CN112316873A - Double-layer glass reaction kettle for preparing aerogel sol - Google Patents

Double-layer glass reaction kettle for preparing aerogel sol Download PDF

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Publication number
CN112316873A
CN112316873A CN202011231931.4A CN202011231931A CN112316873A CN 112316873 A CN112316873 A CN 112316873A CN 202011231931 A CN202011231931 A CN 202011231931A CN 112316873 A CN112316873 A CN 112316873A
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China
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kettle
double
kettle body
interface
reaction kettle
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CN202011231931.4A
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Chinese (zh)
Inventor
张忠伦
王明铭
时红霞
刘振森
辛志军
相博文
侯建业
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China Building Materials Science Innovation Technology Research Institute Shandong Co ltd
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China Building Materials Science Innovation Technology Research Institute Shandong Co ltd
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Priority to CN202011231931.4A priority Critical patent/CN112316873A/en
Publication of CN112316873A publication Critical patent/CN112316873A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/02—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in boilers or stills
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/42—Regulation; Control
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/0091—Preparation of aerogels, e.g. xerogels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B01J19/0013—Controlling the temperature of the process
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/02—Apparatus characterised by being constructed of material selected for its chemically-resistant properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/008—Feed or outlet control devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/005—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the outlet side being of particular interest
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/007—Aspects relating to the heat-exchange of the feed or outlet devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00054—Controlling or regulating the heat exchange system
    • B01J2219/00056—Controlling or regulating the heat exchange system involving measured parameters
    • B01J2219/00058—Temperature measurement
    • B01J2219/0006—Temperature measurement of the heat exchange medium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00094—Jackets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/02—Apparatus characterised by their chemically-resistant properties
    • B01J2219/025—Apparatus characterised by their chemically-resistant properties characterised by the construction materials of the reactor vessel proper
    • B01J2219/0254—Glass

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The invention relates to a double-layer glass reaction kettle for preparing aerogel sol. The double-layer glass reaction kettle comprises: the kettle body is of a jacket structure; the kettle body comprises a circulating medium inlet and a circulating medium outlet; a through insertion pipe is arranged at the upper part of the middle part of the kettle body; a sol discharge port is formed at the bottom of the kettle body; the kettle cover is arranged above the kettle body and is connected with the kettle body through a flange; the kettle cover is provided with a feeding hole, a titration flask interface, a distillation condenser interface, a thermocouple interface, a pressure gauge interface and a stirrer interface; the kettle body is fixedly arranged on the fixed frame; the stirrer comprises a stirring shaft and a stirring paddle; the stirring shaft passes through the stirrer connector from the outside of the kettle cover and extends into the kettle body; a stirring paddle is arranged on the stirring shaft extending into the kettle body. The technical problem to be solved is to enable the aerogel sol preparation device to be used in the preparation of aerogel sol so as to realize the accurate control of sol reaction conditions and ensure the quality of aerogel products, thereby being more practical.

Description

Double-layer glass reaction kettle for preparing aerogel sol
Technical Field
The invention belongs to the technical field of aerogel material manufacturing equipment, and particularly relates to a double-layer glass reaction kettle for preparing aerogel sol.
Background
The preparation process of the aerogel comprises the preparation of sol, the reaction medium of the aerogel is an acidic solution, the aerogel has strong corrosivity, and the aerogel is suitable for a double-layer glass reaction kettle with good corrosion resistance.
In the double-layer glass reaction kettle in the prior art, reaction conditions such as stirring, feeding, condensation and the like are mostly set on a kettle cover, the technological requirements of the reaction process of aerogel sol are complex, and on one hand, the reaction kettle body is required to be provided with a jacket layer so as to flexibly control the temperature of a reaction medium; on the other hand, in the aerogel sol preparation process, besides the conditions of the reaction kettle, such as pressure, stirring speed, temperature and pH value of the reaction medium, and the like, need to be adjusted at any time, particularly, the pH value of the reaction medium needs to be monitored in real time in the reaction process, and the pH value is adjusted at a proper time.
The traditional glass reaction kettle for preparing the sol is difficult to meet the control requirements of sol preparation process on various process conditions, cannot accurately realize the control of the reaction conditions in the glass reaction kettle so as to achieve accurate reaction, and is difficult to control the quality of products, so that the double-layer glass reaction kettle cannot be popularized and applied to the preparation of aerogel sol all the time.
Disclosure of Invention
The invention mainly aims to provide a double-layer glass reaction kettle for preparing aerogel sol, which aims to solve the technical problem that the double-layer glass reaction kettle can be used for preparing aerogel sol so as to realize the accurate control of sol reaction conditions and ensure the quality of aerogel products, thereby being more suitable for practical use.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme. The invention provides a double-layer glass reaction kettle for preparing aerogel sol, which comprises:
the kettle body is of a jacket structure; the kettle body comprises a circulating medium inlet and a circulating medium outlet; an insert pipe penetrating through the side wall of the kettle body is arranged at the upper part of the middle part of the kettle body; a sol discharge hole is formed in the bottom of the kettle body;
the kettle cover is arranged above the kettle body and is connected with the kettle body through a flange; the kettle cover is provided with a feeding hole, a titration flask interface, a distillation condenser interface, a thermocouple interface, a pressure gauge interface and a stirrer interface;
the kettle body is fixedly arranged on the fixed frame;
the stirrer comprises a stirring shaft and a stirring paddle; the stirring shaft passes through the stirrer connector from the outside of the kettle cover and extends into the kettle body; and a stirring paddle is arranged on the stirring shaft extending into the kettle body.
The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures.
Preferably, in the double-layer glass reaction kettle, the insertion pipe is arranged obliquely upwards, and the included angle between the insertion pipe and the vertical direction is 50 +/-10 degrees.
Preferably, the double-layer glass reaction kettle further comprises a PH probe; the PH probe can be inserted into the insertion tube; the inner surface of the insertion tube and the surface of the PH probe contacted with the insertion tube are both made of ground glass.
Preferably, in the double-layer glass reaction kettle, the insert pipe and the kettle body are integrally molded.
Preferably, in the double-layer glass reaction kettle, the kettle cover and the kettle body are detachably connected.
Preferably, in the double-layer glass reaction kettle, a polytetrafluoroethylene sealing gasket is arranged between the kettle body and the kettle cover.
Preferably, the double-layer glass reaction kettle further comprises a titration flask, a distillation condenser, a thermocouple, a pressure gauge and a PH probe; the titration flask, the distillation condenser, the thermocouple and the pressure gauge are respectively arranged on the kettle cover through a titration flask interface, a distillation condenser interface, a thermocouple interface and a pressure gauge interface; the PH probe is arranged on the kettle body through the insertion pipe; the titration flask, the distillation condenser, the thermocouple, the pressure gauge and the PH probe are all fixed on the fixing frame.
Preferably, in the double-layer glass reaction kettle, a fixed sealing element is arranged at the interface of the titration flask, the interface of the distillation condenser, the interface of the thermocouple and the interface of the pressure gauge; and a rotary sealing element is arranged at the contact position of the kettle cover and the stirring shaft.
Preferably, the double-layer glass reaction kettle is provided, wherein the titration bottles comprise an acid titration bottle and an alkali titration bottle.
Preferably, in the double-layer glass reaction kettle, the distillation condenser comprises a distillation flask, a distillation liquid receiving bottle and a cooling pipe; the cooling pipe is coiled in the distillation flask; the distillation liquid receiving bottle is arranged below the distillation bottle.
Preferably, the double-layer glass reaction kettle further comprises a water tank and a water pump; the condensation pipe comprises an upper end water outlet and a lower end water inlet; the water tank is connected with a water outlet at the upper end of the cooling pipe; the water pump is connected with a water inlet at the lower end of the cooling pipe; the water tank, the water pump and the condenser pipe are sequentially connected through a pipeline to form a cooling water circulation system.
Preferably, the double-layer glass reaction kettle further comprises a vacuum pump; the vacuum pump is communicated with the double-layer glass reaction kettle through the distillation flask.
Preferably, the double-layer glass reaction kettle further comprises a circulating medium temperature controller, one end of the circulating medium temperature controller is connected with the circulating medium inlet, and the other end of the circulating medium temperature controller is connected with the circulating medium outlet; the temperature range of the circulating medium is-80 ℃ to 300 ℃.
Preferably, the double-layer glass reaction kettle further comprises a motor and a speed regulator; the motor and the speed regulator are both fixed on the fixed frame; one end of the motor is connected with the speed regulator, the other end of the motor is connected with the stirring shaft, and the rotating speed of the stirrer is regulated through the regulator.
Preferably, in the double-layer glass reaction kettle, the bottom of the fixing frame is provided with universal wheels and brake pads; the universal wheel is used for moving the fixing frame; the brake pad is used for braking the universal wheel.
By means of the technical scheme, the double-layer glass reaction kettle for preparing the aerogel sol at least has the following advantages:
1. the double-layer glass reaction kettle for preparing aerogel sol is characterized in that a feed inlet, a titration flask interface, a distillation condenser interface, a thermocouple interface, a pressure gauge interface and a stirrer interface are arranged on a kettle cover, a kettle body is of a jacket structure, the kettle body is provided with the inserting pipe, the inserting pipe and the kettle body are integrally formed, the effects of uniform thickness and small stress of the inserting pipe are realized by controlling the integrally forming process and the angle of the inserting pipe, the double-layer glass reaction kettle provided by the technical scheme of the invention can realize the preparation process of the aerogel sol, can accurately control the reaction conditions according to the process of the aerogel sol, thereby preparing the aerogel sol with controlled performance, ensuring the quality of the aerogel sol product and realizing the popularization and the application of the double-layer glass reaction kettle in the field of aerogel sol manufacture;
2. according to the double-layer glass reaction kettle for preparing aerogel sol, the fixed sealing piece and the rotary sealing piece are arranged at each interface, so that the sealing between each part which is arranged on the kettle cover in a matched mode is good, the contact surfaces of the inner surface of the insertion pipe and the probe are both provided with the frosted glass surfaces, and the polytetrafluoroethylene sealing washer is arranged between the kettle body and the kettle cover, so that the whole double-layer glass reaction kettle can form a closed space, when the double-layer glass reaction kettle is communicated with the distillation flask through the vacuum pump, the vacuum condition can be realized in the kettle, the sol reaction can be carried out under the vacuum condition, and the application range of a sol preparation process is widened;
3. according to the double-layer glass reaction kettle for preparing the aerogel sol, the temperature of cooling water is accurately controlled through the cooling water circulation system, and the distillation bottle, the distillation liquid receiving bottle and the cooling water circulation system are arranged to be matched, so that the distillation function of the double-layer glass reaction kettle is realized, the sol reaction can be carried out under the distillation condition, and the application range of a sol preparation process is widened;
4. according to the double-layer glass reaction kettle for preparing the aerogel sol, the temperature of the circulating medium can be accurately controlled through the circulating medium temperature controller, and the temperature of the circulating medium can be controlled within a wide range of-80-300 ℃, so that the double-layer glass reaction kettle can realize accurate temperature control within a wide range, and the application range of a sol preparation process is widened;
5. according to the double-layer glass reaction kettle for preparing aerogel sol, the kettle body is detachably connected with the kettle cover, and one kettle body can be provided with different kettle covers with different functions, so that the switching among different sol processes is realized, and the application range of the sol preparation process is widened;
6. according to the double-layer glass reaction kettle for preparing aerogel sol, the kettle body and all components are fixedly arranged on the fixing frame, and the universal wheels and the brake pads are arranged at the bottom of the fixing frame, so that the double-layer glass reaction kettle can flexibly move within a certain range, and the production arrangement is convenient.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 is a schematic structural view of a double-glass reaction vessel according to the present invention.
Detailed Description
To further illustrate the technical means and effects of the present invention for achieving the predetermined objects, the following detailed description of the embodiments, structures, characteristics and effects of the double-layer glass reaction vessel for preparing aerogel sol according to the present invention will be made with reference to the accompanying drawings and preferred embodiments.
The invention provides a double-layer glass reaction kettle for preparing aerogel sol, which is shown as the attached figure 1 and comprises the following components:
the kettle body 1 is of a jacket structure; the kettle body comprises a circulating medium inlet 12 and a circulating medium outlet 13; an insert pipe 14 penetrating through the side wall of the kettle body is arranged at the upper part of the middle part of the kettle body 1; a sol discharge port 8 is formed at the bottom of the kettle body;
the kettle cover 11 is arranged above the kettle body 1 and is connected with the kettle body 1 through a flange; the kettle cover 11 is provided with a feeding hole 111, a titration flask interface, a distillation condenser interface, a thermocouple interface, a pressure gauge interface and a stirrer interface;
the fixing frame 2 is used for fixedly mounting the kettle body 1 on the fixing frame 2;
a stirrer 3 including a stirring shaft 33 and a stirring paddle 34; the stirring shaft 33 passes through the stirrer connector from the outside of the kettle cover 11 and extends into the kettle body 1; a stirring paddle 34 is arranged on the stirring shaft 33 extending into the kettle body 1.
On one hand, the height of the double-layer glass reaction kettle related to the position of the insert pipe cannot be too low, so that the phenomenon that the kettle body leaks liquid accidentally and safety accidents happen when a PH probe is inserted into the insert pipe is avoided; on the other hand, the height should not be too high to prevent the pH probe from reaching the surface of the reaction medium and thus failing to monitor the pH of the reaction medium in real time. Based on the above two factors, the height of the insertion tube is set at a lower position on the basis of reserving a reaction space. Preferably, the insertion pipe is arranged at a position above the middle part of the kettle body.
The discharge port 8 is further provided with a discharge valve 81 for discharging the prepared sol.
Preferably, the insertion tube 14 is disposed obliquely upward, and the included angle between the insertion tube and the vertical direction is 50 +/-10 degrees.
The angle design of the insertion tube is convenient to operate when considering measuring the PH value on one hand, and on the other hand, the PH probe is also considered to be inserted into the insertion tube, the stress between the insertion tube and the kettle body is small, the safety risk of the reaction kettle can be reduced, and the service life of the reaction kettle is prolonged.
Preferably, it further comprises a PH probe; the PH probe can be inserted into the insertion tube; the inner surface of the insertion tube 14 and the surface of the PH probe in contact with the insertion tube are both made of ground glass.
On one hand, because a fine gap is formed between the ground glass, steam in the reaction kettle is condensed between the two layers of ground glass, and a watertight structure of ground glass-liquid-ground glass is formed; on the other hand, the contact area of the ground glass is increased, and the sealing effect between the two layers of ground glass is good due to the acting force between molecules. Therefore, when the PH probe is inserted into the insertion tube, the whole glass reaction kettle still has better sealing performance, so that the double-layer glass reaction kettle can not leak liquid and can react under the vacuum condition.
Preferably, the insertion tube 14 is integrally formed with the kettle body 1.
Making holes in double glazing has been difficult. In order to solve the technical problem, the technical scheme of the invention uses borosilicate glass as a raw material, and the borosilicate glass is integrally formed according to the following process to obtain a double-layer glass reaction kettle body with holes on the side wall. The glass comprises the following ingredients: crushing the raw materials of silica sand (sandstone), soda ash, feldspar and boric acid into powder; weighing various powder materials according to the following mass percentage, namely 50-60% of silica sand (sandstone), 10-15% of soda ash, 10-15% of feldspar and 8-17% of boric acid; mixing the above powders, and stirring to obtain batch. And feeding the batch into a glass melting furnace, and melting the batch into molten glass at 1700 ℃. Blowing the glass liquid at 1500 ℃ into a special mold. And (4) conveying the formed kettle body into an annealing kiln for annealing so as to balance stress and prevent the kettle body from self-explosion and self-cracking.
In the above-mentioned kettle body blowing process, strict requirements are imposed on the air pressure. If the air pressure is too high, the problems of thin bottom and thick opening of the kettle body can occur; if the air pressure is too low, the opening may be too thin or not blown at all, resulting in a problem of material shortage at the opening. Furthermore, in the technical scheme of the invention, the insertion pipe is formed by opening a hole at the upper middle part of the kettle body, so that the forming of the kettle body can be greatly influenced due to non-uniform air pressure in the blowing process. The forming of the kettle body adopts a mode of combining machine blowing and manual blowing, firstly, a machine automatic blowing mode is used for forming the kettle body to a central hole, and the air pressure of the machine in the blowing process is controlled to be 0.1-1 Kpa; when the opening is formed, manual blowing is added while the machine is blowing so as to ensure that the opening of the kettle body can be formed at one time and has uniform thickness.
Preferably, the kettle cover 11 and the kettle body 1 are detachably connected.
The kettle body can be provided with various specifications or different kettle covers so as to adapt to different sol preparation processes. When the product technology changes, the change of the function of the reaction kettle can be realized only by replacing the kettle cover connected with the flange.
Preferably, a polytetrafluoroethylene sealing gasket (not shown) is arranged between the kettle body 1 and the kettle cover 11.
The kettle body and the kettle cover are made of borosilicate glass, the material has excellent physical and chemical properties, and the tetrafluoroethylene sealing ring is arranged between the kettle body and the kettle cover, so that the double-layer glass reaction kettle has good sealing effect, high stability and good safety performance.
Preferably, the device also comprises a titration flask 112, a distillation condenser, a thermocouple 4, a pressure gauge 5 and a pH probe 6; the titration flask 112, the distillation condenser, the thermocouple 4 and the pressure gauge 5 are respectively installed on the kettle cover 11 through a titration flask interface, a distillation condenser interface, a thermocouple interface and a pressure gauge interface; the PH probe 6 is arranged on the kettle body 1 through the insertion pipe 14; the titration flask 112, the distillation condenser, the thermocouple 4, the pressure gauge 4 and the PH probe 6 are all fixed on the fixing frame 2.
The PH probe comprises a display screen, can monitor the PH value of a reaction medium in the double-layer glass reaction kettle in real time, and then adds acid or alkali to adjust the PH value of the reaction medium according to the needs, so that the pH value of the reaction medium always meets the technological requirements.
The thermocouple is used for monitoring the temperature of the reaction medium in real time.
And the pressure gauge monitors the pressure in the reaction kettle in real time.
Preferably, a fixed sealing piece is arranged at the interface of the titration flask, the interface of the distillation condenser, the interface of the thermocouple and the interface of the pressure gauge; and a rotary sealing element 7 is arranged at the contact position of the kettle cover and the stirring shaft.
Sealing parts are arranged at positions related to interface connection on the kettle cover, and are fixedly sealed or rotationally sealed according to conditions, so that the sealing inside the whole double-layer glass reaction kettle is ensured, and the process of reaction under a vacuum condition is realized.
Preferably, the titration flask 112 includes an acid titration flask and a base titration flask.
The PH probe is inserted into the kettle body through the insertion pipe, the PH value of the reaction medium is detected, and then an acid reagent or an alkali reagent is added to adjust the PH value of the sol according to the reading indication of the PH probe. The operation of adding acid or adding alkali can be automatically controlled by a controller, and the acid and alkali reagent can be added manually by using manual monitoring.
Preferably, the distillation condenser comprises a distillation flask 115, a distillation liquid receiver 114 and a cooling pipe 113; the cooling pipe 113 is coiled in the distillation flask 115; the distillation liquid receiving bottle 114 is disposed below the distillation bottle 115.
The reaction medium in the kettle body generates steam under the reaction temperature condition. When the steam rises into the distillation flask, the steam is condensed by the cooling pipe coiled in the distillation flask to form condensate; the condensate is dripped into the distillation liquid receiving bottle downwards and flows back into the reaction kettle after reaching a certain amount.
Preferably, it further comprises a water tank 151 and a water pump 152; the condensation pipe 113 comprises an upper water outlet and a lower water inlet; the water tank 151 is connected with the water outlet at the upper end of the cooling pipe 113; the water pump 152 is connected with the lower water inlet of the cooling pipe 113; the water tank 151, the water pump 152 and the condensation pipe 113 are sequentially connected through a pipe to form a cooling water circulation system.
When distillation is carried out, the water outlet at the upper end of the cooling pipe is connected with the water outlet pipe, and the water inlet at the lower end of the cooling pipe is connected with the water inlet pipe; the water pump conveys the cooling water in the water tank to a water inlet at the lower end of a cooling pipe in the distillation flask; and after the cooling water and the steam in the distillation flask finish indirect heat exchange, the water after absorbing heat is conveyed to a water return tank through a water outlet at the upper end to be cooled.
A thermostat control may be provided in the water tank to regulate the temperature of the cooling water.
Preferably, it also comprises a vacuum pump 9; the vacuum pump 9 is communicated with the double-layer glass reaction kettle through the distillation flask 115.
In actual production, the distillation flask can be connected with a vacuum pump according to the process requirement so as to vacuumize the kettle body; the reading of the pressure gauge shows that the vacuum condition of the reaction can be controlled.
Preferably, the device also comprises a circulating medium temperature controller 10, one end of which is connected with the circulating medium inlet 12, and the other end of which is connected with the circulating medium outlet 13; the temperature range of the circulating medium is-80 ℃ to 300 ℃.
In one embodiment of the present invention, the circulating medium temperature controller is a constant temperature heater for heating the medium fluid to keep the temperature of the medium fluid constant, so that the temperature of the double-layer glass reaction kettle can be kept stable when the medium circulates through the jacket structure.
Preferably, the stirrer 3 further comprises a motor 31 and a speed governor 32; the motor 31 and the speed regulator 32 are both fixed on the fixed frame 2; one end of the motor 31 is connected with the speed regulator 32, the other end of the motor is connected with the stirring shaft 33, and the rotating speed of the stirrer 3 is regulated through the regulator 32.
The stirrer is driven by the motor; the rotating speed of the motor can be adjusted and displayed through the speed regulator.
The speed regulator is connected with a display screen, and can display the rotating speed of the stirrer in real time.
The thermocouple is connected with the display screen and can display the temperature of the reaction medium in the double-layer glass reaction kettle in real time.
Preferably, the bottom of the fixed frame 2 is provided with a universal wheel 21 and a brake pad 211; the universal wheel 21 is used for moving the fixed frame 2; the brake pad 221 is used for braking the universal wheel 21.
The kettle body and all parts of the double-layer glass reaction kettle are fixed on the fixing frame; the fixing frame base angle is provided with the universal wheel with the brake block, so that the whole device can be moved conveniently.
The double-layer glass reaction kettle provided by the technical scheme of the invention can be used for preparing aerogel sol, can realize the accurate control of sol reaction conditions, ensures the quality of aerogel products and has better industrial value.
The features of the invention claimed and/or described in the specification may be combined, and are not limited to the combinations set forth in the claims by the recitations therein. The technical solutions obtained by combining the technical features in the claims and/or the specification also belong to the scope of the present invention.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are still within the scope of the technical solution of the present invention.

Claims (15)

1. The utility model provides a double glazing reation kettle of preparation aerogel sol which characterized in that, it includes:
the kettle body is of a jacket structure; the kettle body comprises a circulating medium inlet and a circulating medium outlet; an insert pipe penetrating through the side wall of the kettle body is arranged at the upper part of the middle part of the kettle body; a sol discharge hole is formed in the bottom of the kettle body;
the kettle cover is arranged above the kettle body and is connected with the kettle body through a flange; the kettle cover is provided with a feeding hole, a titration flask interface, a distillation condenser interface, a thermocouple interface, a pressure gauge interface and a stirrer interface;
the kettle body is fixedly arranged on the fixed frame;
the stirrer comprises a stirring shaft and a stirring paddle; the stirring shaft passes through the stirrer connector from the outside of the kettle cover and extends into the kettle body; and a stirring paddle is arranged on the stirring shaft extending into the kettle body.
2. The double-glazed reaction kettle of claim 1, wherein the insertion tube is disposed in an inclined upward direction, and the angle between the insertion tube and the vertical direction is 50 ± 10 °.
3. The double-glazed reaction kettle of claim 1, further comprising a PH probe; the PH probe can be inserted into the insertion tube; the inner surface of the insertion tube and the surface of the PH probe contacted with the insertion tube are both made of ground glass.
4. The double-glazed reaction kettle of claim 1, wherein the insert tube is integrally molded with the kettle body.
5. The double-layer glass reaction kettle of claim 1, wherein the kettle cover and the kettle body are detachably connected.
6. The double-layer glass reaction kettle of claim 1, wherein a polytetrafluoroethylene sealing gasket is arranged between the kettle body and the kettle cover.
7. The double-layer glass reaction kettle according to claim 1, further comprising a titration flask, a distillation condenser, a thermocouple, a pressure gauge and a pH probe; the titration flask, the distillation condenser, the thermocouple and the pressure gauge are respectively arranged on the kettle cover through a titration flask interface, a distillation condenser interface, a thermocouple interface and a pressure gauge interface; the PH probe is arranged on the kettle body through the insertion pipe; the titration flask, the distillation condenser, the thermocouple, the pressure gauge and the PH probe are all fixed on the fixing frame.
8. The double-layer glass reaction kettle according to claim 7, wherein fixed sealing parts are arranged at the interface of the titration flask, the interface of the distillation condenser, the interface of the thermocouple and the interface of the pressure gauge; and a rotary sealing element is arranged at the contact position of the kettle cover and the stirring shaft.
9. The double-glazed reaction kettle of claim 7, wherein the titration bottles comprise acid titration bottles and alkali titration bottles.
10. The double-layer glass reaction kettle according to claim 1, wherein the distillation condenser comprises a distillation flask, a distillation liquid receiving bottle and a cooling pipe; the cooling pipe is coiled in the distillation flask; the distillation liquid receiving bottle is arranged below the distillation bottle.
11. The double-layer glass reaction kettle according to claim 10, further comprising a water tank and a water pump; the condensation pipe comprises an upper end water outlet and a lower end water inlet; the water tank is connected with a water outlet at the upper end of the cooling pipe; the water pump is connected with a water inlet at the lower end of the cooling pipe; the water tank, the water pump and the condenser pipe are sequentially connected through a pipeline to form a cooling water circulation system.
12. The double-glazed reaction kettle of claim 1, further comprising a vacuum pump; the vacuum pump is communicated with the double-layer glass reaction kettle through the distillation flask.
13. The double-layer glass reaction kettle according to claim 1, further comprising a circulating medium temperature controller, wherein one end of the circulating medium temperature controller is connected with the circulating medium inlet, and the other end of the circulating medium temperature controller is connected with the circulating medium outlet; the temperature range of the circulating medium is-80 ℃ to 300 ℃.
14. The double-glazed reaction kettle of claim 1, wherein the stirrer further comprises a motor and a speed regulator; the motor and the speed regulator are both fixed on the fixed frame; one end of the motor is connected with the speed regulator, the other end of the motor is connected with the stirring shaft, and the rotating speed of the stirrer is regulated through the regulator.
15. The double-layer glass reaction kettle according to claim 1, wherein universal wheels and brake pads are arranged at the bottom of the fixing frame; the universal wheel is used for moving the fixing frame; the brake pad is used for braking the universal wheel.
CN202011231931.4A 2020-11-06 2020-11-06 Double-layer glass reaction kettle for preparing aerogel sol Pending CN112316873A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011231931.4A CN112316873A (en) 2020-11-06 2020-11-06 Double-layer glass reaction kettle for preparing aerogel sol

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Application Number Priority Date Filing Date Title
CN202011231931.4A CN112316873A (en) 2020-11-06 2020-11-06 Double-layer glass reaction kettle for preparing aerogel sol

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CN112316873A true CN112316873A (en) 2021-02-05

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111589392A (en) * 2020-06-28 2020-08-28 苏州北开生化设备有限公司 High-strength corrosion-resistant glass reaction kettle and preparation method thereof
CN113413854A (en) * 2021-07-02 2021-09-21 广东天诚生物降解材料有限公司 Equipment for preparing alkyl boron tetrahydrofuran solution

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111589392A (en) * 2020-06-28 2020-08-28 苏州北开生化设备有限公司 High-strength corrosion-resistant glass reaction kettle and preparation method thereof
CN113413854A (en) * 2021-07-02 2021-09-21 广东天诚生物降解材料有限公司 Equipment for preparing alkyl boron tetrahydrofuran solution

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