CN108864780A - A kind of crack resistence inorganic sealing hole agent - Google Patents
A kind of crack resistence inorganic sealing hole agent Download PDFInfo
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- CN108864780A CN108864780A CN201810762566.6A CN201810762566A CN108864780A CN 108864780 A CN108864780 A CN 108864780A CN 201810762566 A CN201810762566 A CN 201810762566A CN 108864780 A CN108864780 A CN 108864780A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
- C09D1/02—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances alkali metal silicates
- C09D1/04—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances alkali metal silicates with organic additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
Abstract
The invention discloses a kind of crack resistence inorganic sealing hole agent, belong to material corrosion and protection technology field.According to parts by weight, it successively weighs：70~100 parts of waterglass, 15~20 parts of prodans, 10~18 parts of micas, 10~15 parts of modified graphene oxides, 10~15 parts of modified polyvinyl alcohol fabrics, 8~12 parts of modified carbon nano-tubes and 5~8 parts of additives, waterglass and prodan are mixed in blender, and mica is added into blender, modified graphene oxide, modified polyvinyl alcohol fabric, modified carbon nano-tube and additive are 40~50 DEG C in temperature, and revolving speed is under conditions of 300~400r/min, after being stirred 30~40min, crack resistence inorganic sealing hole agent is obtained.The crack resistence inorganic sealing hole agent of technical solution of the present invention preparation has the characteristics that excellent toughness, has broad prospects in development of the material corrosion with guard technology industry.
Description
Technical field
The invention discloses a kind of crack resistence inorganic sealing hole agent, belong to material corrosion and protection technology field.
Background technique
For many hot-spraying coatings, sealing of hole is a necessary last handling process.When coating faces corrosion and oxidation
（Sometimes in high temperature）When environment, sealing of hole is that coating designs the content necessarily considered.Any heat spraying method, especially
It is the coating that one oxygen flame of combustion gas spraying (i.e. flame-spraying) is deposited, and is all that one kind has pore structure.In general, coating porosity
It is quite big to spend range.One oxygen flame spray coating of combustion gas is sometime up to 15% or more, and one combustion gas of high speed oxygen sprays (HVOF) layer then 1%
Below.In practical applications, pore structure is advantageous sometimes.Coating porosity facilitates store oil, promotes lubrication, reduces abrasion；
In certain special applications, porous material is produced using thermal spraying, is used for heat-exchange device or other elements.However, more
In the case where, the hole of coating is undesirable.When coating is exposed to atmosphere, steam, industrial atmosphere, chemically reactive substance, corruption
It loses in gas and hot environment, hole introduces eroded elements, makes coating and matrix that chemistry or electrochemical etching occur, leads to coating
Failure, in such a case it is necessary to carry out sealing of hole to coating.
As a kind of postprocessing working procedures of thermal spraying, the selection of the to the effect that hole sealing agent of sealing of hole operation and construction party
Method.If also need turning or grinding after certain Workpiece paintings, sealing of hole should be implemented before this, pollute to prevent coating porosity,
Guarantee more preferable, cleaner grinding finish.In the case that spraying ceramic coat is for insulating, sealing of hole can maintain Jie of coating
Electric constant.Otherwise, coating porosity moisture absorption or will be polluted, and form undesirable conductive channel in coating.In addition, for pump or
The equipment such as hydraulic press, sealing of hole also prevent the sealing leak of liquid and pressure.
And traditional hole sealing agent in use can not cause there is also problem easy to crack is caused because toughness is bad
Reach ideal effect, therefore, how to improve the shortcomings that traditional hole sealing agent toughness can not further increase, is provided in the hope of exploring to develop
The hole sealing agent of good comprehensive performance is problem to be solved.
Summary of the invention
The present invention solves the technical problem of：For existing for traditional hole sealing agent because toughness is bad cause it is easy to crack
The shortcomings that, provide a kind of crack resistence inorganic sealing hole agent.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that：
A kind of crack resistence inorganic sealing hole agent, is made of the raw material of following parts by weight：70~100 parts of waterglass, 15~20 parts
Prodan, 10~18 parts of micas, the crack resistence inorganic sealing hole agent further include：10~15 parts of modified graphene oxides, 10~
15 parts of modified polyvinyl alcohol fabrics, 8~12 parts of modified carbon nano-tubes and 5~8 parts of additives；
The preparation method of the modified graphene oxide is：
By graphene oxide and petroleum ether in mass ratio 1：150~1：200 mix, and after ultrasonic disperse, graphene oxide matter is added
The wax dispersions of 5~10 times of amount, after being stirred to react, concentrated by rotary evaporation, vacuum drying obtains modified graphene oxide blank, will change
Property graphene oxide blank and nitric acid in mass ratio 1：8~1：12 mixing, filtering obtain modified graphene oxide；
The preparation method of the modified polyvinyl alcohol fabric is：
By poly-vinyl alcohol solution and graphene oxide solution by volume 5：1~8：1 mixing, after being stirred, electrostatic spinning is done
It is dry, obtain modified polyvinyl alcohol fabric；
The preparation method of the modified carbon nano-tube is：
By carbon nanotube and dehydrated alcohol in mass ratio 1：280~1：300 mix, and after ultrasonic disperse, adjust pH to 8~10, stir
After mixing reaction, pH is adjusted to neutrality, filters washing, vacuum drying obtains pre- modified carbon nano-tube；By pre- modified carbon nano-tube and second
Alcoholic solution in mass ratio 1：200~1：280 mix, and after ultrasonic disperse, the ammonium hydroxide of 5~8 times of pre- modified carbon nano-tube quality is added
With 10~30 times of ethyl orthosilicate mixture of pre- modified carbon nano-tube quality, after ultrasonic disperse, it is stirred to react, obtains carbon modified and receive
Nanotube mixture, by modified carbon nano-tube mixture and silane coupled agent composition in mass ratio 20：1~40：1 mixing, filters
It is dry, modified carbon nano tube blank is obtained, by modified carbon nano tube blank and hydrochloric acid in mass ratio 1：5~1：8 mixing, filtering obtain
Modified carbon nano-tube；
The preparation method of told additive is：
By gelatine microsphere and boric acid solution in mass ratio 1：6~1：10 mixing, and pH to 2.3~2.5 is adjusted, after being stirred,
PH to 4.8~5.8 is adjusted, filtering obtains additive.
The wax dispersions are by the paraffin of carbon atom number 24~32 and petroleum ether in mass ratio 1：10~1：12 mixing,
Obtain wax dispersions
The electrospinning conditions are to receive distance 10cm, spinning voltage to be covered with the receiving screen of aluminium-foil paper as reception device
12kV, spinning solution rate of extrusion 0.3mL/h.
The ethanol solution is by dehydrated alcohol and water by volume 4：1 mixing, obtains ethanol solution.
The ethyl orthosilicate mixture is by ethyl orthosilicate and ethyl alcohol in mass ratio 1：15~1：20 mixing, obtain positive silicic acid
Ethyl ester mixture.
The silane coupled agent composition is by ethyl alcohol and acetic acid in mass ratio 1：1 mixing, and be added ethyl alcohol quality 0.4~
0.6 times of silane coupling agent KH-560 after being stirred, obtains silane coupled agent composition.
The gelatine microsphere is according to parts by weight, successively to weigh：100~120 parts of polyvinyl alcohol, 60~80 parts of gelatin,
300~450 parts of water, 30~50 parts of glutaraldehyde water solutions and 10~30 parts of hydrochloric acid, polyvinyl alcohol are mixed with water, heating stirring,
Poly-vinyl alcohol solution is obtained, poly-vinyl alcohol solution is cooled down, and the poly-vinyl alcohol solution after cooling is mixed with gelatin, and is successively added
Enter hydrochloric acid and glutaraldehyde water solution, after being stirred, filtering, stripping and slicing is washed, and vacuum drying obtains gelatine microsphere.
The modulus of the waterglass is 2.6~2.8.
The beneficial effects of the invention are as follows：
（1）Modified carbon nano-tube is added when preparing crack resistence inorganic sealing hole agent in the present invention, firstly, carbon nanotube table after modification
Face grafted silica, after being added in product, silica can be scattered in a certain extent under the action of silane coupling agent
In product, to prevent the reunion of carbon nanotube, and then improve the toughness of product, secondly, the two of modified carbon nano tube pipe surface
Silica has amino, after mixing with acid solution, amino can be made with positive charge, to make modified carbon nano-tube that product be added
In after can be uniformly distributed in product under the action of electrostatic repulsion, and then further increase the toughness of product；
（2）Modified polyvinyl alcohol fabric and additive are added when preparing crack resistence inorganic sealing hole agent by the present invention, on the one hand, modified
It joined graphene oxide in vinal, Electrostatic Absorption and modified carbon nano-tube knot can be passed through in product use process
It closes, so that complicated three-dimensional network is formed in the product, so that the toughness of product is improved, on the other hand, the additive of addition
In contain the microballoon sensitive to pH, be added product in after, with sodium metasilicate solidification be crosslinked, improve the pH of product, thus
Make to produce the boric acid solution release in additive, and then crosslink modified polyvinyl alcohol fabric, makes the crosslinking degree in product
It improves, improves the toughness of product.
Specific embodiment
According to parts by weight, it successively weighs：100~120 parts of polyvinyl alcohol, 60~80 parts of gelatin, 300~450 parts of water, 30
The hydrochloric acid that the glutaraldehyde water solution and 10~30 parts of mass fractions that~50 parts of mass fractions are 22~28% are 32~38%, by poly- second
Enol is mixed with water, is 85~95 DEG C in temperature, after revolving speed stirs 45~80min under conditions of being 220~300r/min, is obtained poly-
Poly-vinyl alcohol solution is cooled to 50~70 DEG C, and the poly-vinyl alcohol solution after cooling is mixed with gelatin by glycohol solution, and
Hydrochloric acid that mass fraction is 32~38% is successively added into the mixture of poly-vinyl alcohol solution and gelatin and mass fraction be 22~
28% glutaraldehyde water solution is 28~38 DEG C in temperature, and revolving speed is stirred 10~12h under conditions of being 250~300r/min
Afterwards, it filters, obtains pretreatment gel, gel stripping and slicing will be pre-processed, and be washed with deionized 5~6 days, change one every 10~12h
Secondary deionized water obtains gelatine microsphere, by graphite oxide by the gel piece after washing after being dried in vacuo 3~5h under room temperature
Alkene and petroleum ether in mass ratio 1：150~1：200 are mixed in beaker, the ultrasonic disperse under conditions of frequency is 55~65kHz
After 30~40min, 5~10 times of graphene oxide quality of wax dispersions are added into beaker, is 65~70 DEG C in temperature, turns
Speed be 300~400r/min under conditions of be stirred to react 60~80min after, by material in beaker in temperature be 70~80 DEG C, turn
Speed is that 120~150r/min obtains concentrate, by concentrate under conditions of pressure is 500~600kPa after 2~3h of concentrated by rotary evaporation
Under conditions of 50~60 DEG C be dried in vacuo 2~3h after, obtain modified graphene oxide blank, by modified graphene oxide blank with
The nitric acid in mass ratio 1 that mass fraction is 20~30%：8~1：12 mixing, after standing 30~40min under room temperature, mistake
Filter, obtains modified graphene oxide；The oxidation for being 1~3% with mass fraction by the polyvinyl alcohol water solution that mass fraction is 5~7%
Graphene solution by volume 5：1~8：1 mixing is 45~55 DEG C in temperature, and revolving speed is 85 under conditions of 300~400r/min
~90 DEG C, after revolving speed is stirred 1~2h under conditions of being 300~400r/min, electrostatic spinning obtains pretreatment modification polyethylene
Alcohol fiber obtains modification after pretreatment modification vinal is dried in vacuo 10~12h under conditions of 50~55 DEG C of temperature
Vinal；By carbon nanotube and dehydrated alcohol in mass ratio 1：280~1：300 are mixed in flask, in frequency be 45
Under conditions of~55kHz after 30~40min of ultrasonic disperse, flask is adjusted with the potassium hydroxide solution that mass fraction is 15~20%
The pH to 8~10 of interior material, and be 85~90 DEG C in temperature, revolving speed is stirred to react 8~9h under conditions of being 300~400r/min
Afterwards, the pH of object in flask is adjusted with the hydrochloric acid that mass fraction is 10~18% to neutrality, is filtered washing, is obtained pre- modified carbon nano-tube
Blank obtains pre- carbon modified and receives after being dried in vacuo 4~5h under conditions of being 70~75 DEG C in temperature by pre- modified carbon nano tube blank
Mitron；By pre- modified carbon nano-tube and ethanol solution in mass ratio 1：200~1：280 are mixed in conical flask, in frequency be 45
Under conditions of~60kHz after 60~70min of ultrasonic disperse, and 5~8 times of pre- modified carbon nano-tube quality is added into conical flask
The ethyl orthosilicate mixture of 10~30 times of ammonium hydroxide and pre- modified carbon nano-tube quality that mass fraction is 25~28%, in frequency
It is 30~40 DEG C in temperature, revolving speed is 250~350r/min's after 50~60min of ultrasonic disperse under conditions of 45~60kHz
Under the conditions of be stirred to react 18~20h after, modified carbon nano-tube mixture is obtained, by modified carbon nano-tube mixture and silane coupling agent
Mixture in mass ratio 20：1~40：1 mixing is 30~40 DEG C in temperature, and revolving speed stirs under conditions of being 300~400r/min
After mixing 15~20min, drying is filtered, modified carbon nano tube blank is obtained, is 10 by modified carbon nano tube blank and mass fraction
~18% hydrochloric acid in mass ratio 1：5~1：8 mixing, after impregnating 30~40min under room temperature, filtering obtains modified carbon nano tube
Pipe；The boric acid solution in mass ratio 1 for being 20~30% by gelatine microsphere and mass fraction：6~1：10 mixing, and use mass fraction
The pH to 2.3~2.5 of gelatine microsphere and boric acid solution mixture is adjusted for 15~20% hydrochloric acid, is 40~50 DEG C in temperature, turns
After speed is stirred 1~2h under conditions of being 300~400r/min, it is micro- that gelatin is adjusted with the ammonium hydroxide that mass fraction is 12~18%
After the pH to 4.8~5.8 of ball and boric acid solution mixture, filtering obtains additive, according to parts by weight, successively weighs：70~
100 parts of waterglass, 15~20 parts of prodans, 10~18 parts of micas, 10~15 parts of modified graphene oxides, 10~15 parts of modifications
Waterglass and prodan are mixed in blender by vinal, 8~12 parts of modified carbon nano-tubes and 5~8 parts of additives
In, and mica is added into blender, modified graphene oxide, modified polyvinyl alcohol fabric, modified carbon nano-tube and additive,
It is 40~50 DEG C in temperature, under conditions of revolving speed is 300~400r/min, after being stirred 30~40min, it is inorganic obtains crack resistence
Hole sealing agent.The wax dispersions are by the paraffin of carbon atom number 24~32 and petroleum ether in mass ratio 1：10~1：12 mixing,
Obtaining electrospinning conditions described in wax dispersions is to receive distance 10cm to be covered with the receiving screen of aluminium-foil paper as reception device,
Spinning voltage 12kV, spinning solution rate of extrusion 0.3mL/h.The ethanol solution is by dehydrated alcohol and water by volume 4：1 is mixed
It closes, obtains ethanol solution.The ethyl orthosilicate mixture is by ethyl orthosilicate and ethyl alcohol in mass ratio 1：15~1：20 mixing, obtain
Ethyl orthosilicate mixture.The silane coupled agent composition is by ethyl alcohol and acetic acid in mass ratio 1：1 mixing, and ethyl alcohol is added
0.4~0.6 times of quality of silane coupling agent KH-560 after being stirred, obtains silane coupled agent composition.The mould of the waterglass
Number is 2.6~2.8.
Example 1
According to parts by weight, it successively weighs：120 parts of polyvinyl alcohol, 80 parts of gelatin, 450 parts of water, 50 parts of mass fractions are 28%
The hydrochloric acid that glutaraldehyde water solution and 30 parts of mass fractions are 38%, polyvinyl alcohol is mixed with water, is 95 DEG C in temperature, revolving speed is
After stirring 80min under conditions of 300r/min, poly-vinyl alcohol solution is obtained, poly-vinyl alcohol solution is cooled to 70 DEG C, and will cooling
Poly-vinyl alcohol solution afterwards is mixed with gelatin, and mass fraction is successively added into the mixture of poly-vinyl alcohol solution and gelatin and is
The glutaraldehyde water solution that 38% hydrochloric acid and mass fraction is 28% is 38 DEG C in temperature, and revolving speed stirs under conditions of being 300r/min
After mixing mixing 12h, filtering obtains pretreatment gel, will pre-process gel stripping and slicing, and be washed with deionized 6 days, changes every 12h
Deionized water obtains gelatine microsphere, by graphene oxide by the gel piece after washing after being dried in vacuo 5h under room temperature
With petroleum ether in mass ratio 1：200 are mixed in beaker, under conditions of frequency is 65kHz after ultrasonic disperse 40min, to beaker
The middle wax dispersions for being added 10 times of graphene oxide quality are 70 DEG C in temperature, and revolving speed stirs under conditions of being 400r/min
React 80min after, by material in beaker in temperature be 80 DEG C, revolving speed 150r/min, pressure be 600kPa under conditions of rotate
After 3h is concentrated, concentrate is obtained, after concentrate is dried in vacuo 3h under conditions of 60 DEG C, obtains modified graphene oxide blank, it will
The nitric acid in mass ratio 1 that modified graphene oxide blank and mass fraction are 30%：12 mixing, in standing 40min under room temperature
Afterwards, it filters, obtains modified graphene oxide；The oxidation stone for being 3% with mass fraction by the polyvinyl alcohol water solution that mass fraction is 7%
Black alkene solution by volume 8：1 mixing is 55 DEG C in temperature, and revolving speed is revolving speed 400r/ 90 DEG C under conditions of 400r/min
After being stirred 2h under conditions of min, electrostatic spinning obtains pretreatment modification vinal, by pretreatment modification polyethylene
After alcohol fiber is dried in vacuo 12h under conditions of 55 DEG C of temperature, modified polyvinyl alcohol fabric is obtained；By carbon nanotube and dehydrated alcohol
In mass ratio 1：300 are mixed in flask, under conditions of frequency is 55kHz after ultrasonic disperse 40min, are with mass fraction
20% potassium hydroxide solution adjusts the pH to 10 of material in flask, and is 90 DEG C in temperature, and revolving speed is under conditions of 400r/min
After being stirred to react 9h, the pH for adjusting object in flask with the hydrochloric acid that mass fraction is 18% filters washing, obtains pre- carbon modified to neutrality
Nanometer blank obtains pre- carbon modified and receives after being dried in vacuo 5h under conditions of being 75 DEG C in temperature by pre- modified carbon nano tube blank
Mitron；By pre- modified carbon nano-tube and ethanol solution in mass ratio 1：280 are mixed in conical flask, in the item that frequency is 60kHz
Under part after ultrasonic disperse 70min, and the ammonia that the mass fraction of 8 times of pre- modified carbon nano-tube quality is 28% is added into conical flask
The ethyl orthosilicate mixture of 30 times of water and pre- modified carbon nano-tube quality, the ultrasonic disperse under conditions of frequency is 60kHz
After 60min, it is 40 DEG C in temperature, after revolving speed is stirred to react 20h under conditions of being 350r/min, obtains modified carbon nano-tube mixing
Object, by modified carbon nano-tube mixture and silane coupled agent composition in mass ratio 40：1 mixing is 40 DEG C in temperature, and revolving speed is
After being stirred 20min under conditions of 400r/min, drying is filtered, modified carbon nano tube blank is obtained, by modified carbon nano tube pipe
The hydrochloric acid in mass ratio 1 that material is 18% with mass fraction：8 mixing, after impregnating 40min under room temperature, filtering obtains carbon modified
Nanotube；The boric acid solution in mass ratio 1 for being 30% by gelatine microsphere and mass fraction：10 mixing, and be 20% with mass fraction
Hydrochloric acid adjust gelatine microsphere and boric acid solution mixture pH to 2.5, in temperature be 50 DEG C, revolving speed for 400r/min condition
Under be stirred 2h after, after the pH to 5.8 that gelatine microsphere and boric acid solution mixture are adjusted with the ammonium hydroxide that mass fraction is 18%,
Filtering, obtains additive, according to parts by weight, successively weighs：100 parts of waterglass, 20 parts of prodans, 18 parts of micas, 15 parts change
Property graphene oxide, 15 parts of modified polyvinyl alcohol fabrics, 12 parts of modified carbon nano-tubes and 8 parts of additives, by waterglass and fluorine silicon
Sour sodium is mixed in blender, and mica is added into blender, modified graphene oxide, modified polyvinyl alcohol fabric, modified
Carbon nanotube and additive are 50 DEG C in temperature, under conditions of revolving speed is 400r/min, after being stirred 40min, obtain crack resistence
Inorganic sealing hole agent.The wax dispersions are by the paraffin of carbon atom number 32 and petroleum ether in mass ratio 1：12 mixing, obtain paraffin
Electrospinning conditions described in dispersion liquid are to receive distance 10cm, spinning electricity to be covered with the receiving screen of aluminium-foil paper as reception device
Press 12kV, spinning solution rate of extrusion 0.3mL/h.The ethanol solution is by dehydrated alcohol and water by volume 4：1 mixing, obtains second
Alcoholic solution.The ethyl orthosilicate mixture is by ethyl orthosilicate and ethyl alcohol in mass ratio 1：20 mixing, it is mixed to obtain ethyl orthosilicate
Close object.The silane coupled agent composition is by ethyl alcohol and acetic acid in mass ratio 1：1 mixing, and it is added 0.6 times of ethyl alcohol quality
Silane coupling agent KH-560 after being stirred, obtains silane coupled agent composition.The modulus of the waterglass is 2.8.
Example 2
According to parts by weight, it successively weighs：120 parts of polyvinyl alcohol, 80 parts of gelatin, 450 parts of water, 50 parts of mass fractions are 28%
The hydrochloric acid that glutaraldehyde water solution and 30 parts of mass fractions are 38%, polyvinyl alcohol is mixed with water, is 95 DEG C in temperature, revolving speed is
After stirring 80min under conditions of 300r/min, poly-vinyl alcohol solution is obtained, poly-vinyl alcohol solution is cooled to 70 DEG C, and will cooling
Poly-vinyl alcohol solution afterwards is mixed with gelatin, and mass fraction is successively added into the mixture of poly-vinyl alcohol solution and gelatin and is
The glutaraldehyde water solution that 38% hydrochloric acid and mass fraction is 28% is 38 DEG C in temperature, and revolving speed stirs under conditions of being 300r/min
After mixing mixing 12h, filtering obtains pretreatment gel, will pre-process gel stripping and slicing, and be washed with deionized 6 days, changes every 12h
Deionized water obtains gelatine microsphere, by graphene oxide by the gel piece after washing after being dried in vacuo 5h under room temperature
With petroleum ether in mass ratio 1：200 are mixed in beaker, under conditions of frequency is 65kHz after ultrasonic disperse 40min, in temperature
It is 70 DEG C, in temperature is 80 DEG C by material in beaker, revolving speed is after revolving speed is stirred to react 80min under conditions of being 400r/min
150r/min, pressure be 600kPa under conditions of after concentrated by rotary evaporation 3h, obtain concentrate, by concentrate under conditions of 60 DEG C vacuum
After dry 3h, modified graphene oxide blank is obtained, the nitric acid that modified graphene oxide blank and mass fraction are 30% is pressed into quality
Than 1：12 mixing, after standing 40min under room temperature, filtering obtains modified graphene oxide；The poly- second for being 7% by mass fraction
The graphene oxide solution that enol aqueous solution and mass fraction are 3% by volume 8：1 mixing is 55 DEG C in temperature, and revolving speed is
90 DEG C under conditions of 400r/min, after revolving speed is stirred 2h under conditions of being 400r/min, electrostatic spinning obtains pretreatment modification
Vinal after pretreatment modification vinal is dried in vacuo 12h under conditions of 55 DEG C of temperature, must be modified poly-
Alcohol fibers；By carbon nanotube and dehydrated alcohol in mass ratio 1：300 are mixed in flask, in the condition that frequency is 55kHz
After lower ultrasonic disperse 40min, the pH to 10 of material in flask is adjusted with the potassium hydroxide solution that mass fraction is 20%, and in temperature
Degree is 90 DEG C, after revolving speed is stirred to react 9h under conditions of being 400r/min, adjusts object in flask with the hydrochloric acid that mass fraction is 18%
PH to neutrality, filter washing, obtain pre- modified carbon nano tube blank, the item for being 75 DEG C in temperature by pre- modified carbon nano tube blank
After being dried in vacuo 5h under part, pre- modified carbon nano-tube is obtained；By pre- modified carbon nano-tube and ethanol solution in mass ratio 1：280 mixing
In conical flask, under conditions of frequency is 60kHz after ultrasonic disperse 70min, and pre- modified carbon nano tube is added into conical flask
The ethyl orthosilicate mixture of 30 times of ammonium hydroxide and pre- modified carbon nano-tube quality that the mass fraction that 8 times of pipe quality is 28%, Yu Pin
It is 40 DEG C in temperature, revolving speed is stirred to react under conditions of being 350r/min under conditions of rate is 60kHz after ultrasonic disperse 60min
After 20h, modified carbon nano-tube mixture is obtained, by modified carbon nano-tube mixture and silane coupled agent composition in mass ratio 40：1
Mixing is 40 DEG C in temperature, after revolving speed is stirred 20min under conditions of being 400r/min, filters drying, obtain modified carbon nano tube
Blank, the hydrochloric acid in mass ratio 1 for being 18% by modified carbon nano tube blank and mass fraction：8 mixing, in soaking under room temperature
After steeping 40min, filtering obtains modified carbon nano-tube；The boric acid solution in mass ratio 1 for being 30% by gelatine microsphere and mass fraction：10
Mixing, and with mass fraction be 20% hydrochloric acid adjust gelatine microsphere and boric acid solution mixture pH to 2.5, in temperature be 50
DEG C, after revolving speed is stirred 2h under conditions of being 400r/min, gelatine microsphere and boric acid are adjusted with the ammonium hydroxide that mass fraction is 18%
After the pH to 5.8 of solution mixture, filtering obtains additive, according to parts by weight, successively weighs：100 parts of waterglass, 20 parts of fluorine
Sodium metasilicate, 18 parts of micas, 15 parts of modified graphene oxides, 15 parts of modified polyvinyl alcohol fabrics, 12 parts of modified carbon nano-tubes and 8 parts
Waterglass and prodan are mixed in blender, and mica are added into blender by additive, modified graphene oxide,
Modified polyvinyl alcohol fabric, modified carbon nano-tube and additive are 50 DEG C in temperature, under conditions of revolving speed is 400r/min, stir
After mixing mixing 40min, crack resistence inorganic sealing hole agent is obtained.The ethanol solution is by dehydrated alcohol and water by volume 4：1 mixing,
Obtain ethanol solution.The ethyl orthosilicate mixture is by ethyl orthosilicate and ethyl alcohol in mass ratio 1：20 mixing, obtain positive silicic acid second
Ester admixture.The silane coupled agent composition is by ethyl alcohol and acetic acid in mass ratio 1：1 mixing, and ethyl alcohol quality 0.6 is added
Silane coupling agent KH-560 again, after being stirred, obtains silane coupled agent composition.The modulus of the waterglass is 2.8.
Example 3
According to parts by weight, it successively weighs：120 parts of polyvinyl alcohol, 80 parts of gelatin, 450 parts of water, 50 parts of mass fractions are 28%
The hydrochloric acid that glutaraldehyde water solution and 30 parts of mass fractions are 38%, polyvinyl alcohol is mixed with water, is 95 DEG C in temperature, revolving speed is
After stirring 80min under conditions of 300r/min, poly-vinyl alcohol solution is obtained, poly-vinyl alcohol solution is cooled to 70 DEG C, and will cooling
Poly-vinyl alcohol solution afterwards is mixed with gelatin, and mass fraction is successively added into the mixture of poly-vinyl alcohol solution and gelatin and is
The glutaraldehyde water solution that 38% hydrochloric acid and mass fraction is 28% is 38 DEG C in temperature, and revolving speed stirs under conditions of being 300r/min
After mixing mixing 12h, filtering obtains pretreatment gel, will pre-process gel stripping and slicing, and be washed with deionized 6 days, changes every 12h
Deionized water obtains gelatine microsphere, by graphene oxide by the gel piece after washing after being dried in vacuo 5h under room temperature
With petroleum ether in mass ratio 1：200 are mixed in beaker, under conditions of frequency is 65kHz after ultrasonic disperse 40min, to beaker
The middle wax dispersions for being added 10 times of graphene oxide quality are 70 DEG C in temperature, and revolving speed stirs under conditions of being 400r/min
React 80min after, by material in beaker in temperature be 80 DEG C, revolving speed 150r/min, pressure be 600kPa under conditions of rotate
After 3h is concentrated, concentrate is obtained, after concentrate is dried in vacuo 3h under conditions of 60 DEG C, obtains modified graphene oxide blank, it will
The nitric acid in mass ratio 1 that modified graphene oxide blank and mass fraction are 30%：12 mixing, in standing 40min under room temperature
Afterwards, it filters, obtains modified graphene oxide；The oxidation stone for being 3% with mass fraction by the polyvinyl alcohol water solution that mass fraction is 7%
Black alkene solution by volume 8：1 mixing is 55 DEG C in temperature, and revolving speed is revolving speed 400r/ 90 DEG C under conditions of 400r/min
After being stirred 2h under conditions of min, electrostatic spinning obtains pretreatment modification vinal, by pretreatment modification polyethylene
After alcohol fiber is dried in vacuo 12h under conditions of 55 DEG C of temperature, modified polyvinyl alcohol fabric is obtained；By carbon nanotube and dehydrated alcohol
In mass ratio 1：300 are mixed in flask, under conditions of frequency is 55kHz after ultrasonic disperse 40min, are with mass fraction
20% potassium hydroxide solution adjusts the pH to 10 of material in flask, and is 90 DEG C in temperature, and revolving speed is under conditions of 400r/min
After being stirred to react 9h, the pH for adjusting object in flask with the hydrochloric acid that mass fraction is 18% filters washing, obtains pre- carbon modified to neutrality
Nanometer blank obtains pre- carbon modified and receives after being dried in vacuo 5h under conditions of being 75 DEG C in temperature by pre- modified carbon nano tube blank
Mitron；By pre- modified carbon nano-tube in conical flask, under conditions of frequency is 60kHz after ultrasonic disperse 70min, and to taper
30 times of the ammonium hydroxide and pre- modified carbon nano-tube quality that the mass fraction of 8 times of pre- modified carbon nano-tube quality is 28% are added in bottle
Ethyl orthosilicate mixture is 40 DEG C in temperature, revolving speed is under conditions of frequency is 60kHz after ultrasonic disperse 60min
After being stirred to react 20h under conditions of 350r/min, modified carbon nano-tube mixture is obtained, by modified carbon nano-tube mixture and silane
It is coupled agent composition in mass ratio 40：1 mixing is 40 DEG C in temperature, and revolving speed is stirred 20min under conditions of being 400r/min
Afterwards, drying is filtered, modified carbon nano tube blank is obtained, the hydrochloric acid that modified carbon nano tube blank and mass fraction are 18% is pressed into quality
Than 1：8 mixing, after impregnating 40min under room temperature, filtering obtains modified carbon nano-tube；It is by gelatine microsphere and mass fraction
30% boric acid solution in mass ratio 1：10 mixing, and the hydrochloric acid for being 20% with mass fraction adjusts gelatine microsphere and boric acid solution is mixed
The pH to 2.5 for closing object is 50 DEG C in temperature, is 18% with mass fraction after revolving speed is stirred 2h under conditions of being 400r/min
Ammonium hydroxide adjust the pH to 5.8 of gelatine microsphere and boric acid solution mixture after, filtering obtains additive, according to parts by weight, successively
It weighs：100 parts of waterglass, 20 parts of prodans, 18 parts of micas, 15 parts of modified graphene oxides, 15 parts of modified polyvinylalcohol fibres
Waterglass and prodan are mixed in blender by dimension, 12 parts of modified carbon nano-tubes and 8 parts of additives, and into blender
Mica, modified graphene oxide, modified polyvinyl alcohol fabric, modified carbon nano-tube and additive is added, is 50 DEG C in temperature, turns
Under conditions of speed is 400r/min, after being stirred 40min, crack resistence inorganic sealing hole agent is obtained.The wax dispersions are by carbon
The paraffin and petroleum ether in mass ratio 1 of atomicity 32：12 mixing, obtaining electrospinning conditions described in wax dispersions is to be covered with
The receiving screen of aluminium-foil paper is reception device, receives distance 10cm, spinning voltage 12kV, spinning solution rate of extrusion 0.3mL/h.It is described
Ethyl orthosilicate mixture is by ethyl orthosilicate and ethyl alcohol in mass ratio 1：20 mixing, obtain ethyl orthosilicate mixture.The silicon
It is by ethyl alcohol and acetic acid in mass ratio 1 that alkane, which is coupled agent composition,：1 mixing, and 0.6 times of ethyl alcohol quality of silane coupling agent is added
KH-560 after being stirred, obtains silane coupled agent composition.The modulus of the waterglass is 2.8.
Example 4
According to parts by weight, it successively weighs：120 parts of polyvinyl alcohol, 80 parts of gelatin, 450 parts of water, 50 parts of mass fractions are 28%
The hydrochloric acid that glutaraldehyde water solution and 30 parts of mass fractions are 38%, polyvinyl alcohol is mixed with water, is 95 DEG C in temperature, revolving speed is
After stirring 80min under conditions of 300r/min, poly-vinyl alcohol solution is obtained, poly-vinyl alcohol solution is cooled to 70 DEG C, and will cooling
Poly-vinyl alcohol solution afterwards is mixed with gelatin, and mass fraction is successively added into the mixture of poly-vinyl alcohol solution and gelatin and is
The glutaraldehyde water solution that 38% hydrochloric acid and mass fraction is 28% is 38 DEG C in temperature, and revolving speed stirs under conditions of being 300r/min
After mixing mixing 12h, filtering obtains pretreatment gel, will pre-process gel stripping and slicing, and be washed with deionized 6 days, changes every 12h
Deionized water obtains gelatine microsphere, by graphene oxide by the gel piece after washing after being dried in vacuo 5h under room temperature
With petroleum ether in mass ratio 1：200 are mixed in beaker, under conditions of frequency is 65kHz after ultrasonic disperse 40min, to beaker
The middle wax dispersions for being added 10 times of graphene oxide quality are 70 DEG C in temperature, and revolving speed stirs under conditions of being 400r/min
React 80min after, by material in beaker in temperature be 80 DEG C, revolving speed 150r/min, pressure be 600kPa under conditions of rotate
After 3h is concentrated, concentrate is obtained, after concentrate is dried in vacuo 3h under conditions of 60 DEG C, obtains modified graphene oxide blank, it will
The nitric acid in mass ratio 1 that modified graphene oxide blank and mass fraction are 30%：12 mixing, in standing 40min under room temperature
Afterwards, it filters, obtains modified graphene oxide；The oxidation stone for being 3% with mass fraction by the polyvinyl alcohol water solution that mass fraction is 7%
Black alkene solution by volume 8：1 mixing is 55 DEG C in temperature, and revolving speed is revolving speed 400r/ 90 DEG C under conditions of 400r/min
After being stirred 2h under conditions of min, electrostatic spinning obtains pretreatment modification vinal, by pretreatment modification polyethylene
After alcohol fiber is dried in vacuo 12h under conditions of 55 DEG C of temperature, modified polyvinyl alcohol fabric is obtained；By carbon nanotube and dehydrated alcohol
In mass ratio 1：300 are mixed in flask, under conditions of frequency is 55kHz after ultrasonic disperse 40min, are with mass fraction
20% potassium hydroxide solution adjusts the pH to 10 of material in flask, and is 90 DEG C in temperature, and revolving speed is under conditions of 400r/min
After being stirred to react 9h, the pH for adjusting object in flask with the hydrochloric acid that mass fraction is 18% filters washing, obtains pre- carbon modified to neutrality
Nanometer blank obtains pre- carbon modified and receives after being dried in vacuo 5h under conditions of being 75 DEG C in temperature by pre- modified carbon nano tube blank
Mitron；By pre- modified carbon nano-tube and ethanol solution in mass ratio 1：280 are mixed in conical flask, in the item that frequency is 60kHz
Under part after ultrasonic disperse 70min, and the ammonia that the mass fraction of 8 times of pre- modified carbon nano-tube quality is 28% is added into conical flask
Water is 40 DEG C in temperature, revolving speed stirs under conditions of being 350r/min under conditions of frequency is 60kHz after ultrasonic disperse 60min
After mixing reaction 20h, modified carbon nano-tube mixture is obtained, modified carbon nano-tube mixture and silane coupled agent composition are pressed into quality
Than 40：1 mixing is 40 DEG C in temperature, after revolving speed is stirred 20min under conditions of being 400r/min, filters drying, obtain modification
Carbon nanotube blank, the hydrochloric acid in mass ratio 1 for being 18% by modified carbon nano tube blank and mass fraction：8 mixing, in room temperature item
After impregnating 40min under part, filtering obtains modified carbon nano-tube；The boric acid solution that gelatine microsphere and mass fraction are 30% is pressed into quality
Than 1：10 mixing, and the hydrochloric acid for being 20% with mass fraction adjusts the pH to 2.5, Yu Wen of gelatine microsphere and boric acid solution mixture
Degree is 50 DEG C, after revolving speed is stirred 2h under conditions of being 400r/min, adjusts gelatine microsphere with the ammonium hydroxide that mass fraction is 18%
After the pH to 5.8 of boric acid solution mixture, filtering obtains additive, according to parts by weight, successively weighs：100 parts of waterglass,
20 parts of prodans, 18 parts of micas, 15 parts of modified graphene oxides, 15 parts of modified polyvinyl alcohol fabrics, 12 parts of modified carbon nano tubes
Waterglass and prodan are mixed in blender, and mica are added into blender by pipe and 8 parts of additives, modified oxidized
Graphene, modified polyvinyl alcohol fabric, modified carbon nano-tube and additive are 50 DEG C in temperature, and revolving speed is the item of 400r/min
Under part, after being stirred 40min, crack resistence inorganic sealing hole agent is obtained.The wax dispersions be by the paraffin of carbon atom number 32 with
Petroleum ether in mass ratio 1：12 mixing, obtaining electrospinning conditions described in wax dispersions is to be with the receiving screen for being covered with aluminium-foil paper
Reception device receives distance 10cm, spinning voltage 12kV, spinning solution rate of extrusion 0.3mL/h.The ethanol solution is will be anhydrous
Ethyl alcohol and water by volume 4：1 mixing, obtains ethanol solution.The silane coupled agent composition be by ethyl alcohol and acetic acid in mass ratio
1：1 mixing, and 0.6 times of ethyl alcohol quality of silane coupling agent KH-560 is added, after being stirred, obtain silane coupled agent composition.
The modulus of the waterglass is 2.8.
Example 5
According to parts by weight, it successively weighs：120 parts of polyvinyl alcohol, 80 parts of gelatin, 450 parts of water, 50 parts of mass fractions are 28%
The hydrochloric acid that glutaraldehyde water solution and 30 parts of mass fractions are 38%, polyvinyl alcohol is mixed with water, is 95 DEG C in temperature, revolving speed is
After stirring 80min under conditions of 300r/min, poly-vinyl alcohol solution is obtained, poly-vinyl alcohol solution is cooled to 70 DEG C, and will cooling
Poly-vinyl alcohol solution afterwards is mixed with gelatin, and mass fraction is successively added into the mixture of poly-vinyl alcohol solution and gelatin and is
The glutaraldehyde water solution that 38% hydrochloric acid and mass fraction is 28% is 38 DEG C in temperature, and revolving speed stirs under conditions of being 300r/min
After mixing mixing 12h, filtering obtains pretreatment gel, will pre-process gel stripping and slicing, and be washed with deionized 6 days, changes every 12h
Deionized water obtains gelatine microsphere, by graphene oxide by the gel piece after washing after being dried in vacuo 5h under room temperature
With petroleum ether in mass ratio 1：200 are mixed in beaker, under conditions of frequency is 65kHz after ultrasonic disperse 40min, to beaker
The middle wax dispersions for being added 10 times of graphene oxide quality are 70 DEG C in temperature, and revolving speed stirs under conditions of being 400r/min
React 80min after, by material in beaker in temperature be 80 DEG C, revolving speed 150r/min, pressure be 600kPa under conditions of rotate
After 3h is concentrated, concentrate is obtained, after concentrate is dried in vacuo 3h under conditions of 60 DEG C, obtains modified graphene oxide blank, it will
The nitric acid in mass ratio 1 that modified graphene oxide blank and mass fraction are 30%：12 mixing, in standing 40min under room temperature
Afterwards, it filters, obtains modified graphene oxide；The oxidation stone for being 3% with mass fraction by the polyvinyl alcohol water solution that mass fraction is 7%
Black alkene solution by volume 8：1 mixing is 55 DEG C in temperature, and revolving speed is revolving speed 400r/ 90 DEG C under conditions of 400r/min
After being stirred 2h under conditions of min, electrostatic spinning obtains pretreatment modification vinal, by pretreatment modification polyethylene
After alcohol fiber is dried in vacuo 12h under conditions of 55 DEG C of temperature, modified polyvinyl alcohol fabric is obtained；By carbon nanotube and dehydrated alcohol
In mass ratio 1：300 are mixed in flask, under conditions of frequency is 55kHz after ultrasonic disperse 40min, are with mass fraction
20% potassium hydroxide solution adjusts the pH to 10 of material in flask, and is 90 DEG C in temperature, and revolving speed is under conditions of 400r/min
After being stirred to react 9h, the pH for adjusting object in flask with the hydrochloric acid that mass fraction is 18% filters washing, obtains pre- carbon modified to neutrality
Nanometer blank obtains pre- carbon modified and receives after being dried in vacuo 5h under conditions of being 75 DEG C in temperature by pre- modified carbon nano tube blank
Mitron；By pre- modified carbon nano-tube and ethanol solution in mass ratio 1：280 are mixed in conical flask, in the item that frequency is 60kHz
Under part after ultrasonic disperse 70min, and the ammonia that the mass fraction of 8 times of pre- modified carbon nano-tube quality is 28% is added into conical flask
The ethyl orthosilicate mixture of 30 times of water and pre- modified carbon nano-tube quality, the ultrasonic disperse under conditions of frequency is 60kHz
After 60min, it is 40 DEG C in temperature, after revolving speed is stirred to react 20h under conditions of being 350r/min, obtains modified carbon nano-tube mixing
Object, by modified carbon nano-tube mixture in temperature be 40 DEG C, revolving speed be 400r/min under conditions of be stirred 20min after, take out
It is filtered dry dry, obtains modified carbon nano tube blank, the hydrochloric acid in mass ratio 1 for being 18% by modified carbon nano tube blank and mass fraction：8
Mixing, after impregnating 40min under room temperature, filtering obtains modified carbon nano-tube；It is 30% by gelatine microsphere and mass fraction
Boric acid solution in mass ratio 1：10 mixing, and the hydrochloric acid for being 20% with mass fraction adjusts gelatine microsphere and boric acid solution mixture
PH to 2.5, in temperature be 50 DEG C, revolving speed be 400r/min under conditions of be stirred 2h after, with mass fraction be 18% ammonia
After water adjusts the pH to 5.8 of gelatine microsphere and boric acid solution mixture, filtering obtains additive, according to parts by weight, successively claims
It takes：100 parts of waterglass, 20 parts of prodans, 18 parts of micas, 15 parts of modified graphene oxides, 15 parts of modified polyvinyl alcohol fabrics,
Waterglass and prodan are mixed in blender, and are added into blender by 12 parts of modified carbon nano-tubes and 8 parts of additives
Mica, modified graphene oxide, modified polyvinyl alcohol fabric, modified carbon nano-tube and additive are 50 DEG C in temperature, and revolving speed is
Under conditions of 400r/min, after being stirred 40min, crack resistence inorganic sealing hole agent is obtained.The wax dispersions are by carbon atom
The paraffin and petroleum ether in mass ratio 1 of number 32：12 mixing, obtaining electrospinning conditions described in wax dispersions is to be covered with aluminium foil
The receiving screen of paper is reception device, receives distance 10cm, spinning voltage 12kV, spinning solution rate of extrusion 0.3mL/h.The ethyl alcohol
Solution is by dehydrated alcohol and water by volume 4：1 mixing, obtains ethanol solution.The ethyl orthosilicate mixture is by positive silicic acid second
Ester and ethyl alcohol in mass ratio 1：20 mixing, obtain ethyl orthosilicate mixture.The modulus of the waterglass is 2.8.
Comparative example：The crack resistence inorganic sealing hole agent of Shanghai tech materials production Co., Ltd production.
Example 1 to the resulting crack resistence inorganic sealing hole agent of example 5 and comparative example product are subjected to performance detection, it is specific to detect
Method is as follows：
After being coated with the sample solidification of test specimen, is handled 7 days as constant temperature in 200 DEG C of insulating boxs, it is inorganic to detect above-mentioned crack resistence
Hole sealing agent tensile strength and elasticity modulus；Whether there are cracks for observation after 180 days to be dried.
Specific testing result is as shown in table 1：
1 crack resistence inorganic sealing hole agent performance test results of table
| Detection project | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example |
| Tensile strength/MPa | 2.2 | 1.8 | 1.5 | 1.4 | 1.2 | 0.9 |
| Elasticity modulus/GPa | 30.1 | 35.4 | 29.7 | 34.6 | 29.3 | 34.1 |
| Cracking resistance | Flawless | There is crackle | There is crackle | There is crackle | There is crackle | There is crackle |
By 1 testing result of table it is found that the crack resistence inorganic sealing hole agent of technical solution of the present invention preparation has excellent toughness
The characteristics of, it has broad prospects in development of the material corrosion with guard technology industry.
Claims (8)
1. a kind of crack resistence inorganic sealing hole agent, is made of the raw material of following parts by weight：70~100 parts of waterglass, 15~20
Part prodan, 10~18 parts of micas, which is characterized in that the crack resistence inorganic sealing hole agent further includes：10~15 parts of modified oxygen
Graphite alkene, 10~15 parts of modified polyvinyl alcohol fabrics, 8~12 parts of modified carbon nano-tubes and 5~8 parts of additives；
The preparation method of the modified graphene oxide is：
By graphene oxide and petroleum ether in mass ratio 1：150~1：200 mix, and after ultrasonic disperse, graphene oxide matter is added
The wax dispersions of 5~10 times of amount, after being stirred to react, concentrated by rotary evaporation, vacuum drying obtains modified graphene oxide blank, will change
Property graphene oxide blank and nitric acid in mass ratio 1：8~1：12 mixing, filtering obtain modified graphene oxide；
The preparation method of the modified polyvinyl alcohol fabric is：
By poly-vinyl alcohol solution and graphene oxide solution by volume 5：1~8：1 mixing, after being stirred, electrostatic spinning is done
It is dry, obtain modified polyvinyl alcohol fabric；
The preparation method of the modified carbon nano-tube is：
By carbon nanotube and dehydrated alcohol in mass ratio 1：280~1：300 mix, and after ultrasonic disperse, adjust pH to 8~10, stir
After mixing reaction, pH is adjusted to neutrality, filters washing, vacuum drying obtains pre- modified carbon nano-tube；By pre- modified carbon nano-tube and second
Alcoholic solution in mass ratio 1：200~1：280 mix, and after ultrasonic disperse, the ammonium hydroxide of 5~8 times of pre- modified carbon nano-tube quality is added
With 10~30 times of ethyl orthosilicate mixture of pre- modified carbon nano-tube quality, after ultrasonic disperse, it is stirred to react, obtains carbon modified and receive
Nanotube mixture, by modified carbon nano-tube mixture and silane coupled agent composition in mass ratio 20：1~40：1 mixing, filters
It is dry, modified carbon nano tube blank is obtained, by modified carbon nano tube blank and hydrochloric acid in mass ratio 1：5~1：8 mixing, filtering obtain
Modified carbon nano-tube；
The preparation method of told additive is：
By gelatine microsphere and boric acid solution in mass ratio 1：6~1：10 mixing, and pH to 2.3~2.5 is adjusted, after being stirred,
PH to 4.8~5.8 is adjusted, filtering obtains additive.
2. a kind of crack resistence inorganic sealing hole agent according to claim 1, it is characterised in that：The wax dispersions are by carbon
The paraffin and petroleum ether in mass ratio 1 of atomicity 24~32：10~1：12 mixing, obtain wax dispersions
3. a kind of crack resistence inorganic sealing hole agent according to claim 1, it is characterised in that：The electrospinning conditions be with
The receiving screen for being covered with aluminium-foil paper is reception device, receives distance 10cm, spinning voltage 12kV, spinning solution rate of extrusion 0.3mL/
h。
4. a kind of crack resistence inorganic sealing hole agent according to claim 1, it is characterised in that：The ethanol solution is will be anhydrous
Ethyl alcohol and water by volume 4：1 mixing, obtains ethanol solution.
5. a kind of crack resistence inorganic sealing hole agent according to claim 1, it is characterised in that：The ethyl orthosilicate mixture
By ethyl orthosilicate and ethyl alcohol in mass ratio 1：15~1：20 mixing, obtain ethyl orthosilicate mixture.
6. a kind of crack resistence inorganic sealing hole agent according to claim 1, it is characterised in that：The silane coupled agent composition
For by ethyl alcohol and acetic acid in mass ratio 1：1 mixing, and 0.4~0.6 times of ethyl alcohol quality of silane coupling agent KH-560, stirring is added
After mixing, silane coupled agent composition is obtained.
7. a kind of crack resistence inorganic sealing hole agent according to claim 1, it is characterised in that：The gelatine microsphere is by weight
Number meter, successively weighs：100~120 parts of polyvinyl alcohol, 60~80 parts of gelatin, 300~450 parts of water, 30~50 parts of glutaraldehyde water
Solution and 10~30 parts of hydrochloric acid, polyvinyl alcohol is mixed with water, and heating stirring obtains poly-vinyl alcohol solution, by poly-vinyl alcohol solution
Cooling, and the poly-vinyl alcohol solution after cooling is mixed with gelatin, and sequentially add hydrochloric acid and glutaraldehyde water solution, it is stirred
Afterwards, it filters, stripping and slicing, washs, vacuum drying obtains gelatine microsphere.
8. a kind of crack resistence inorganic sealing hole agent according to claim 1, it is characterised in that：The modulus of the waterglass is
2.6~2.8.
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| CN115851015A (en) * | 2022-12-28 | 2023-03-28 | 常州瑞赛激光技术有限公司 | Hole sealing agent for reducing pores of thermal spraying coating of ceramic anilox roller and preparation method |
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| CN1544559A (en) * | 2003-11-26 | 2004-11-10 | 公安部上海消防研究所 | Fireproof coating composition and application thereof |
| CN102786644A (en) * | 2012-08-21 | 2012-11-21 | 陕西科技大学 | Preparation method of acrylic resin finishing agent modified by nano silicon dioxide (SiO2)-coated multi-walled carbon nanotubes |
| CN103172344A (en) * | 2013-04-09 | 2013-06-26 | 江西恒大高新技术股份有限公司 | Heat-resisting compact inorganic hole sealing agent coating |
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| CN1544559A (en) * | 2003-11-26 | 2004-11-10 | 公安部上海消防研究所 | Fireproof coating composition and application thereof |
| CN102786644A (en) * | 2012-08-21 | 2012-11-21 | 陕西科技大学 | Preparation method of acrylic resin finishing agent modified by nano silicon dioxide (SiO2)-coated multi-walled carbon nanotubes |
| CN103172344A (en) * | 2013-04-09 | 2013-06-26 | 江西恒大高新技术股份有限公司 | Heat-resisting compact inorganic hole sealing agent coating |
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| CN115851015A (en) * | 2022-12-28 | 2023-03-28 | 常州瑞赛激光技术有限公司 | Hole sealing agent for reducing pores of thermal spraying coating of ceramic anilox roller and preparation method |
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