CN108103837A - Novel nano sheathing paper and preparation method thereof - Google Patents
Novel nano sheathing paper and preparation method thereof Download PDFInfo
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- CN108103837A CN108103837A CN201711238316.4A CN201711238316A CN108103837A CN 108103837 A CN108103837 A CN 108103837A CN 201711238316 A CN201711238316 A CN 201711238316A CN 108103837 A CN108103837 A CN 108103837A
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H19/00—Coated paper; Coating material
- D21H19/10—Coatings without pigments
- D21H19/14—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H23/00—Processes or apparatus for adding material to the pulp or to the paper
- D21H23/02—Processes or apparatus for adding material to the pulp or to the paper characterised by the manner in which substances are added
- D21H23/22—Addition to the formed paper
- D21H23/50—Spraying or projecting
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H25/00—After-treatment of paper not provided for in groups D21H17/00 - D21H23/00
- D21H25/04—Physical treatment, e.g. heating, irradiating
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Paper (AREA)
Abstract
The present invention provides a kind of novel nano sheathing paper and preparation method thereof, and the preparation method includes preparing colloidal sol step, Shower gels step and supercritical drying step.In colloidal sol step is prepared, the presoma of preset blending ratio, alcoholic solvent, pure water and acidic catalyst are configured to colloidal sol.Spray is mixed in inorganic fibre paper in Shower gels step, while by colloidal sol and basic catalyst, to adhere to silica nanometer porous aerogel on inorganic fibre paper.In supercritical drying step, inorganic fibre paper is placed in the dried medium of ethyl alcohol, and ethyl alcohol is made to be maintained under pressure and 235 DEG C~300 DEG C of the temperature conditionss of 7MPa~10MPa, to extract the liquid phase in inorganic fibre paper.
Description
Technical field
The present invention relates to a kind of heat preserving and insulating material and preparation method thereof more particularly to a kind of novel nano sheathing paper and its
Preparation method.
Technical background
The composite material that inorfil matrix and aerosil are combined combines inorfil matrix
High temperature resistant, the lower thermal conductivity of the superior function that will not be burnt and aerosil, insulation, hydrophobic superiority
Can, it has a good application prospect.
Have at present much on the combination process research that aerosil and inorfil matrix are combined with each other.
For example, one way in which is by silicon dioxide aerogel powder, inorfil matrix and bonding agent compression moulding.Also one
Kind mode is to use fiber and porous article as skeleton the composite material of aerosil and inorfil is made.But
Due to the limitation of these combination process, aerosil dispersiveness is poor, and finally composite finished product obtained is heat-insulated
Property and heatproof combustion resistance are difficult to get a desired effect；The bad control of ratio in preparation process in addition, mechanical strength compared with
It is low so that the use scope of composite finished product is limited to very much, it is difficult to extensive use.
In another improved combination process, it would be desirable to colloidal sol first be made, then by colloidal sol obtained using spray
Mode be sprayed onto on inorfil basis material, and form aerosil on inorfil basis material, finally adopt
The inorfil matrix for being compounded with aerosil is dried by the use of carbon dioxide as dried medium, obtains inorganic fibre
The composite finished product of Wiki body and aerosil.But there is drawback in a manner that carbon dioxide is dried：
First, in addition to moisture, addition acid, alkali, salt and organic solvent etc. can be also related in combination process, therefore in drying
In the process, we are not only needed moisture, alcohol, organic substance removal, it is also necessary to are eliminated as much as residual on inorfil matrix
Some impurity stayed.And based on the property of carbon dioxide itself, for removal in a manner that carbon dioxide is as dried medium
The effect of impurity is undesirable.Second, since organic component being failed to remove in the drying process, composite finished product obtained is resistance to
Temperature is not high, if not adding hydrophobic material, the time kept in terms of hydrophobicity is not grown, also higher (the calcination lapse rate of calcination lapse rate
Generally more than 5%).3rd, high (in 300 DEG C of environment, paper shrinking percentage reaches paper shrinking percentage in 5 minutes during high temperature
10%), composite finished product can not be used in temperature end, and be suitable only in less than 260 DEG C of environment.This undoubtedly causes nothing
The application range of machine fibrous matrix and silicon dioxide silica aerogel composite material is restricted.
The content of the invention
The object of the present invention is to provide a kind of novel nano sheathing papers and preparation method thereof, solve existing silica airsetting
Glue and inorfil the matrix composite retention time in terms of hydrophobicity is not long, calcination lapse rate is high, can not be special at 300 DEG C or more
It is not the problem of 500 DEG C or so of temperature end uses.
To solve the above problems, the present invention provides a kind of preparation method of novel nano sheathing paper, the preparation method bag
It includes and prepares colloidal sol step, Shower gels step and supercritical drying step.
Prepare colloidal sol step：The presoma of preset blending ratio, alcoholic solvent, pure water and acidic catalyst are configured to colloidal sol.
Shower gels step：Colloidal sol and basic catalyst are mixed into spray in inorganic fibre paper simultaneously, in inorfil
Adhere to silica nanometer porous aerogel on paper.
Supercritical drying step：Inorganic fibre paper is placed in the dried medium of ethyl alcohol, and make ethyl alcohol be maintained at 7MPa~
Under the pressure of 10MPa and 235 DEG C~300 DEG C of temperature conditionss, to extract the liquid phase in inorganic fibre paper.
An embodiment according to the present invention, supercritical drying step include placing step, extraction step, separating step and release
Put pressure step.
Place step：Inorganic fibre paper is put into drying device.
Extraction step：The ethyl alcohol is poured into drying device, ethyl alcohol is heated to 235 DEG C~300 DEG C and is progressively pressurizeed
Kept for a few hours after to 7MPa~10MPa, so that the liquid phase in ethyl alcohol extraction inorganic fibre paper.
Separating step：Open the relief valve of drying device, the liquid phase that will be extracted and inorganic fibre paper separation.
Discharge pressure step：After completing separating step, the relief valve of the drying device is opened to discharge drying device
Interior pressure, until pressure and external pressure dynamic balance in drying device, wherein the pressure x velocity of release drying device is
1Mpa/h~3Mpa/h.
An embodiment according to the present invention, Shower gels step includes continuous spraying step and gel keeps step,
Continuous spraying step：Inorganic fibre paper is put into sprinkling equipment and spray is passed through with the speed of 15m/hr~20m/hr
The spraying zone of equipment, the colloidal sol and the basic catalyst are mixed spray simultaneously by the spraying zone of the sprinkling equipment
In the inorganic fibre paper, wherein the spray flow of the colloidal sol is 40L/h~200L/h, the spray stream of the basic catalyst
It measures as 8L/h~40L/h.
Gel keeps step：The inorganic fibre paper is impregnated 4~8 in alcohol liquid under 25 DEG C~60 DEG C of temperature conditionss
Hour, silica nanometer porous aerogel is adhered on the inorganic fibre paper with aging.
An embodiment according to the present invention, inorganic fibre paper using all-glass paper, quartz fibre paper, high silica fiber paper,
It is one or more in aluminum silicate fiber paper, mullite fiber paper, sepiolite fibre paper and basalt fibre paper.
An embodiment according to the present invention, in colloidal sol step is prepared, the presoma, alcoholic solvent, pure water, acidic catalyst
Molal weight proportioning for 1:(1~10):(0.4~3):(0.0005~0.1).
An embodiment according to the present invention, the raw material for preparing presoma are selected from methyl orthosilicate, ethyl orthosilicate and positive silicon
It is one or more in acid butyl ester.
An embodiment according to the present invention, alcoholic solvent are one or more in methanol, ethyl alcohol and isopropanol.
An embodiment according to the present invention, acidic catalyst are a kind of in hydrochloric acid, sulfuric acid, nitric acid, oxalic acid and hydrofluoric acid
It is or a variety of.
An embodiment according to the present invention, basic catalyst is one in sodium hydroxide, calcium hydroxide, ammonium hydroxide and sodium carbonate
Kind is a variety of.
According to another aspect of the present invention, the present invention also provides the preparation sides according to any of the above-described novel nano sheathing paper
Novel nano sheathing paper made from method, wherein the novel nano sheathing paper includes matrix, described matrix is attached with silica
Nanoporous aerogel, described matrix are the inorganic fibre paper, and the specific surface of the silica nanometer porous aerogel is
600m2/ g~1000m2/ g, the density 0.05g/cm of the silica nanometer porous aerogel3~0.08g/cm3, described two
The hole ratio 85%~98% of silica nanoporous aerogel, the bore hole size of the silica nanometer porous aerogel are
30nm~50nm, the novel nano sheathing paper keep the calcination lapse rate under conditions of 30min to be less than thousand points in 500 DEG C of environment
Three.
Compared with prior art, the technical program has the following advantages：
The present invention causes ethyl alcohol dried medium to protect by being used as dried medium using ethyl alcohol in supercritical drying step
The liquid phase extracted under the pressure of 7MPa~10MPa and 235 DEG C~300 DEG C of temperature conditionss in inorganic fibre paper is held, ethyl alcohol is not
There is good intermiscibility only for water, and be particularly remaining organic solvent for the other impurities in inorfil also to have
Good intermiscibility, it is particularly remaining so as to more thoroughly remove the moisture and other impurities in inorganic fibre paper
Organic solvent.Compared to traditional technology, supercritical drying process using the present invention can obtain better drying effect so that
The time that the novel nano sheathing paper of preparation is kept in terms of hydrophobicity is more long, and calcination lapse rate is lower.Specifically, novel nano every
The calcination lapse rate that hot paper places half an hour under 500 DEG C of hot environments is less than 3/1000ths.In addition, Performances of Novel Nano-Porous produced by the present invention
Rice sheathing paper keeps that 30min shrinking percentages are almost nil, i.e., finished product produced by the present invention is in 500 DEG C of height under 500 DEG C of hot environments
30min almost ungauged regions are kept under warm environment.
Description of the drawings
Fig. 1 is the flow chart of the preparation method of novel nano sheathing paper provided by one embodiment of the present invention；
Fig. 2 is the flow chart of the preparation method for the novel nano sheathing paper that another embodiment of the present invention provides.
Specific embodiment
It is described below and is served only for disclosing the present invention so that those skilled in the art can implement the present invention.In being described below
Embodiment be only used as illustrating, it may occur to persons skilled in the art that other obvious are deformed.It defines in the following description
The basic principle of the present invention can be applied to other embodiments, deformation scheme, improvement project, equivalent program and other do not carry on the back
Other schemes from spirit and scope of the invention.
As shown in Figure 1, one embodiment of the invention provides a kind of preparation method of novel nano sheathing paper and passes through institute
State novel nano sheathing paper made from preparation method.The preparation method of the novel nano sheathing paper include preparing colloidal sol step,
Shower gels step and supercritical drying step.
In colloidal sol step is prepared, the presoma of preset blending ratio, alcoholic solvent, pure water and acidic catalyst are configured to molten
Glue.
The presoma, alcoholic solvent, pure water, the molal weight proportioning of acidic catalyst are 1:(1~10):(0.4~3):
(0.0005~0.1).Wherein presoma uses silicon alkoxide, and the raw material for preparing presoma is selected from methyl orthosilicate, ethyl orthosilicate
It is or one or more in butyl silicate.Alcoholic solvent is one or more in methanol, ethyl alcohol, isopropanol.Acidic catalyst selects
One or more from hydrochloric acid, sulfuric acid, nitric acid, oxalic acid, hydrofluoric acid.
It it is noted that can be using a variety of mixing in methanol, ethyl alcohol and isopropanol as alcoholic solvent；Can by hydrochloric acid,
A variety of mixing in sulfuric acid, nitric acid, oxalic acid and hydrofluoric acid are as acidic catalyst.
Spray is mixed in inorganic fibre paper in Shower gels step, while by colloidal sol and basic catalyst, with inorganic
Adhere to silica nanometer porous aerogel in fibrous paper.That is, by the way of spray on inorganic fibre paper simultaneously
The colloidal sol and basic catalyst that mixing spray is prepared, colloidal sol and basic catalyst are finally generated by reaction on inorganic fibre paper
And adhere to silica nanometer porous aerogel.
Optionally, inorganic fibre paper using all-glass paper, quartz fibre paper, high silica fiber paper, aluminum silicate fiber paper,
It is one or more in mullite fiber paper, sepiolite fibre paper or basalt fibre paper.
Optionally, basic catalyst is one or more in sodium hydroxide, calcium hydroxide, ammonium hydroxide, sodium carbonate.For changing
One of it, basic catalyst may be employed in sodium hydroxide, calcium hydroxide, ammonium hydroxide, sodium carbonate；It or can also be by hydrogen
A variety of in sodium oxide molybdena, calcium hydroxide, ammonium hydroxide, sodium carbonate carry out mixing as basic catalyst.
Further, as shown in Fig. 2, in another embodiment of the present invention, using continuous point in the Shower gels step
Not spray-gel process, the Shower gels step includes continuous spraying step and gel keeps step.
Continuous spraying step：Inorganic fibre paper is put into sprinkling equipment and spray is passed through with the speed of 15m/hr~20m/hr
The spraying zone of equipment, colloidal sol and basic catalyst are mixed spray in inorfil simultaneously by the spraying zone of sprinkling equipment
Paper, wherein the spray flow of the colloidal sol is 40L/h~200L/h (l/h), the spray flow of the basic catalyst is 8L/
H~40L/h.
Specifically, the colloidal sol and basic catalyst that spray is prepared are mixed on inorganic fibre paper using a sprinkling equipment.
Sprinkling equipment has spraying zone, and colloidal sol and basic catalyst are mixed spray in inorganic fibre simultaneously by the spraying zone of sprinkling equipment
Tie up paper.Such as the sprinkling equipment of the new model ZL-Q01 of just grand mechanical Science and Technology Ltd. in Kunshan may be employed.In practical operation
In, the colloidal sol of preparation and basic catalyst are first stored respectively in sprinkling equipment, then by inorganic fibre paper with 15m/hr~
Colloidal sol and basic catalyst are mixed spray by the speed of 20m/hr by the spraying zone of sprinkling equipment, sprinkling equipment by spraying zone
To inorganic fibre paper.
Gel keeps step：The inorganic fibre paper is impregnated 4~8 in alcohol liquid under 25 DEG C~60 DEG C of temperature conditionss
Hour, silica nanometer porous aerogel is adhered on the inorganic fibre paper with aging.In this way, it is sprayed to inorganic fibre paper
On colloidal sol and basic catalyst under 25 DEG C~60 DEG C of temperature conditionss in alcohol liquid keep 4~8 it is small when, finally in inorganic fibre
Adhere to aerosil on dimension paper, and by 4~8 retention time when small, aerosil is aging reinforcing.
In supercritical drying step, the inorganic fibre paper is placed in the dried medium of ethyl alcohol, and keeps ethyl alcohol
Under the pressure of 7MPa~10MPa and 235 DEG C~300 DEG C of temperature conditionss, to extract the liquid phase in the inorganic fibre paper.It can
With understanding, after Shower gels step, the silica nanometer porous aerogel of inorganic fibre paper and attachment contains
There are moisture, organic solvent and some other impurity.These moisture, organic solvent and impurity can influence novel nano obtained
The performance parameters such as hydrophobicity, shrinking percentage, the calcination lapse rate of sheathing paper, therefore also need to through the supercritical drying step
Processing is dried.And ethyl alcohol has preferable compatibility for moisture, organic solvent and some other impurity, in 7MPa
Ethyl alcohol can preferably extract inorganic fibre paper and particularly adhere under the pressure of~10MPa and 235 DEG C~300 DEG C of temperature conditionss
Silica nanometer porous aerogel in liquid phase, play the role of dry removal of impurities.
Further, in another embodiment of the present invention, the supercritical drying step, which further includes, places step, extraction step
Suddenly, separating step and release pressure step.Place step：The inorganic fibre paper is put into drying device.Extraction step：
The ethyl alcohol is poured into the drying device, by the ethyl alcohol be heated to 235 DEG C~300 DEG C and be progressively forced into 7MPa~
A few hours are kept after 10MPa, so that the ethyl alcohol extracts the liquid phase in the inorganic fibre paper.Separating step：It opens described dry
The relief valve of dry device, the liquid phase that will be extracted and inorganic fibre paper separation.Discharge pressure step：Complete separating step it
Afterwards, the relief valve of the drying device is opened to discharge the pressure in the drying device, until the pressure in the drying device
Power and external pressure dynamic balance, wherein the pressure x velocity for discharging the drying device is 1Mpa/h~3Mpa/h.
In separating step, the ethyl alcohol for having liquid phase with extraction is released, and the pressure in drying device will be declined, this
When can close relief valve, slowly heat up, the pressure in drying device to be kept to maintain 7MPa~10MPa.
Wherein described extraction step and the separating step are carried out at the same time.That is, it is originally poured into drying device
Ethyl alcohol, ethyl alcohol can be extracted in the case where reaching 235 DEG C~300 DEG C of temperature, the pressure condition of 7MPa~10MPa in inorganic fibre paper
Liquid phase；, it is necessary to open the relief valve of drying device during alcohol extraction liquid phase, slowly to discharge ethyl alcohol, so extract
The ethyl alcohol for having liquid phase is released, and liquid phase is separated with ethyl alcohol and inorganic fibre paper.Extraction step and separating step are carried out at the same time, dry
Ethyl alcohol pressure and temperature in device keeps dynamic equilibrium.
Pass through the porous airsetting of silica nanometer of its attachment of novel nano sheathing paper made from the preparation method of the present invention
The specific surface of glue is 600m2/ g~1000m2/ g, the density 0.05g/cm of silica nanometer porous aerogel3~0.08g/
cm3, the hole ratio 85%~98% of silica nanometer porous aerogel, the bore hole size of silica nanometer porous aerogel
30nm~50nm.(calcination subtracts the calcination lapse rate that novel nano sheathing paper is placed under conditions of half an hour under 500 DEG C of hot environments
Rate refers to that sample is placed on the slip of its rear quality in high-temperature heating environment) it is less than 3/1000ths.
The thickness of final obtained novel nano sheathing paper is 0.2mm~2.0mm, the room temperature heat conduction of novel nano sheathing paper
Coefficient (establishing criteria GB/T10295-2008) is below 0.023W/mK, and the compressive strength of novel nano sheathing paper is (according to mark
Quasi- GJB1585A-2004) it is 6.5MPa.
The time that novel nano sheathing paper provided by the invention is kept in terms of hydrophobicity is longer, and calcination lapse rate is lower.Tool
Body, the time that the novel nano sheathing paper is kept in terms of hydrophobicity is more longlasting, and novel nano sheathing paper is in 500 DEG C of high temperature
The calcination lapse rate that half an hour is placed under environment is less than 3/1000ths.The novel nano sheathing paper is protected under 500 DEG C of hot environments
It is almost nil to hold 30min shrinking percentages, i.e., described novel nano sheathing paper almost ungauged regions under the high temperature conditions.It is provided by the invention
The novel nano sheathing paper high temperature resistance is good, is very suitable for using in high temperature environments, is particluarly suitable for 500 DEG C or more
It is used in hot environment.The novel nano sheathing paper can meet Aeronautics and Astronautics, military equipment and it is civilian in all kinds of harshnesses
Thermal protection requirement, the fields such as fire prevention, fire-retardant, sound insulation, damping can also be applied to.
Embodiment 1：
In the embodiment of the present invention 1, the preparation method of the novel nano sheathing paper comprises the following steps：
A, it is 1 by mole quality proportioning by presoma, alcoholic solvent, pure water and acidic catalyst:1:0.4:0.0005 matches somebody with somebody
Colloidal sol is made, wherein presoma uses methyl orthosilicate, and alcoholic solvent uses methanol, and acidic catalyst uses hydrochloric acid；
B, inorganic fibre paper is put into sprinkling equipment and spraying zone with the speed of 15m/hr by sprinkling equipment, to pass through
Colloidal sol and basic catalyst are mixed spray in the spray rate of inorganic fibre paper, wherein colloidal sol by the spraying zone of sprinkling equipment simultaneously
For 40L/h, the spray rate of basic catalyst is 8L/h；Wherein inorganic fibre paper uses all-glass paper, and basic catalyst is adopted
With sodium hydroxide, the molal weight of methyl orthosilicate and sodium hydroxide is than 1:0.0005；
C, inorganic fibre paper is impregnated in alcohol liquid under 25 DEG C of temperature conditionss 4 it is small when, with aging in inorganic fibre paper
Upper attachment silica nanometer porous aerogel；
D, inorganic fibre paper is put into drying device；
E, ethyl alcohol is poured into drying device, ethyl alcohol is heated to 235 DEG C and is kept for a few hours after being progressively forced into 7MPa,
So that the liquid phase in ethyl alcohol extraction inorganic fibre paper；
F, the relief valve of drying device, the liquid phase that will be extracted and inorganic fibre paper separation are opened；
G, after completing separating step, the relief valve of drying device is opened to discharge the pressure in drying device, until dry
Pressure and external pressure dynamic balance in dry device, wherein the pressure x velocity for discharging the drying device is 1Mpa/h.
Pass through the porous airsetting of silica nanometer of its attachment of novel nano sheathing paper made from the above-mentioned steps of embodiment 1
The specific surface of glue is 600m2/ g, density 0.05g/cm3, hole ratio 85%, bore hole size 30nm-50nm.Final novel nano
The thickness of sheathing paper is 0.4mm；Its room temperature thermal conductivity factor (establishing criteria GB/T10295-2008) is：0.021W/m·K；Compression
Intensity (establishing criteria GJB1585A-2004) is：6.5MPa.
Embodiment 2：
In the embodiment of the present invention 2, the preparation method of the novel nano sheathing paper comprises the following steps：
A, it is 1 by mole quality proportioning by presoma, alcoholic solvent, pure water and acidic catalyst:10:3:0.1 is configured to
Colloidal sol, wherein presoma use ethyl orthosilicate, and alcoholic solvent uses ethyl alcohol, and acidic catalyst uses oxalic acid；
B, inorganic fibre paper is put into sprinkling equipment and spraying zone with the speed of 20m/hr by sprinkling equipment, to pass through
Colloidal sol and basic catalyst are mixed spray in the spray rate of inorganic fibre paper, wherein colloidal sol by the spraying zone of sprinkling equipment simultaneously
For 200L/h, the spray rate of basic catalyst is 40L/h；Wherein inorganic fibre paper uses quartz fibre paper, basic catalyst
Using calcium hydroxide, the molal weight of ethyl orthosilicate and calcium hydroxide is than 1:0.0005；
C, inorganic fibre paper is impregnated in alcohol liquid under 60 DEG C of temperature conditionss 8 it is small when, with aging in inorganic fibre paper
Upper attachment silica nanometer porous aerogel；
D, inorganic fibre paper is put into drying device；
E, ethyl alcohol is poured into drying device, ethyl alcohol is heated to 300 DEG C and keeps number small after being progressively forced into 10MPa
When, so that the liquid phase in ethyl alcohol extraction inorganic fibre paper；
F, the relief valve of drying device, the liquid phase that will be extracted and inorganic fibre paper separation are opened；
G, after completing separating step, the relief valve of drying device is opened to discharge the pressure in drying device, until dry
Pressure and external pressure dynamic balance in dry device, wherein the pressure x velocity of release drying device is 3Mpa/h.
Pass through the porous airsetting of silica nanometer of its attachment of novel nano sheathing paper made from the above-mentioned steps of embodiment 2
The specific surface of glue is 800m2/ g, density 0.08g/cm3, hole ratio 89%, bore hole size 50nm.Final novel nano sheathing paper
Thickness be 0.5mm；Its room temperature thermal conductivity factor (establishing criteria GB/T10295-2008) is：0.022W/m·K；Compressive strength
(establishing criteria GJB1585A-2004) is：6.5MPa.
Embodiment 3：
In the embodiment of the present invention 3, the preparation method of the novel nano sheathing paper comprises the following steps：
A, it is 1 by mole quality proportioning by presoma, alcoholic solvent, pure water and acidic catalyst:5:1.8:0.05 prepares
Into colloidal sol, wherein presoma uses butyl silicate, and alcoholic solvent uses isopropanol, and acidic catalyst uses hydrofluoric acid；
B, inorganic fibre paper is put into sprinkling equipment and spraying zone with the speed of 17.5m/hr by sprinkling equipment, with logical
Colloidal sol and basic catalyst are mixed spray in the spray speed of inorganic fibre paper, wherein colloidal sol by the spraying zone for crossing sprinkling equipment simultaneously
It spends for 120L/h, the spray rate of basic catalyst is 24L/h；Wherein inorganic fibre paper uses high silica fiber paper, and alkalescence is urged
Agent uses ammonium hydroxide, and the molal weight of butyl silicate and ammonium hydroxide is than 1:0.0005；
C, inorganic fibre paper is impregnated in alcohol liquid under 40 DEG C of temperature conditionss 6 it is small when, with aging in inorganic fibre paper
Upper attachment silica nanometer porous aerogel；
D, inorganic fibre paper is put into drying device；
E, ethyl alcohol is poured into drying device, ethyl alcohol is heated to 270 DEG C and keeps number small after being progressively forced into 8.5MPa
When, so that the liquid phase in ethyl alcohol extraction inorganic fibre paper；
F, the relief valve of drying device, the liquid phase that will be extracted and inorganic fibre paper separation are opened；
G, after completing separating step, the relief valve of drying device is opened to discharge the pressure in drying device, until dry
Pressure and external pressure dynamic balance in dry device, wherein the pressure x velocity of release drying device is 2Mpa/h.
Pass through the porous airsetting of silica nanometer of its attachment of novel nano sheathing paper made from the above-mentioned steps of embodiment 3
The specific surface of glue is 900m2/ g, density 0.065g/cm3, hole ratio 98%, bore hole size 40nm.Final novel nano is heat-insulated
The thickness of paper is 1.1mm；Its room temperature thermal conductivity factor (establishing criteria GB/T10295-2008) is：0.020W/m·K；Compressive strength
(establishing criteria GJB1585A-2004) is：6.5MPa.
Embodiment 4：
In the embodiment of the present invention 4, the preparation method of the novel nano sheathing paper comprises the following steps：
A, it is 1 by mole quality proportioning by presoma, alcoholic solvent, pure water and acidic catalyst:6:2:0.08 is configured to
Colloidal sol, wherein presoma use butyl silicate, and alcoholic solvent uses isopropanol, and acidic catalyst uses hydrofluoric acid；
B, inorganic fibre paper is put into sprinkling equipment and spraying zone with the speed of 16m/hr by sprinkling equipment, to pass through
Colloidal sol and basic catalyst are mixed spray in the spray rate of inorganic fibre paper, wherein colloidal sol by the spraying zone of sprinkling equipment simultaneously
For 100L/h, the spray rate of basic catalyst is 30L/h；Wherein inorganic fibre paper uses high silica fiber paper, base catalysis
Agent uses ammonium hydroxide, and the molal weight of butyl silicate and ammonium hydroxide is than 1:0.0005；
C, inorganic fibre paper is impregnated in alcohol liquid under 50 DEG C of temperature conditionss 7 it is small when, with aging in inorganic fibre paper
Upper attachment silica nanometer porous aerogel；
D, inorganic fibre paper is put into drying device；
E, ethyl alcohol is poured into drying device, ethyl alcohol is heated to 285 DEG C and is kept for a few hours after being progressively forced into 9MPa,
So that the liquid phase in ethyl alcohol extraction inorganic fibre paper；
F, the relief valve of drying device, the liquid phase that will be extracted and inorganic fibre paper separation are opened；
G, after completing separating step, the relief valve of drying device is opened to discharge the pressure in drying device, until dry
Pressure and external pressure dynamic balance in dry device, wherein the pressure x velocity of release drying device is 2.5Mpa/h.
Pass through the porous airsetting of silica nanometer of its attachment of novel nano sheathing paper made from the above-mentioned steps of embodiment 4
The specific surface of glue is 1000m2/ g, density 0.06g/cm3, hole ratio 96%, bore hole size 37nm.Final novel nano is heat-insulated
The thickness of paper is 1.5mm；Its room temperature thermal conductivity factor (establishing criteria GB/T10295-2008) is：0.021W/m·K；Compressive strength
(establishing criteria GJB1585A-2004) is：6.5MPa.
Take its specific surface of silica nanometer porous aerogel obtained in the range of present invention process higher, density compared with
Height, final finished product room temperature thermal conductivity factor smaller obtained, compressive strength higher.And the data beyond the processing range are taken, most
Its specific surface of silica nanometer porous aerogel is larger made from end, and density is relatively low, final finished product room temperature heat conduction system obtained
Number bigger, compressive strength are lower.
It will be appreciated by those skilled in the art that foregoing description and attached the embodiment of the present invention shown in figure are only used as lifting
Example, is not intended to limit the present invention.The purpose of the present invention has been fully and effectively achieved.The function and structure principle of the present invention exists
Show and illustrate in embodiment, in the case that without departing from the principle, embodiments of the present invention can have any deformation and
Modification.
Claims (10)
1. a kind of preparation method of novel nano sheathing paper, which is characterized in that comprise the following steps：
Prepare colloidal sol step：The presoma of preset blending ratio, alcoholic solvent, pure water and acidic catalyst are configured to colloidal sol；
Shower gels step：The colloidal sol and basic catalyst are mixed into spray in inorganic fibre paper simultaneously, with described inorganic
Adhere to silica nanometer porous aerogel in fibrous paper；And
Supercritical drying step：The inorganic fibre paper is placed in the dried medium of ethyl alcohol, and make ethyl alcohol be maintained at 7MPa~
Under the pressure of 10MPa and 235 DEG C~300 DEG C of temperature conditionss, to extract the liquid phase in the inorganic fibre paper.
2. the preparation method of novel nano sheathing paper according to claim 1, which is characterized in that the supercritical drying step
Suddenly include：
Place step：The inorganic fibre paper is put into drying device；
Extraction step：The ethyl alcohol is poured into the drying device, the ethyl alcohol is heated to 235 DEG C~300 DEG C and progressively
Kept for a few hours after being forced into 7MPa~10MPa, so that the ethyl alcohol extracts the liquid phase in the inorganic fibre paper；
Separating step：The relief valve of the drying device is opened, the liquid phase that will be extracted and inorganic fibre paper separation；And
Discharge pressure step：After completing separating step, the relief valve of the drying device is opened to discharge the drying device
Interior pressure, until pressure and external pressure dynamic balance in the drying device, wherein discharging the pressure of the drying device
Power speed is 1Mpa/h~3Mpa/h.
3. the preparation method of novel nano sheathing paper according to claim 1, which is characterized in that the Shower gels step
Including：
Continuous spraying step：The inorganic fibre paper is put into sprinkling equipment and is passed through with the speed of 15m/hr~20m/hr described
The spraying zone of sprinkling equipment, simultaneously to be mixed the colloidal sol and the basic catalyst by the spraying zone of the sprinkling equipment
It sprays in the inorganic fibre paper, wherein the spray flow of the colloidal sol is 40L/h~200L/h, the spray of the basic catalyst
Leaching flow is 8L/h~40L/h；And
Gel keeps step：It is small that the inorganic fibre paper is impregnated in alcohol liquid to 4~8 under 25 DEG C~60 DEG C of temperature conditionss
When, silica nanometer porous aerogel is adhered on the inorganic fibre paper with aging.
4. the preparation method of novel nano sheathing paper according to claim 1, which is characterized in that the inorganic fibre paper is adopted
With all-glass paper, quartz fibre paper, high silica fiber paper, aluminum silicate fiber paper, mullite fiber paper, sepiolite fibre paper with
It is and one or more in basalt fibre paper.
5. the preparation method of novel nano sheathing paper according to claim 1, which is characterized in that in the preparation colloidal sol step
In rapid, the presoma, alcoholic solvent, pure water, the molal weight proportioning of acidic catalyst are 1:(1~10):(0.4~3):
(0.0005~0.1).
6. the preparation method of novel nano sheathing paper according to claim 1, which is characterized in that prepare the presoma
Raw material is one or more in methyl orthosilicate, ethyl orthosilicate and butyl silicate.
7. the preparation method of novel nano sheathing paper according to claim 1, which is characterized in that the alcoholic solvent is selected from first
It is one or more in alcohol, ethyl alcohol and isopropanol.
8. the preparation method of novel nano sheathing paper according to claim 1, which is characterized in that the acidic catalyst choosing
It is one or more from hydrochloric acid, sulfuric acid, nitric acid, oxalic acid and hydrofluoric acid.
9. the preparation method of novel nano sheathing paper according to claim 1, which is characterized in that the basic catalyst choosing
It is one or more from sodium hydroxide, calcium hydroxide, ammonium hydroxide and sodium carbonate.
10. novel nano made from the preparation method of novel nano sheathing paper according to any one of claims 1 to 9 is heat-insulated
Paper, wherein the novel nano sheathing paper includes matrix, described matrix is attached with silica nanometer porous aerogel, the base
Body is the inorganic fibre paper, and the specific surface of the silica nanometer porous aerogel is 600m2/ g~1000m2/ g, it is described
The density 0.05g/cm of silica nanometer porous aerogel3~0.08g/cm3, the silica nanometer porous aerogel
Hole ratio 85%~98%, the bore hole size of the silica nanometer porous aerogel are 30nm~50nm, the Performances of Novel Nano-Porous
Rice sheathing paper keeps the calcination lapse rate under conditions of 30min to be less than 3/1000ths in 500 DEG C of environment.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110219201A (en) * | 2019-05-05 | 2019-09-10 | 齐鲁工业大学 | A kind of preparation method of basalt fibre paper |
| CN111778649A (en) * | 2020-06-18 | 2020-10-16 | 华陆工程科技有限责任公司 | Method for quickly preparing nano heat-insulating material through supercritical drying |
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| WO2009062518A1 (en) * | 2007-11-12 | 2009-05-22 | Biolocus A/S | Anti-fouling composition comprising an aerogel |
| CN101445356A (en) * | 2008-11-27 | 2009-06-03 | 中南大学 | Nano-hole aerogel heat-insulating composite material and preparation method thereof |
| CN107313289A (en) * | 2017-06-28 | 2017-11-03 | 浙江贝来新材料有限公司 | Hydrophobicity thermal insulating paper and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009062518A1 (en) * | 2007-11-12 | 2009-05-22 | Biolocus A/S | Anti-fouling composition comprising an aerogel |
| CN101445356A (en) * | 2008-11-27 | 2009-06-03 | 中南大学 | Nano-hole aerogel heat-insulating composite material and preparation method thereof |
| CN107313289A (en) * | 2017-06-28 | 2017-11-03 | 浙江贝来新材料有限公司 | Hydrophobicity thermal insulating paper and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110219201A (en) * | 2019-05-05 | 2019-09-10 | 齐鲁工业大学 | A kind of preparation method of basalt fibre paper |
| CN110219201B (en) * | 2019-05-05 | 2022-01-28 | 齐鲁工业大学 | Preparation method of basalt fiber paper |
| CN111778649A (en) * | 2020-06-18 | 2020-10-16 | 华陆工程科技有限责任公司 | Method for quickly preparing nano heat-insulating material through supercritical drying |
| CN111778649B (en) * | 2020-06-18 | 2024-04-26 | 中化学华陆新材料有限公司 | Method for rapidly preparing nano heat insulation material by supercritical drying |
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