CN114653529A - Device and method for preparing silica aerogel felt and silica aerogel felt - Google Patents
Device and method for preparing silica aerogel felt and silica aerogel felt Download PDFInfo
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- CN114653529A CN114653529A CN202210336128.XA CN202210336128A CN114653529A CN 114653529 A CN114653529 A CN 114653529A CN 202210336128 A CN202210336128 A CN 202210336128A CN 114653529 A CN114653529 A CN 114653529A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C3/00—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material
- B05C3/02—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material
- B05C3/12—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material for treating work of indefinite length
- B05C3/15—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material for treating work of indefinite length not supported on conveying means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C11/00—Component parts, details or accessories not specifically provided for in groups B05C1/00 - B05C9/00
- B05C11/10—Storage, supply or control of liquid or other fluent material; Recovery of excess liquid or other fluent material
- B05C11/1039—Recovery of excess liquid or other fluent material; Controlling means therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C13/00—Means for manipulating or holding work, e.g. for separate articles
- B05C13/02—Means for manipulating or holding work, e.g. for separate articles for particular articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C9/00—Apparatus or plant for applying liquid or other fluent material to surfaces by means not covered by any preceding group, or in which the means of applying the liquid or other fluent material is not important
- B05C9/08—Apparatus or plant for applying liquid or other fluent material to surfaces by means not covered by any preceding group, or in which the means of applying the liquid or other fluent material is not important for applying liquid or other fluent material and performing an auxiliary operation
- B05C9/14—Apparatus or plant for applying liquid or other fluent material to surfaces by means not covered by any preceding group, or in which the means of applying the liquid or other fluent material is not important for applying liquid or other fluent material and performing an auxiliary operation the auxiliary operation involving heating or cooling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/18—Processes for applying liquids or other fluent materials performed by dipping
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/04—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
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Abstract
The invention relates to a device and method for preparing a silicon dioxide aerogel felt and the silicon dioxide aerogel felt. The device comprises a glue dipping tank, wherein the glue dipping tank is provided with a pressing roller; a liquid collecting tank is arranged on one side of the glue dipping tank, and a winding roller group is arranged above the liquid collecting tank; a hydrophobic drying box is arranged above the liquid collecting tank, the hydrophobic drying box is provided with a felt inlet and a felt outlet, and a tensioning mechanism and a drying assembly are arranged in the hydrophobic drying box; the tensioning mechanism comprises a tensioning roller group, and the tensioning roller group is used for tensioning the gel felt located between the felt inlet and the felt outlet; the drying assembly comprises an air injection assembly communicated with an air inlet pipe, the air injection assembly comprises an air distribution row and a plurality of hot air cutters communicated with the air distribution row, air outlets of the hot air cutters are aligned with the tensioned gel felt, and the air injection assembly is used for injecting preheated nitrogen and a gas-phase hydrophobic reagent to a fiber felt body; and an exhaust hole for discharging gas is reserved in the hydrophobic drying box. Hydrophobic and drying treatment of the silicon dioxide wet gel felt is realized, and the formed hydrophobic silicon dioxide aerogel felt is ensured to have relatively high quality.
Description
Technical Field
The invention belongs to the technical field of aerogel felt preparation, and particularly relates to a device and a method for preparing a silicon dioxide aerogel felt and the silicon dioxide aerogel felt.
Background
The aerogel is a gel material taking a dispersion medium as gas, has a highly-crosslinked continuous three-dimensional network nano hollow structure inside, and has a large specific surface area (500-2G) low density (30-150 Kg/m)3) High porosity (85-99%), small average pore diameter (2-50 nm), and lower thermal conductivity (0.01-0.02W/m.K) than room temperature air. Is currently recognized as the lowest thermal conductivity solid material. The silicon dioxide aerogel and the felt body thereof have unique physical and chemical properties, and are widely researched and applied in the aspects of aerospace, chemical engineering, energy-saving buildings, heat insulation, catalyst carriers, optics, acoustics and the like.
The existing preparation technology of the silica aerogel felt is mainly divided into two parts, namely: preparing gel and drying the gel. Silica gel to be dried is prepared by hydrolysis, gelation, aging and hydrophobization treatment of a silicon source, a solvent and a catalyst, and then the aerogel is obtained by drying the gel. The currently common hydrophobization method is to place the gum-dipped felt body into a prepared hydrophobization solution for hydrophobization after the gel reaction is finished, and then take out the treated gel felt for drying. Although this method can produce a hydrophobized silica aerogel blanket, it involves many times of solvent replacement in actual production, has a long reaction period, increases production costs, and is inefficient because the hydrophobization of the gel is not uniform due to the hydrophobization modification treatment of the gel by autolysis.
Disclosure of Invention
In view of the above, the present invention aims to provide a device for preparing a silica aerogel felt, which further realizes efficient, low-cost and uniform hydrophobization treatment on the basis of ensuring good structural performance of the aerogel felt; meanwhile, the invention also provides a method for preparing the silica aerogel felt; the invention also provides a silica aerogel felt.
In order to achieve the purpose, the technical scheme adopted by the device for preparing the silica aerogel felt is as follows:
an apparatus for continuously preparing a hydrophobic silica aerogel blanket at atmospheric pressure, comprising:
a glue dipping tank: the glue dipping tank is internally provided with a press roller for pressing the fiber felt body into the glue;
a liquid collecting tank: the winding roller group is arranged on one side of the dipping tank, the winding roller group is arranged above the liquid collecting tank, the fiber felt body after dipping is gelled between the dipping tank and the hydrophobic drying box to form a gel felt, and the winding roller group is a hot roller;
the hydrophobic drying box: the dewatering drying box is arranged above the liquid collecting tank, the dewatering drying box is provided with a felt inlet and a felt outlet, and a tensioning mechanism and a drying assembly are arranged inside the dewatering drying box;
the tensioning mechanism comprises a tensioning roller set, and the tensioning roller set is used for tensioning the gel felt positioned between the felt inlet and the felt outlet;
the drying component comprises an air injection component communicated with the air inlet pipe, the air injection component comprises an air distribution row and a plurality of hot air knives communicated with the air distribution row, air outlets of the hot air knives are aligned with the tensioned gel felt, and the air injection component is used for injecting preheated nitrogen and gas phase hydrophobization reagent to the gel felt; the hydrophobic drying box is provided with an exhaust hole for exhausting air.
Has the advantages that: the device for preparing the silica aerogel felt is simple in structure, the gel felt is blown by a gas-phase hydrophobic reagent with hot nitrogen in a hydrophobic drying box, the wet gel felt is subjected to hydrophobic treatment on the wet gel felt, and simultaneously an organic solvent in the wet gel can be brought out to realize hydrophobic and drying treatment on the silica aerogel felt, the formed hydrophobic silica aerogel felt is ensured to have higher quality.
Further, the air injection assembly comprises a first air injection assembly communicated with the first air inlet pipe and a second air injection assembly communicated with the second air inlet pipe.
Has the advantages that: the arrangement of the two groups of air injection assemblies is convenient to realize more uniform air injection when the gel felt is subjected to drying and hydrophobization treatment.
The felt inlet is arranged at the bottom of the hydrophobic drying box, the felt outlet is arranged at the top of the hydrophobic drying box, and the felt inlet and the felt outlet are arranged up and down correspondingly; the tensioning roller group comprises a first tensioning roller arranged at the felt inlet, a second tensioning roller arranged at the felt outlet, a third tensioning roller and a fourth tensioning roller, wherein the third tensioning roller and the fourth tensioning roller are positioned between the first tensioning roller and the second tensioning roller, and the third tensioning roller and the fourth tensioning roller are arranged at intervals in a vertically corresponding mode.
Has the advantages that: the tensioning roller group is arranged to tension the gel felt in the vertical extending direction in the hydrophobic drying box.
Furthermore, a wind shielding assembly is further arranged in the hydrophobic drying box and comprises a first wind shielding assembly and a second wind shielding assembly, the air injection assembly is positioned between the first wind shielding assembly and the second wind shielding assembly in the vertical direction, the first wind shielding assembly comprises a first supporting plate fixed on the inner wall of the hydrophobic drying box and a first wind shielding film fixed on the first supporting plate, and the first wind shielding film is in contact with a fourth tensioning roller; the second keeps off the wind subassembly including fixing the second backup pad at hydrophobic drying cabinet inner wall and fixing the second membrane that keeps off wind on first backup pad, the second membrane that keeps off wind contacts with third tensioning roller.
Has the advantages that: the setting of the subassembly that keeps out the wind can form the region of admitting air with jet-propelled subassembly combined action in one side of gel felt to make the gaseous gathering of jet-propelled subassembly spun in the region of admitting air, and make the gaseous and gel felt better emergence reaction of jet-propelled subassembly spun.
The gel felt is preheated by a heating device before entering a hydrophobic drying box.
Has the advantages that: the felt body is preheated by the heating device before the hydrophobic drying area, so that the hydrophobic drying time is shortened.
The winding roller group comprises a first winding roller and a second winding roller, the first winding roller and the second winding roller are arranged at left and right intervals, the second winding roller is located below the first winding roller, the liquid collecting tank is located right below the second winding roller, and the second winding roller and a felt inlet of the hydrophobic drying box are arranged up and down correspondingly.
Has the advantages that: the arrangement of the winding roller group prolongs the gel time of the wet gel felt on one hand, and facilitates the dripping of the redundant sol on the wet gel felt to the liquid collecting tank on the other hand.
The invention discloses a method for continuously preparing hydrophobic silica aerogel felt under normal pressure, which adopts the technical scheme that
A method of making a silica aerogel blanket comprising the steps of:
s1: unreeling a fiber roll felt, immersing a fiber felt body into a dipping tank under the action of a press roller for dipping treatment, and dipping the fiber felt into sol to obtain wet fiber felt combined with the sol;
s2: the wet fiber felt after the dipping treatment passes through a winding roller set, the dropped sol is collected into a liquid collecting tank, and the sol is gelatinized to form a gel felt before entering a hydrophobic drying box;
s3: and (3) the gel felt passes through a hydrophobic drying box, and the tensioned gel felt is swept by using preheated nitrogen and a gas-phase hydrophobic reagent in the hydrophobic drying box to obtain the dried aerogel felt.
Has the advantages that: the device for preparing the silica aerogel felt of the invention dips a fiber felt body through a dip tank to obtain a wet fiber felt, the wet fiber felt passes through a winding roller group, the gel felt is formed in the winding process of the winding roller group, meanwhile, sol dripped from the wet fiber felt is collected in a liquid collecting tank, the gel felt passes through the winding roller group and then enters a hydrophobic drying box, a tensioning roller group in the hydrophobic drying box tensions the gel felt, and a drying component in the hydrophobic drying box blows preheated nitrogen and a gas phase hydrophobic reagent on the gel felt, so that the gel felt forms a dry hydrophobic silica aerogel felt. The formed hydrophobic silica aerogel felt is ensured to have higher quality.
Further, in S3, the gel mat is first blown with a preheating gas through a purge valve to preheat the gel mat; then nitrogen is introduced into the hydrophobic drying box through the first gas injection assembly, and then the hot nitrogen and the gas phase hydrophobic reagent mixed gas are injected into the hydrophobic drying box through the second gas injection assembly.
Has the advantages that: the gel felt which is about to enter the hydrophobic drying box is preheated, so that the gel felt and the gas-phase hydrophobic reagent can react conveniently, and before the gas-phase hydrophobic reagent is introduced for hydrophobic treatment, the cyclic purging is performed through preheated nitrogen, so that the content of inert gas in the hydrophobic drying box is improved, and the consistency of a hydrophobic environment is improved.
In S3, blowing preheating gas to the gel felt through a purging valve to preheat the gel felt; hot nitrogen and gas phase hydrophobization reagents are directly sprayed into the hydrophobization drying box at the same time, and the nitrogen and the gas phase hydrophobization reagents are respectively and independently heated.
Has the advantages that: the gel felt which is about to enter the hydrophobic drying box is preheated, so that the gel felt and the gas-phase hydrophobic reagent are conveniently reacted, hot nitrogen and the gas-phase hydrophobic reagent are sprayed simultaneously, the nitrogen and the gas-phase hydrophobic reagent are respectively and independently heated, and are respectively sprayed by different air spraying assemblies or are sprayed by the same air spraying assembly, and the operation is simpler and more convenient.
When the mixed gas of the hot nitrogen and the gas-phase hydrophobization reagent is prepared, the hot nitrogen is introduced into the liquid-phase hydrophobization reagent, the liquid-phase hydrophobization reagent is heated by the hot nitrogen to be evaporated to obtain the gas-phase hydrophobization reagent, and the gas-phase hydrophobization reagent is introduced into the hydrophobization drying box along with the hot nitrogen through the gas injection assembly.
Has the advantages that: the hot nitrogen gas can change the liquid-phase hydrophobizing agent into the gas-phase hydrophobizing agent, and meanwhile, the hot nitrogen gas can also increase the content of inert gas in the hydrophobic drying oven.
A silica aerogel felt, the hydrophobic rate of the hydrophobic silica aerogel felt is 85.0-99.0%.
Drawings
FIG. 1 is a schematic diagram of the construction of an apparatus for making silica aerogel blankets according to the present invention;
FIG. 2 is a schematic view of the construction of the hydrophobic drying box of FIG. 1;
FIG. 3 is a schematic view of a first air jet assembly of the hydrophobic drying box of FIG. 2;
FIG. 4 is a left side view of the first jet assembly of FIG. 3;
FIG. 5 is a schematic view of a second air jet assembly of the hydrophobic drying box of FIG. 2;
fig. 6 is a left side view of the second air injection assembly of fig. 5.
Reference numerals: 1-a glue dipping tank; 2-a fibrous mat body; 3-pressing roller; 4-a liquid collecting tank; 5-a second winding roller; 6-first winding roller; 7-a purge valve; 8-hydrophobic drying oven; 9-a felt inlet; 10-a felt outlet; 11-an exhaust hole; 12-a set of tensioning rollers; 13-a gas injection assembly; 14-a first tensioning roller; 15-a second tensioning roller; 16-a third tensioning roller; 17-a fourth tensioning roller; 18-a sealing ring; 19-a first support plate; 20-a first wind-blocking film; 21-a second support plate; 22-a second wind-blocking film; 23-a first gas injection assembly; 24-first branch gas exhaust; 25-a first hot air knife; 26-a second gas injection assembly; 27-second gas distribution row; 28-a second hot air knife; 29-a first inlet line; 30-second inlet line.
Detailed Description
The invention relates to a device for preparing silica aerogel felt under normal pressure, which is further described in detail by combining the attached drawings and the specific embodiment:
as shown in figure 1, the device for preparing the silica aerogel felt comprises a dipping tank 1, a liquid collecting tank 4 and a hydrophobic drying box 8. The dipping tank 1 is used for containing a sol, and in this embodiment, the sol is a silica sol. The dipping tank 1 is provided with a press roller 3 for pressing the fiber felt body 2 into the sol to fully combine the fiber felt body 2 with the sol, in the embodiment, two parallel press rollers 3 are arranged in the dipping tank 1, and the spread fiber felt body 2 is pressed into the dipping tank by the two press rollers 3 to fully dip the sol in the dipping tank 1 on the fiber felt body 2. A sol replenishing tank (not shown in the figure) is arranged beside the dipping tank 1 and is used for continuously replenishing the sol in the dipping tank 1 to ensure that the liquid level of the sol in the dipping tank 1 keeps a certain height. In this embodiment, the fiber felt body 2 is continuously unreeled by an unreeling structure, which is a prior art and will not be described herein again, so as to continuously supply the fiber felt body 2 to the apparatus of the present invention. The fiber felt body 2 is combined with the sol in the glue dipping tank 1 to form a wet fiber felt;
a liquid collecting tank 4 is arranged on one side of the glue dipping tank 1, in the embodiment, the liquid collecting tank is arranged on the right side of the glue dipping tank 1, an opening of the liquid collecting tank 4 is arranged upwards, a winding roller group is arranged above the liquid collecting tank 4, and the impregnated fiber felt body 2 is gelled between the glue dipping tank and a hydrophobic drying box to form a gel felt. The winding roller group comprises a first winding roller 6 and a second winding roller 5, the first winding roller 6 and the second winding roller 5 are arranged at left and right intervals, the second winding roller 5 is positioned below the first winding roller 6, and the liquid collecting tank 4 is positioned right below the second winding roller 5; the wet fiber felt after the impregnation treatment passes through a winding roller group, and the sol is gelatinized to form gel felt when passing through the winding roller group. In the present invention, since the height of the second winding roller 5 is low, the sol is easily dropped at the second winding roller 5, and the dropped sol is collected in the sump 4. In this embodiment, the winding roller group is a hot roller, and the heating manner of the winding roller group is the prior art, which is not described herein again.
As shown in figure 2, a hydrophobic drying box 8 is arranged right above the liquid collecting tank 4, the hydrophobic drying box 8 is cuboid, a heat-insulating layer is arranged outside the box body of the hydrophobic drying box 8, the heat-insulating layer is made of heat-insulating materials, and the heat-insulating materials comprise one or more heat-insulating materials of aerogel, foam and mica. The hydrophobic drying box 8 is provided with a felt inlet 9 and a felt outlet 10, the felt inlet 9 is arranged at the bottom of the hydrophobic drying box 8, the felt outlet 10 is arranged at the top of the hydrophobic drying box 8, and the felt inlet 9 and the felt outlet 10 are arranged up and down correspondingly; elastic sealing rings 18 are arranged at the felt inlet 9 and the felt outlet 10, the outer edges of the sealing rings 18 are fixed at the felt inlet 9 and the felt outlet 10, and the inner edges of the sealing rings 18 are used for being in contact with the gel felt.
The gel felt is preheated through heating equipment before entering the hydrophobic drying box, in the embodiment, a purging valve 7 is arranged outside a felt inlet 9 of the hydrophobic drying box 8, the purging valve 7 is used for purging preheating gas to the fiber felt body 2, in the embodiment, the preheating gas is preheating nitrogen, the felt body is preheated nitrogen purged before a hydrophobic drying area, the felt body can be preheated firstly, and then a gas-phase hydrophobic reagent with hot nitrogen is used for purging, so that the hydrophobic drying time is shortened. In this embodiment, preheated nitrogen is blown out of the purge valve 7. The purge valve 7 is prior art and will not be described in detail herein. In this embodiment, the preheated nitrogen is heated by a nitrogen heater, and the temperature of the heated preheated nitrogen is 0-100 ℃ higher than the boiling point of the hydrophobizing agent, wherein the nitrogen heater is the prior art and is not described herein again.
A tensioning mechanism and a drying component are arranged in the hydrophobic drying box 8. Wherein, straining device includes tensioning roller set 12, tensioning roller set 12 is used for the tensioning to be located the gel felt between felt inlet 9 and the felt mouth 10, tensioning roller set 12 is including setting up the first tensioning roller 14 at felt inlet 9, the second tensioning roller 15 of setting at felt mouth 10, third tensioning roller 16, fourth tensioning roller 17, third tensioning roller 16 and fourth tensioning roller 17 are located between first tensioning roller 14 and second tensioning roller 15, third tensioning roller 16 corresponds the interval setting with fourth tensioning roller 17 from top to bottom, under straining device's effect, with the gel felt tensioning along upper and lower direction in the hydrophobic drying cabinet 8.
The drying assembly comprises an air injection assembly 13 communicated with the air inlet pipe, as shown in fig. 3-6, the air injection assembly 13 comprises an air distribution row and a plurality of hot air knives communicated with the air distribution row, air outlets of the hot air knives are aligned with the tensioned gel felt, and the air injection assembly 13 is used for injecting preheated nitrogen and gas phase hydrophobic reagent to the gel felt; an air vent 11 for exhausting air is reserved on the hydrophobic drying box 8.
In this embodiment, the air injection assembly 13 includes a first air injection assembly 23 communicated with a first air inlet pipe 29 and a second air injection assembly 26 communicated with a second air inlet pipe 30, the first air injection assembly 23 and the second air injection assembly 26 have the same structure, the first air injection assembly 23 includes a first air exhaust 24 extending in the vertical direction and a first hot air knife 25 communicating with the first air exhaust 24, the first hot air knife 25 is provided in a plurality at intervals in the vertical direction, the first hot air knife 25 extends horizontally and has a certain width in the front-rear direction, the cross-sectional area of the first hot air knife 25 decreases gradually from left to right, so that the air moves from left to right in the first hot air knife 25 and finally blows out from the air outlet on the right side at a high air speed. The second air injection assembly 26 includes a second air distribution row 27 extending along the vertical direction and a second hot air knife 28 communicating with the second air distribution row 27, the second hot air knife 28 is provided with a plurality of gaps along the vertical direction, the second hot air knife 28 extends horizontally and has a certain width in the front-rear direction, the cross-sectional area of the second hot air knife 28 decreases gradually from left to right, so that the air moves from left to right in the second hot air knife 28 and is finally blown out from the air outlet on the right side at a strong air speed.
A wind shielding assembly is further arranged in the hydrophobic drying box 8 and comprises a first wind shielding assembly and a second wind shielding assembly, the air injection assembly 13 is positioned between the first wind shielding assembly and the second wind shielding assembly in the vertical direction, the first wind shielding assembly comprises a first supporting plate 19 fixed on the inner wall of the hydrophobic drying box 8 and a first wind shielding film 20 fixed on the first supporting plate 19, the first wind shielding film 20 is soft, and the first wind shielding film 20 is in contact with a fourth tensioning roller 17; the second wind blocking component comprises a second supporting plate 21 fixed on the inner wall of the hydrophobic drying box 8 and a second wind blocking film 22 fixed on the first supporting plate 19, the second wind blocking film 22 is soft, and the second wind blocking film 22 is in contact with the third tensioning roller 16. The wind shielding assembly and the gas spraying assembly 13 can cooperate to form a gas inlet area on one side of the gel felt, so that gas sprayed by the gas spraying assembly 13 can be gathered in the gas inlet area, and the gel felt can be subjected to hydrophobic treatment better.
In this embodiment, the sol in the dipping tank 1 is a silica sol, and the silica sol is prepared by the following steps: taking a silicon source, ethanol and water, uniformly mixing the silicon source, the ethanol and the water according to the molar ratio of (1: 2-60) to (1-30), then adding a catalyst, and uniformly stirring to obtain the silica sol. The silicon source is one or more of ethyl orthosilicate, methyl orthosilicate, butyl orthosilicate, isopropyl orthosilicate and alkyl alkoxy silane. The alkylalkoxysilane includes one or more of methyltrimethoxysilane, dimethyldimethoxysilane, methyltriethoxysilane, dimethyldiethoxysilane, vinyltriethoxysilane, propyltrimethoxysilane, propyltriethoxysilane. The gel catalyst comprises an alkaline catalyst, and the alkaline catalyst is one or the combination of two of sodium hydroxide, potassium hydroxide, ammonia water and ammonium fluoride aqueous solution; alternatively, the gel catalyst may also be an acidic catalyst.
And a nitrogen making machine and a nitrogen heater (not shown in the figure) are arranged outside the hydrophobic drying box 8, the nitrogen making machine is communicated with the nitrogen heater through a connecting pipe, nitrogen is prepared through the nitrogen making machine, the volume content of the nitrogen is more than 99%, the prepared nitrogen is heated through the nitrogen heater, and then the gel felt is blown.
The invention discloses a method for preparing a silica aerogel felt, which comprises the following steps:
s1: unreeling the fiber roll felt, immersing the fiber felt body 2 into a dipping tank 1 for dipping under the action of a press roller 3, immersing the fiber felt into silica sol, and standing and aging for 8-24h at 30-60 ℃ to obtain the wet fiber felt combined with the sol.
S2: the wet fiber felt after the dipping treatment passes through the winding roller group, the dropped sol is collected into the liquid collecting tank 4, and the sol is gelatinized to form the gel felt before entering the hydrophobic drying box.
S3: and (3) the gel felt passes through a hydrophobic drying box, and the tensioned gel felt is swept by using preheated nitrogen and a gas-phase hydrophobic reagent in the hydrophobic drying box to obtain the dried aerogel felt.
In S3, the gel mat is first subjected to a preheating treatment by blowing a preheating gas through the purge valve 7 to the gel mat; then nitrogen is introduced into the hydrophobic drying box 8 through the first air injection assembly 23, and then hot nitrogen and gas phase hydrophobic reagent mixed gas is sprayed into the hydrophobic drying box 8 through the second air injection assembly 26; in this embodiment, when the mixed gas of the hot nitrogen and the gas-phase hydrophobizing agent is prepared, the hot nitrogen is introduced into the liquid-phase hydrophobizing agent, the liquid-phase hydrophobizing agent is heated by the hot nitrogen to evaporate the liquid-phase hydrophobizing agent to obtain the gas-phase hydrophobizing agent, and the gas-phase hydrophobizing agent is introduced into the hydrophobizing drying oven 8 along with the hot nitrogen through the gas injection assembly 13. According to the invention, the gas-phase hydrophobization reagent is adopted to carry out hydrophobization treatment on the gel felt, the gas-phase hydrophobization reagent can be rapidly diffused, dead angles are eliminated, the diffusion time is shortened, the using amount of the hydrophobization reagent is reduced, the hydrophobization efficiency is improved, meanwhile, a large amount of solvent replacement after the traditional hydrophobization reaction is finished can be avoided, and the whole preparation process is simple in process.
In this example, the hydrophobizing agent is methyltrimethoxysilane, dimethyldimethoxysilane, trimethylmethoxysilane, tetraethoxysilane, methyltriethoxysilane, dimethyldiethoxysilane, trimethylethoxysilane, ethyltrimethoxysilane, diethyldimethoxysilane, triethylmethoxysilane, triethylethoxysilane, diethyldiethoxysilane, ethyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, vinyltris (2-methoxyethoxy) silane, methylvinyldimethoxysilane, vinyltrichlorosilane, hexamethyldisiloxane, hexamethyldisilazane, heptamethyldisiloxane, heptamethyldisilazane, chloropropyltriethoxysilane, chloropropylmethyldimethoxysilane, dimethoxybis (2-methylpropyl) silane, dimethoxydimethoxydimethoxysilane, or a mixture thereof, One or more of bis (trimethylsiloxy) methylsilane, bis (1, 2-methyldichlorosilyl) ethane, bis (1, 2-trichlorosilane) ethane, bis (1, 2-methyldimethoxysilyl) ethane, bis (1, 2-methyldiethoxysilyl) ethane, bis (1, 2-trimethoxysilyl) ethane, bis (1, 2-triethoxysilyl) ethane, octyltriethoxysilane, trimethylchlorosilane, dimethyldichlorosilane, methyltrichlorosilane, triethylchlorosilane, diethyldichlorosilane and ethyltrichlorosilane.
The hydrophobic rate of the silica aerogel felt prepared by the silica aerogel felt is 85.0-99.0%.
In the invention, the gel felt is blown by a gas-phase hydrophobic reagent with hot nitrogen in the hydrophobic drying box 8, so that the hydrophobic treatment is carried out on the wet gel felt, meanwhile, the organic solvent in the wet gel can be brought out, and the hydrophobic and drying treatment on the silicon dioxide wet gel felt is realized. The preparation method disclosed by the invention can be used for continuously preparing the hydrophobic silica aerogel under normal pressure, the preparation period of the conventional hydrophobic aerogel can be obviously shortened, the production cost is reduced, the aerogel felt drying process and the aerogel hydrophobization treatment are simultaneously carried out, the operation is easy, the hydrophobization rate of the prepared hydrophobic silica aerogel is 85.0-99.0%, and the hydrophobization effect is good. In other embodiments, re-drying may also be performed, including one or more of ethanol supercritical drying, CO2 supercritical drying, atmospheric drying, and freeze drying.
In the above embodiment, the air injection assembly includes a first air injection assembly communicated with the first air inlet pipe and a second air injection assembly communicated with the second air inlet pipe; in other embodiments, only the first air injection assembly or only the second air injection assembly, or the first air injection assembly, the second air injection assembly, and the third air injection assembly may be provided according to the tensioned gel mat.
In the above embodiment, the tensioning roller group includes a first tensioning roller arranged at the felt inlet, a second tensioning roller arranged at the felt outlet, a third tensioning roller and a fourth tensioning roller, the third tensioning roller is located between the first tensioning roller and the second tensioning roller, the fourth tensioning roller is located between the first tensioning roller and the second tensioning roller, and the third tensioning roller and the fourth tensioning roller are correspondingly arranged at intervals up and down; in other embodiments, the tensioning roller group comprises a first tensioning roller arranged at the felt inlet, a second tensioning roller arranged at the felt outlet, a third tensioning roller, a fourth tensioning roller and a fifth tensioning roller, wherein the third tensioning roller is arranged between the first tensioning roller and the second tensioning roller, the fourth tensioning roller is arranged between the first tensioning roller and the second tensioning roller, the fifth tensioning roller is arranged between the first tensioning roller and the second tensioning roller, and the third tensioning roller, the fourth tensioning roller and the fifth tensioning roller are arranged at intervals up and down.
In the above embodiment, a wind shielding assembly is further arranged in the hydrophobic drying box, the wind shielding assembly comprises a first wind shielding assembly and a second wind shielding assembly, and the air injection assembly is located between the first wind shielding assembly and the second wind shielding assembly in the vertical direction; in other embodiments, the wind shielding assembly may not be provided, or only the first wind shielding assembly may be provided, or only the second wind shielding assembly may be provided.
In the embodiment, the purging valve is arranged outside the felt inlet of the hydrophobic drying box and used for purging the preheated gas to the fiber felt body; in other embodiments, the purge valve may not be provided; alternatively, the gel mat is preheated by radiant heating or preheated gas conduction heating.
In the embodiment, the winding roller group comprises a first winding roller and a second winding roller, the first winding roller and the second winding roller are arranged at left and right intervals, the second winding roller is positioned below the first winding roller, the liquid collecting tank is positioned right below the second winding roller, and the second winding roller and a felt inlet of the hydrophobic drying box are arranged up and down correspondingly; in other embodiments, the winding roller group comprises a first winding roller, a second winding roller and a third winding roller, the first winding roller, the second winding roller and the third winding roller are arranged at left and right intervals, the second winding roller is positioned below the first winding roller and the third winding roller, and the liquid collecting tank is positioned right below the second winding roller.
In the above embodiment, in S3, the gel mat is first subjected to a preheating treatment by blowing a preheating gas through the purge valve to the gel mat; then nitrogen is introduced into the hydrophobic drying box through the first gas injection assembly, and then the hot nitrogen and the gas phase hydrophobic reagent mixed gas are respectively injected into the hydrophobic drying box through the second gas injection assembly; in other embodiments, the gel mat may also be preheated without first passing through a purge valve; or when gas is introduced into the hydrophobic drying box, hot nitrogen and the gas-phase hydrophobic reagent are directly sprayed into the hydrophobic drying box simultaneously, and the nitrogen and the gas-phase hydrophobic reagent are respectively and independently heated.
Claims (10)
1. An apparatus for preparing silica aerogel blanket, comprising:
a glue dipping tank: the glue dipping tank is internally provided with a press roller for pressing the fiber felt body into the glue;
a liquid collecting tank: the winding roller group is arranged on one side of the dipping tank, the winding roller group is arranged above the liquid collecting tank, the fiber felt body after dipping is gelled between the dipping tank and the hydrophobic drying box to form a gel felt, and the winding roller group is a hot roller;
the hydrophobic drying box: the dewatering drying box is arranged above the liquid collecting tank, the dewatering drying box is provided with a felt inlet and a felt outlet, and a tensioning mechanism and a drying assembly are arranged inside the dewatering drying box;
the tensioning mechanism comprises a tensioning roller set, and the tensioning roller set is used for tensioning the gel felt positioned between the felt inlet and the felt outlet;
the drying assembly comprises an air injection assembly communicated with the air inlet pipe, the air injection assembly comprises an air distribution row and a plurality of hot air knives communicated with the air distribution row, air outlets of the hot air knives are aligned with the tensioned gel felt, and the air injection assembly is used for injecting preheated nitrogen and gas phase hydrophobic reagent to the gel felt; the hydrophobic drying box is provided with an exhaust hole for exhausting air.
2. The apparatus of claim 1, wherein the gas injection assembly comprises a first gas injection assembly in communication with a first gas inlet line and a second gas injection assembly in communication with a second gas inlet line.
3. The device for preparing the silica aerogel felt according to claim 1 or 2, wherein the felt inlet is arranged at the bottom of the hydrophobic drying box, the felt outlet is arranged at the top of the hydrophobic drying box, and the felt inlet and the felt outlet are arranged up and down correspondingly; the tensioning roller group comprises a first tensioning roller arranged at the felt inlet, a second tensioning roller arranged at the felt outlet, a third tensioning roller and a fourth tensioning roller, wherein the third tensioning roller and the fourth tensioning roller are positioned between the first tensioning roller and the second tensioning roller, and the third tensioning roller and the fourth tensioning roller are correspondingly arranged at intervals up and down; the gel felt is preheated by a heating device before entering a hydrophobic drying box.
4. The apparatus according to claim 3, wherein a wind shielding assembly is further disposed in the hydrophobic drying chamber, the wind shielding assembly comprises a first wind shielding assembly and a second wind shielding assembly, the air injection assembly is located between the first wind shielding assembly and the second wind shielding assembly in the up-down direction, the first wind shielding assembly comprises a first supporting plate fixed on the inner wall of the hydrophobic drying chamber and a first wind shielding film fixed on the first supporting plate, and the first wind shielding film is in contact with the fourth tensioning roller; the second keeps off the wind subassembly including fixing the second backup pad at hydrophobic drying cabinet inner wall and fixing the second membrane that keeps off wind on first backup pad, the second membrane that keeps off wind contacts with third tensioning roller.
5. The device for preparing the silica aerogel felt according to claim 1 or 2, wherein the winding roller group comprises a first winding roller and a second winding roller, the first winding roller and the second winding roller are arranged at a left-right interval, the second winding roller is arranged below the first winding roller, the liquid collecting tank is arranged right below the second winding roller, and the second winding roller is arranged corresponding to the felt inlet of the hydrophobic drying box up and down.
6. A method for preparing silica aerogel felt is characterized by comprising the following steps:
s1: unreeling a fiber roll felt, immersing a fiber felt body into a dipping tank under the action of a press roller for dipping treatment, and dipping the fiber felt into sol to obtain wet fiber felt combined with the sol;
s2: the wet fiber felt after the dipping treatment passes through a winding roller set, the dropped sol is collected into a liquid collecting tank, and the sol is gelatinized to form a gel felt before entering a hydrophobic drying box;
s3: and (3) the gel felt passes through a hydrophobic drying box, and the tensioned gel felt is swept by using preheated nitrogen and a gas-phase hydrophobic reagent in the hydrophobic drying box to obtain the dried aerogel felt.
7. The method of claim 6, wherein in step S3, the gel mat is preheated by blowing a preheating gas through the purge valve to the gel mat; then nitrogen is introduced into the hydrophobic drying box through the first gas injection assembly, and then the hot nitrogen and the gas phase hydrophobic reagent mixed gas are injected into the hydrophobic drying box through the second gas injection assembly.
8. The method of claim 6, wherein in step S3, the gel mat is preheated by blowing a preheating gas through the purge valve to the gel mat; hot nitrogen and gas phase hydrophobization reagents are directly sprayed into the hydrophobization drying box at the same time, and the nitrogen and the gas phase hydrophobization reagents are respectively and independently heated.
9. The method of claim 7, wherein the gas mixture of hot nitrogen and the vapor phase hydrophobizing agent is prepared by introducing hot nitrogen into the liquid phase hydrophobizing agent, heating the liquid phase hydrophobizing agent with the hot nitrogen to vaporize the resulting vapor phase hydrophobizing agent, and introducing the vapor phase hydrophobizing agent into the hydrophobic drying oven through the gas injection assembly with the hot nitrogen.
10. A silica aerogel blanket made by the process of any of claims 6-9, wherein the hydrophobic silica aerogel blanket made has a water repellency of 85.0% to 99.0%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115090227A (en) * | 2022-07-28 | 2022-09-23 | 巩义市泛锐熠辉复合材料有限公司 | Equipment and method for continuously preparing aerogel powder and aerogel powder |
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