompanying drawings.
As shown in fig. 1, an apparatus for synthesizing mesoporous silica by using silicon-containing waste comprises a mixing reaction tank 1, a mixing stirring tank 2, a temperature control reaction tank 3 and a muffle furnace 4, wherein the mixing reaction tank 1, the mixing stirring tank 2 and the temperature control reaction tank 3 are sequentially connected, and a control valve is arranged at the connection position.
The mixed reaction box 1 is used for fully mixing the silicon-containing waste with NaOH alkali liquor to generate sodium silicate solution;
the mixing and stirring box 2 is used for uniformly mixing the sodium silicate solution extracted by the mixing and reaction box 1 with the template agent and the like;
the temperature control reaction box 3 is used for reacting the uniformly mixed template agent with a sodium silicate solution to generate a mesoporous silica material;
and the muffle furnace 4 is used for calcining the reaction product of the temperature-controlled reaction box 3 to remove the template agent in the product.
The top of the mixing reaction box 1 is provided with a NaOH feeding port 101 and a silicon-containing waste feeding port 102, and an electric stirrer I103 is arranged in the mixing reaction box 1; the electric stirrer I103 is used for quickly mixing NaOH alkali liquor and silicon-containing waste to generate sodium silicate solution, and is also provided with a device capable of regulating the rotating speed, so that the extraction rate of the silicon-containing waste is effectively controlled by controlling the rotating speed of the electric stirrer I103; because the silicon-containing waste contains some components which can not react with NaOH alkali liquor, the silicon-containing waste can exist in the form of solid waste residues finally after the reaction of the mixed reaction box 1, in order to be convenient for cleaning, the tail end of the mixed reaction box 1 is provided with a waste residue discharge port 105, an automatic slag pusher 104 is arranged in the mixed reaction box 1, when the reaction in the mixed reaction box 1 is completed and sodium silicate solution is discharged into a subsequent mixing and stirring box 2, the automatic slag pusher 104 is started to push the solid waste residues to the waste residue discharge port 105 for discharging, and the discharged waste residues can be used as industrial raw materials such as cement. The automatic slag pusher 104 adopts an automatic slag removing device commonly used in the art, such as a combination of a swing type reciprocating motion and an automatic horizontal pushing technology, adopts a conventional structure, and is not described in detail herein.
The top of the mixing and stirring box 2 is connected with the mixing and reacting box 1, the mixing and stirring box 2 is provided with a template agent adding port 201, an electric stirrer II 202, a pH measurer 203 and an HCl adding rod 204 are arranged in the mixing and stirring box 2, the electric stirrer II 202 is used for uniformly mixing a sodium silicate solution generated by the reaction of the mixing and reacting box 1 with the template agent, HCl is added through the HCl adding rod 204 to regulate and control the pH value to be proper, meanwhile, the pH measurer 203 monitors the pH value in the mixing and stirring box 2 in real time, and the HCl adding rod 204 is provided with an HCl adding speed regulator 205 for regulating the HCl adding amount, the adding speed and the like; the addition amount and the addition rate of the HCl adding rod 204 are correlated with the values monitored by the pH measurer 203 so as to reduce the consumption of HCl.
The top of the temperature control reaction box 3 is connected with the mixing and stirring box 2, and the template agent and the extracted silicon source react in the temperature control reaction box 3 to generate a mesoporous silica material; an electric heating plate 302 is arranged on the inner wall of the temperature control reaction box 3 and used for ensuring normal hydrothermal reaction, the reaction temperature in the temperature control reaction box 3 is regulated, a thermometer 301 is arranged in the temperature control reaction box 3 and used for monitoring the reaction temperature in the temperature control reaction box 3, a water outlet 303 and a material outlet 304 are arranged at the bottom of the temperature control reaction box 3, waste liquid after the reaction is completed is discharged from the water outlet 303, reaction precipitates are collected by the material outlet 304, and finally the reaction precipitates are placed in a muffle furnace 4 to be heated and calcined to remove a template agent, so that mesoporous silica is finally obtained. The muffle 4 is a heating device commonly used in the market and is not described in detail.
The utility model discloses the working process of device is as follows:
the silicon-containing waste and NaOH alkali liquor are respectively fed into a mixing reaction box 1 through a silicon-containing waste feeding port 10 and a NaOH feeding port 101 according to the adding amount of 1:2, an electric stirrer I103 is stirred for 6 hours at the rotating speed of 1000rpm and then stands, and Na is added2SiO3The solution is extracted, and the residual silicon slag is pushed to a waste slag discharge port 105 by an automatic slag pusher 104 to be discharged;
opening the mixing reaction box 1 and mixing and stirringValves between the tanks 2, mixing reaction tank 1 for extracting Na2SiO3The method comprises the following steps that a solution enters a mixing and stirring box 2 through a valve, a CTAB template agent according to a certain proportion is put into the mixing and stirring box 2 through a template agent adding port 201, a HCl solution according to a certain proportion is put into the mixing and stirring box through a full-automatic HCl adding speed regulator 205 and an HCl adding rod 204 until the pH value is 7, a pH value of the mixing and stirring box 2 is monitored by a pH value tester 203, an electric stirrer II 202 is stirred for 2 hours at the rotating speed of 1000rpm, and the solution is uniformly stirred;
opening a valve between the temperature control reaction box 3 and the mixing and stirring box 2, enabling the uniformly stirred solution to enter the temperature control reaction box 3 through the valve, heating by an electric heating plate 302, monitoring the temperature in the temperature control reaction box 3 in real time by a thermometer 301, controlling the temperature to react at 120 ℃ for 12 hours, aging at normal temperature for 48 hours after reaction, discharging waste liquid by a water outlet 303, collecting precipitates by a discharge port 304, and heating and calcining in a muffle furnace 4 to remove a template agent.
In specific implementation, the utility model discloses still include the control system of each unit, like the drive control system of automatic slag pusher 104, the temperature regulating device of electric plate 302, the control system of HCl throwing rate regulator 205 and so on for the opening of each component of relevance stops, adjusts and so on, adopt conventional autonomous system can, the utility model discloses not described in detail.
The foregoing merely illustrates preferred embodiments of the present invention, which are described in considerable detail and detail, but are not to be construed as limiting the scope of the invention. It should be noted that, for those skilled in the art, without departing from the spirit of the present invention, several changes, modifications and substitutions can be made, which are all within the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the appended claims.

Claims (5)

1. A device for synthesizing mesoporous silica by using silicon-containing waste is characterized in that: the device comprises a mixing reaction box (1), a mixing stirring box (2), a temperature control reaction box (3) and a muffle furnace (4), wherein the mixing reaction box (1), the mixing stirring box (2) and the temperature control reaction box (3) are sequentially connected, and a control valve is arranged at the connection part;
the mixed reaction box (1) is used for fully mixing silicon-containing waste with NaOH alkali liquor to generate a sodium silicate solution, the top of the mixed reaction box (1) is provided with a NaOH feeding port (101) and a silicon-containing waste feeding port (102), and an electric stirrer I (103) is arranged in the mixed reaction box (1);
the mixing and stirring tank (2) is used for uniformly mixing the sodium silicate solution extracted from the mixing and reaction tank (1) with the template agent, the top of the mixing and stirring tank (2) is connected with the mixing and reaction tank (1), the mixing and stirring tank (2) is provided with a template agent feeding port (201), and an electric stirrer II (202) and an HCl feeding rod (204) are arranged in the mixing and stirring tank (2);
the temperature control reaction box (3) is used for reacting the uniformly mixed template agent with a sodium silicate solution to generate a mesoporous silica material, the top of the temperature control reaction box (3) is connected with the mixing and stirring box (2), an electric heating plate (302) is installed on the inner wall of the temperature control reaction box (3), and a water outlet (303) and a discharge hole (304) are formed in the bottom of the temperature control reaction box (3);
and the muffle furnace (4) is used for calcining the reaction product of the temperature-controlled reaction box (3) so as to remove the template agent in the product.
2. The apparatus for synthesizing mesoporous silica using silicon-containing waste according to claim 1, wherein: the tail end of the mixed reaction box (1) is provided with a waste residue outlet (105), and an automatic slag pusher (104) is arranged in the mixed reaction box (1).
3. The apparatus for synthesizing mesoporous silica using silicon-containing waste according to claim 1, wherein: a pH measuring device (203) is arranged in the mixing and stirring box (2).
4. The apparatus for synthesizing mesoporous silica using silicon-containing waste according to claim 1, wherein: a thermometer (301) is arranged in the temperature control reaction box (3).
5. The apparatus for synthesizing mesoporous silica using silicon-containing waste according to claim 3, wherein: an HCl adding rate regulator (205) is arranged on the HCl adding rod (204), and the HCl adding rate regulator (205) is associated with the pH measuring device (203).
CN202022485949.9U 2020-10-31 2020-10-31 Device for synthesizing mesoporous silica by using silicon-containing waste Active CN213895215U (en)

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Application Number Priority Date Filing Date Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113526511A (en) * 2021-08-17 2021-10-22 日月光半导体制造股份有限公司 Method for producing porous silica
CN113578255A (en) * 2021-08-17 2021-11-02 日月光半导体制造股份有限公司 Method for treating porous silica

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113526511A (en) * 2021-08-17 2021-10-22 日月光半导体制造股份有限公司 Method for producing porous silica
CN113578255A (en) * 2021-08-17 2021-11-02 日月光半导体制造股份有限公司 Method for treating porous silica

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