CN109354026A - A kind of preparation method of the uniform mesoporous silicon foam material in aperture - Google Patents
A kind of preparation method of the uniform mesoporous silicon foam material in aperture Download PDFInfo
- Publication number
- CN109354026A CN109354026A CN201811078339.8A CN201811078339A CN109354026A CN 109354026 A CN109354026 A CN 109354026A CN 201811078339 A CN201811078339 A CN 201811078339A CN 109354026 A CN109354026 A CN 109354026A
- Authority
- CN
- China
- Prior art keywords
- reaction kettle
- foam material
- aperture
- reaction
- mesoporous silicon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
- C01B32/963—Preparation from compounds containing silicon
- C01B32/97—Preparation from SiO or SiO2
-
- 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
-
- 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
Abstract
The invention discloses a kind of preparation methods of the uniform mesoporous silicon foam material in aperture, belong to technical field of inorganic nonmetallic materials.First self-control block copolymer is prepared using (N- amidino groups) dodecylacrylamide and polyethylene glycol phosphate as raw material in the present invention, fatty acid, alcohol, ethyl orthosilicate and self-control block copolymer are sequentially added in dry reaction kettle again, after being uniformly mixed, carbon dioxide gas is passed through into reaction kettle, until reacting kettle inner pressure reaches 0.2~0.4MPa, by the closed pressure maintaining of reaction kettle；Reaction kettle heater and blender are opened, heating stirring reaction, to after reaction, stand cooling, after reacting kettle inner pressure is reduced to 0.15~0.17MPa, reaction kettle is opened in slow pressure release to normal pressure, is discharged, and it is dry, obtain dry base substrate；After the heat preservation charing of gained dry base substrate, continue temperature reaction, it is cooling, it discharges to get the uniform mesoporous silicon foam material in aperture.
Description
Technical field
The invention discloses a kind of preparation methods of the uniform mesoporous silicon foam material in aperture, belong to inorganic non-metallic material skill
Art field.
Background technique
Since the researcher of Mobil company in 1992 synthesize for the first time aperture between 2~10nm can modulation MCM-
After 41 meso-hole structure molecular sieves, mesopore molecular sieve is rapidly developed.These are with uniform adjustable mesoporous pore size, height
The mesoporous material of specific surface area and good thermal stability overcomes the limitation of micro-pore zeolite molecular sieve bore diameter undersize, in crowd
It is multi-field to receive the concern of researchers, but some common ordered mesoporous silicon material such as SBA-15, MCM-48 and HMS
Deng since its aperture is smaller and limited in the use of some fields.Mesoporous silicon foam (MCF) is to be found within 1999 a kind of novel
Mesoporous silica-base material is a kind of material in aperture maximum (up to 50nm) in mesoporous material synthesized at present, it possesses typical case
Foam-like three-dimensional cubic meso-hole structure, specific surface area is up to 1000cm2/ g, aperture and hole appearance are larger, wherein biggish spherical shape
Hole is connected with each other by lesser window aperture.Relative to the lesser MCM series in aperture and the mesoporous silica-base material of SBA series, MCF has
Big specific surface area, big and adjustable aperture, hole holds and special three-dimensional foam shape architectural characteristic, has it in various fields
Important theoretical significance and wide application prospect are such as more advantageous to the load for improving active metal as catalyst carrier
Amount is conducive to the mass transfer diffusion etc. of reactant, product.At present had reported literature applied alcohol esterification solidification, plus
Hydrogen dehydrogenation, CO2The fields such as absorption, the synthesis of hydrogen peroxide, and embody good performance.
There are many method, Antonietti etc. to be made using polystyrene polymeric microballoon for current synthesising mesoporous silicon foam material
Go out pore diameter range in the foam silicon materials of 20nm to 200nm for templated synthesis, but this material pore diameter range is too wide and too big,
Specific surface area is small, strongly limits its application range.Schmidt-Winkel etc. is closed using trimethylbenzene as emulsifier
At pore diameter range has been gone out in the mesoporous foam silicon materials of 22nm to 36nm, pore-size distribution is narrow.The silicon foam material of conventional synthesis at present
Blanking aperture distribution is too wide and aperture is excessive, and product specific surface area is small, limits the application range of product, therefore also needs to it
It is studied.
Summary of the invention
The present invention solves the technical problem of: it is too wide for the silicon foam material pore size distribution range of conventional synthesis and
The drawbacks of aperture is excessive, and product specific surface area is small, limits the application range of product provides a kind of uniform mesoporous silicon bubble in aperture
The preparation method of foam material.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
(1) (N- amidino groups) dodecylacrylamide is mixed with polyethylene glycol phosphate 5:1~10:1 in mass ratio, and be added
The paracide of 0.2~0.4 times of polyethylene glycol phosphate quality and two cyclopentadienyls of 0.02~0.08 times of polyethylene glycol phosphate quality
Iron, constant temperature are stirred to react, discharging, derived from block copolymer processed；
(2) according to parts by weight, 10~30 parts of self-control block copolymers, 20~30 parts of esters of silicon acis, 20~25 parts of fat are successively taken
Acid, 30~50 parts of alcohol first sequentially add fatty acid, alcohol, ethyl orthosilicate and self-control block copolymer in dry reaction kettle,
After being uniformly mixed, carbon dioxide gas is passed through into reaction kettle, until reacting kettle inner pressure reaches 0.2~0.4MPa, it will
The closed pressure maintaining of reaction kettle；
(3) reaction kettle heater and blender, heating stirring reaction, to after reaction, cooling be stood, in reaction kettle are opened
After pressure reduction to 0.15~0.17MPa, reaction kettle is opened in slow pressure release to normal pressure, is discharged, dry, obtains dry base substrate；
(4) by gained dry base substrate under inert gas shielding state, 500~600 DEG C, after heat preservation charing are heated to, after
Continuous to be warming up to 1480~1500 DEG C, after insulation reaction, cooling, discharging is to get the uniform mesoporous silicon foam material in aperture.
Step (2) esters of silicon acis is any one in methyl orthosilicate, ethyl orthosilicate or positive silicic acid propyl ester.
Step (2) fatty acid is any one in linolenic acid, linoleic acid, palmitinic acid or arachidonic acid.
Step (2) alcohol is methanol, ethyl alcohol, normal propyl alcohol, isopropanol, 1,2- propylene glycol, 1,3- propylene glycol or glycerine
In any one.
Step (3) the slow pressure release is to carry out pressure release with 100~150Pa/min rate.
Step (4) inert gas is any one in nitrogen, argon gas or helium.
The beneficial effects of the present invention are:
(1) technical solution of the present invention is to make block copolymer by oneself as the regulatable template of pattern, and is made with carbon dioxide gas
For the special agent of its Morphological control, in product preparation process, first to occur based on dehydrating condensation between fatty acid and alcohol,
The reaction can form corresponding aliphatic ester and water, and since the reaction is reversible reaction, reaction speed is controllable, makes whole system
Moisture generation can disperse in system uniform throughout, ensured and ethyl orthosilicate contact uniformity and adequacy, make positive silicon
Acetoacetic ester slowly occurs hydrolysis and generates silica, meanwhile, with the generation of moisture, due to making block copolymer structure by oneself
Middle polyethylene glycol segment is hydrophilic, and (N- amidino groups) dodecylacrylamide segment is hydrophobic, therefore can be self-assembly of in water
Imitated vesicle structure, in addition, carbon dioxide can interact with the amidine group in self-control block copolymer structure, to make
Amidine group has identical positive charge, due to the repulsive interaction of like charges, makes to make the vesica that block copolymer is formed by oneself
The volume of structure expands, and the volume of the vesica is determined by the quantity of charge, and the number of amount of charge can pass through two
The intake of carbon oxide gas reaches accurate control, makes to form the relatively narrow imitated vesicle structure of a large amount of volume distributions inside system,
Due to the consumption of carbon dioxide, reaction kettle internal pressure is also reduced；Furthermore it is a large amount of due to existing in polyethylene glycol segment
Hydroxyl, once in system teos hydrolysis product generation can be adsorbed by the segment, effectively prevent hydrolysate into
One step growth and reunion, to form the uniform spherical vesicles core-shell structure in aperture；
(2) present invention cooperates by using charing under inert gas shielding state and further pyroreaction, realizes to silicon foam
Reinforcing, firstly, organic matter kernel gradually forms carbonaceous skeleton in carbonization process, with the further raising of temperature, carbonaceous
Firm C-Si chemical bond can be formed between skeleton and outer shell silica, to effectively improve inner skeleton and external titanium dioxide
Bond strength between silicon, and the generation of C-Si chemical bond, the i.e. formation of silicon carbide, further improve the mechanics of foaming structure
Performance and stability, and the generation of the reaction, make script hole-closing structure be changed into through-hole structure, make internal specific surface area obtain into
The promotion of one step.
Specific embodiment
(N- amidino groups) dodecylacrylamide and polyethylene glycol phosphate are poured into three mouthfuls for 5:1~10:1 in mass ratio
In flask, and sequentially add into three-necked flask the paracide and polyethylene glycol of 0.2~0.4 times of polyethylene glycol phosphate quality
Three-necked flask is then moved to digital display and tested the speed constant temperature blender with magnetic force by the ferrocene that 0.02~0.08 times of phosphate quality, Yu Wen
Degree is 65~70 DEG C, under the conditions of speed of agitator is 600~800r/min, after constant temperature is stirred to react 2~5h, naturally cools to room
Temperature, discharging, derived from block copolymer processed；According to parts by weight, 10~30 parts of self-control block copolymers, 20~30 parts of silicon are successively taken
Acid esters, 20~25 parts of fatty acid, 30~50 parts of alcohol first successively add fatty acid, alcohol, ethyl orthosilicate and self-control block copolymer
Enter in dry reaction kettle, open reactor agitator, after being stirred 45~60min with 300~500r/min revolving speed, stops
Stirring, and carbon dioxide gas is passed through into reaction kettle with 300~500mL/min rate, until reacting kettle inner pressure reaches 0.2
~0.4MPa, then by the closed pressure maintaining of reaction kettle, later on reaction kettle heater and blender, be 80~85 DEG C in temperature, stir
Revolving speed is mixed after 3~5h of heating stirring reaction, to stop stirring, keeping the temperature 2~3h under the conditions of 400~600r/min, stopping is heated,
Make material in reactor temperature cooled to room temperature, to reacting kettle inner pressure because the further progress of internal-response voluntarily reduces
To 0.15~1.17MPa, fully open reaction kettle internal pressure to normal pressure, with the slow pressure release of 100~150Pa/min rate
Reaction kettle discharges, dry, obtains dry base substrate；Gained dry base substrate is moved into tube furnace, and with 200~400mL/min rate
It is passed through inert gas into furnace, under inert gas shielding state, is warming up to 500~600 DEG C with 3~5 DEG C/min rate program,
After 3~5h of heat preservation charing, continue to be warming up to 1480~1500 DEG C with 8~10 DEG C/min rate program, after 2~4h of insulation reaction,
Under inert gas shielding state, room temperature is cooled to the furnace, discharge to get the uniform mesoporous silicon foam material in aperture.The silicic acid
Ester is any one in methyl orthosilicate, ethyl orthosilicate or positive silicic acid propyl ester.The fatty acid be linolenic acid, linoleic acid,
Any one in palmitinic acid or arachidonic acid.The alcohol be methanol, ethyl alcohol, normal propyl alcohol, isopropanol, 1,2- propylene glycol, 1,
Any one in 3-propanediol or glycerine.The inert gas is any one in nitrogen, argon gas or helium.
(N- amidino groups) dodecylacrylamide and polyethylene glycol phosphate are poured into three-necked flask for 10:1 in mass ratio
In, and sequentially add into three-necked flask the paracide and polyethylene glycol phosphate matter of 0.4 times of polyethylene glycol phosphate quality
Three-necked flask is then moved to digital display and tested the speed constant temperature blender with magnetic force, is 70 DEG C in temperature, stirring turns by 0.08 times of ferrocene of amount
Under the conditions of speed is 800r/min, after constant temperature is stirred to react 5h, cooled to room temperature, discharging, derived from block copolymer processed；By weight
Measure number meter, successively take 30 parts of self-control block copolymers, 30 parts of esters of silicon acis, 25 parts of fatty acid, 50 parts of alcohol, first by fatty acid, alcohol,
Ethyl orthosilicate and self-control block copolymer sequentially add in dry reaction kettle, reactor agitator are opened, with 500r/min
After revolving speed is stirred 60min, stop stirring, and carbon dioxide gas is passed through into reaction kettle with 500mL/min rate, until
Reacting kettle inner pressure reaches 0.4MPa, then by the closed pressure maintaining of reaction kettle, later on reaction kettle heater and blender, in temperature
It is 85 DEG C, under the conditions of speed of agitator is 600r/min, after heating stirring reacts 5h, stops stirring, keep the temperature 3h, stop heating, make
Material in reactor temperature cooled to room temperature, to reacting kettle inner pressure because the further progress of internal-response is voluntarily reduced to
After 1.17MPa, make reaction kettle internal pressure with the slow pressure release of 150Pa/min rate to normal pressure, fully open reaction kettle, discharges,
It is dry, obtain dry base substrate；Gained dry base substrate is moved into tube furnace, and indifferent gas is passed through into furnace with 400mL/min rate
Body is warming up to 600 DEG C under inert gas shielding state with 5 DEG C/min rate program, after heat preservation charing 5h, continue with 10 DEG C/
Min rate program is warming up to 1500 DEG C, after insulation reaction 4h, under inert gas shielding state, cools to room temperature with the furnace, out
Material is to get the uniform mesoporous silicon foam material in aperture.The esters of silicon acis is methyl orthosilicate.The fatty acid is linolenic acid.It is described
Alcohol is methanol.The inert gas is nitrogen.
According to parts by weight, 30 parts of trimethylbenzenes are successively taken, 30 parts of esters of silicon acis, 25 parts of fatty acid, 50 parts of alcohol first will be fatty
Acid, alcohol, ethyl orthosilicate and trimethylbenzene sequentially add in dry reaction kettle, reactor agitator are opened, with 500r/min
After revolving speed is stirred 60min, stop stirring, and carbon dioxide gas is passed through into reaction kettle with 500mL/min rate, until
Reacting kettle inner pressure reaches 0.4MPa, then by the closed pressure maintaining of reaction kettle, later on reaction kettle heater and blender, in temperature
It is 85 DEG C, under the conditions of speed of agitator is 600r/min, after heating stirring reacts 5h, stops stirring, keep the temperature 3h, stop heating, make
Material in reactor temperature cooled to room temperature, to reacting kettle inner pressure because the further progress of internal-response is voluntarily reduced to
After 1.17MPa, make reaction kettle internal pressure with the slow pressure release of 150Pa/min rate to normal pressure, fully open reaction kettle, discharges,
It is dry, obtain dry base substrate；Gained dry base substrate is moved into tube furnace, and indifferent gas is passed through into furnace with 400mL/min rate
Body is warming up to 600 DEG C under inert gas shielding state with 5 DEG C/min rate program, after heat preservation charing 5h, continue with 10 DEG C/
Min rate program is warming up to 1500 DEG C, after insulation reaction 4h, under inert gas shielding state, cools to room temperature with the furnace, out
Material is to get the uniform mesoporous silicon foam material in aperture.The esters of silicon acis is methyl orthosilicate.The fatty acid is linolenic acid.It is described
Alcohol is methanol.The inert gas is nitrogen.
(N- amidino groups) dodecylacrylamide and polyethylene glycol phosphate are poured into three-necked flask for 10:1 in mass ratio
In, and sequentially add into three-necked flask the paracide and polyethylene glycol phosphate matter of 0.4 times of polyethylene glycol phosphate quality
Three-necked flask is then moved to digital display and tested the speed constant temperature blender with magnetic force, is 70 DEG C in temperature, stirring turns by 0.08 times of ferrocene of amount
Under the conditions of speed is 800r/min, after constant temperature is stirred to react 5h, cooled to room temperature, discharging, derived from block copolymer processed；By weight
Number meter is measured, successively takes 30 parts of self-control block copolymers, 30 parts of esters of silicon acis, 50 parts of alcohol first by alcohol, ethyl orthosilicate and are made by oneself embedding
Section copolymer sequentially adds in dry reaction kettle, opens reactor agitator, is stirred 60min with 500r/min revolving speed
Afterwards, stop stirring, and carbon dioxide gas is passed through into reaction kettle with 500mL/min rate, until reacting kettle inner pressure reaches
0.4MPa, then by the closed pressure maintaining of reaction kettle, later on reaction kettle heater and blender, in temperature be 85 DEG C, speed of agitator
Under the conditions of 600r/min, after heating stirring reacts 5h, stops stirring, keep the temperature 3h, stop heating, make material in reactor temperature
Cooled to room temperature makes to react after reacting kettle inner pressure is voluntarily reduced to 1.17MPa because of the further progress of internal-response
Kettle internal pressure fully opens reaction kettle with the slow pressure release of 150Pa/min rate to normal pressure, discharges, dry, obtains dry base substrate；
Gained dry base substrate is moved into tube furnace, and inert gas is passed through into furnace with 400mL/min rate, in inert gas shielding
Under state, 600 DEG C, after heat preservation carbonizes 5h are warming up to 5 DEG C/min rate program, continuation is warming up to 10 DEG C/min rate program
It 1500 DEG C, after insulation reaction 4h, under inert gas shielding state, cools to room temperature with the furnace, discharges uniform mesoporous to get aperture
Silicon foam material.The esters of silicon acis is methyl orthosilicate.The alcohol is methanol.The inert gas is nitrogen.
(N- amidino groups) dodecylacrylamide and polyethylene glycol phosphate are poured into three-necked flask for 10:1 in mass ratio
In, and sequentially add into three-necked flask the paracide and polyethylene glycol phosphate matter of 0.4 times of polyethylene glycol phosphate quality
Three-necked flask is then moved to digital display and tested the speed constant temperature blender with magnetic force, is 70 DEG C in temperature, stirring turns by 0.08 times of ferrocene of amount
Under the conditions of speed is 800r/min, after constant temperature is stirred to react 5h, cooled to room temperature, discharging, derived from block copolymer processed；By weight
Measure number meter, successively take 30 parts of self-control block copolymers, 30 parts of esters of silicon acis, 25 parts of fatty acid, 50 parts of alcohol, first by fatty acid, alcohol,
Ethyl orthosilicate and self-control block copolymer sequentially add in dry reaction kettle, reactor agitator are opened, with 500r/min
After revolving speed is stirred 60min, stop stirring, later on reaction kettle heater and blender, is 85 DEG C in temperature, stirring turns
Under the conditions of speed is 600r/min, after heating stirring reacts 5h, stops stirring, keep the temperature 3h, stop heating, make material in reactor temperature
Cooled to room temperature is spent, after reacting kettle inner pressure is voluntarily reduced to 1.17MPa because of the further progress of internal-response, is made anti-
It answers kettle internal pressure with the slow pressure release of 150Pa/min rate to normal pressure, fully opens reaction kettle, discharge, it is dry, obtain dry base
Body；Gained dry base substrate is moved into tube furnace, and inert gas is passed through into furnace with 400mL/min rate, in inert gas
Under guard mode, 600 DEG C, after heat preservation carbonizes 5h are warming up to 5 DEG C/min rate program, is continued with 10 DEG C/min rate program liter
Temperature is to 1500 DEG C, after insulation reaction 4h, under inert gas shielding state, cools to room temperature with the furnace, discharges uniform to get aperture
Mesoporous silicon foam material.The esters of silicon acis is methyl orthosilicate.The fatty acid is linolenic acid.The alcohol is methanol.It is described lazy
Property gas be nitrogen.
(N- amidino groups) dodecylacrylamide and polyethylene glycol phosphate are poured into three-necked flask for 10:1 in mass ratio
In, and sequentially add into three-necked flask the paracide and polyethylene glycol phosphate matter of 0.4 times of polyethylene glycol phosphate quality
Three-necked flask is then moved to digital display and tested the speed constant temperature blender with magnetic force, is 70 DEG C in temperature, stirring turns by 0.08 times of ferrocene of amount
Under the conditions of speed is 800r/min, after constant temperature is stirred to react 5h, cooled to room temperature, discharging, derived from block copolymer processed；By weight
Measure number meter, successively take 30 parts of self-control block copolymers, 30 parts of esters of silicon acis, 25 parts of fatty acid, 50 parts of alcohol, first by fatty acid, alcohol,
Ethyl orthosilicate and self-control block copolymer sequentially add in dry reaction kettle, reactor agitator are opened, with 500r/min
After revolving speed is stirred 60min, stop stirring, and carbon dioxide gas is passed through into reaction kettle with 500mL/min rate, until
Reacting kettle inner pressure reaches 0.4MPa, then by the closed pressure maintaining of reaction kettle, later on reaction kettle heater and blender, in temperature
It is 85 DEG C, under the conditions of speed of agitator is 600r/min, after heating stirring reacts 5h, stops stirring, keep the temperature 3h, stop heating, make
Material in reactor temperature cooled to room temperature, to reacting kettle inner pressure because the further progress of internal-response is voluntarily reduced to
After 1.17MPa, make reaction kettle internal pressure with the slow pressure release of 150Pa/min rate to normal pressure, fully open reaction kettle, discharges,
Drying is to get the uniform mesoporous silicon foam material in aperture.The esters of silicon acis is methyl orthosilicate.The fatty acid is linolenic acid.Institute
Stating alcohol is methanol.The inert gas is nitrogen.
Comparative example: the silicon foam material of Changzhou packaging material Co., Ltd production.
1 to 5 gained silicon foam material of example and comparative example product are subjected to performance detection, the specific detection method is as follows:
The pore structure parameter test of sample is tested using the Autosorb-1-C-TCD-MS of Kang Ta company.Specific surface area by
N2Adsorption isothermal curve combination BET equation acquires, and pore-size distribution is calculated by BJH model.
Specific testing result is as shown in table 1:
Table 1: performance detection table
| Detection content | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example |
| Aperture/nm | 9.4 | 15.4 | 14.5 | 12.1 | 13.5 | 20.6 |
| Specific surface area/cm2/g | 765.6 | 628.4 | 663.2 | 683.7 | 654.2 | 541.3 |
By 1 testing result of table it is found that the present invention gained uniform mesoporous silicon foam material in aperture has uniform aperture and excellent
Specific surface area.
Claims (6)
1. a kind of preparation method of the uniform mesoporous silicon foam material in aperture, it is characterised in that specific preparation step are as follows:
(1) (N- amidino groups) dodecylacrylamide is mixed with polyethylene glycol phosphate 5:1~10:1 in mass ratio, and be added
The paracide of 0.2~0.4 times of polyethylene glycol phosphate quality and two cyclopentadienyls of 0.02~0.08 times of polyethylene glycol phosphate quality
Iron, constant temperature are stirred to react, discharging, derived from block copolymer processed；
(2) according to parts by weight, 10~30 parts of self-control block copolymers, 20~30 parts of esters of silicon acis, 20~25 parts of fat are successively taken
Acid, 30~50 parts of alcohol first sequentially add fatty acid, alcohol, ethyl orthosilicate and self-control block copolymer in dry reaction kettle,
After being uniformly mixed, carbon dioxide gas is passed through into reaction kettle, until reacting kettle inner pressure reaches 0.2~0.4MPa, it will
The closed pressure maintaining of reaction kettle；
(3) reaction kettle heater and blender, heating stirring reaction, to after reaction, cooling be stood, in reaction kettle are opened
After pressure reduction to 0.15~0.17MPa, reaction kettle is opened in slow pressure release to normal pressure, is discharged, dry, obtains dry base substrate；
(4) by gained dry base substrate under inert gas shielding state, 500~600 DEG C, after heat preservation charing are heated to, after
Continuous to be warming up to 1480~1500 DEG C, after insulation reaction, cooling, discharging is to get the uniform mesoporous silicon foam material in aperture.
2. a kind of preparation method of the uniform mesoporous silicon foam material in aperture according to claim 1, it is characterised in that step
(2) esters of silicon acis is any one in methyl orthosilicate, ethyl orthosilicate or positive silicic acid propyl ester.
3. a kind of preparation method of the uniform mesoporous silicon foam material in aperture according to claim 1, it is characterised in that step
(2) fatty acid is any one in linolenic acid, linoleic acid, palmitinic acid or arachidonic acid.
4. a kind of preparation method of the uniform mesoporous silicon foam material in aperture according to claim 1, it is characterised in that step
(2) alcohol is any one in methanol, ethyl alcohol, normal propyl alcohol, isopropanol, 1,2- propylene glycol, 1,3- propylene glycol or glycerine.
5. a kind of preparation method of the uniform mesoporous silicon foam material in aperture according to claim 1, it is characterised in that step
(3) the slow pressure release is to carry out pressure release with 100~150Pa/min rate.
6. a kind of preparation method of the uniform mesoporous silicon foam material in aperture according to claim 1, it is characterised in that step
(4) inert gas is any one in nitrogen, argon gas or helium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811078339.8A CN109354026A (en) | 2018-09-17 | 2018-09-17 | A kind of preparation method of the uniform mesoporous silicon foam material in aperture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811078339.8A CN109354026A (en) | 2018-09-17 | 2018-09-17 | A kind of preparation method of the uniform mesoporous silicon foam material in aperture |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109354026A true CN109354026A (en) | 2019-02-19 |
Family
ID=65350815
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811078339.8A Withdrawn CN109354026A (en) | 2018-09-17 | 2018-09-17 | A kind of preparation method of the uniform mesoporous silicon foam material in aperture |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109354026A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113198468A (en) * | 2021-04-27 | 2021-08-03 | 中国科学院上海高等研究院 | Modified mesoporous material and preparation method and application thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5091271A (en) * | 1988-10-05 | 1992-02-25 | Teijin Limited | Shaped silion carbide-eased ceramic article |
| CN1730392A (en) * | 2005-06-16 | 2006-02-08 | 复旦大学 | Large aperture capacity silicon oxide vesicle, foamed material and process for preparing the same |
| CN101214965A (en) * | 2008-01-11 | 2008-07-09 | 北京化工大学 | Preparation method and application of macropore-mesoporous silicon dioxide hollow micro-sphere |
| CN103157450A (en) * | 2013-04-08 | 2013-06-19 | 南开大学 | Method for preparing efficient, environment-friendly and functional meso-porous silicon ball |
| CN103923614A (en) * | 2014-04-18 | 2014-07-16 | 北京科技大学 | Preparation method of orderly porous matrix shaping composite phase change material |
| CN104190444A (en) * | 2014-09-15 | 2014-12-10 | 安徽工业大学 | Preparation method of sulphated mesoporous SiO2 colloidal sphere catalyst for synthesizing biodiesel |
| CN107188181A (en) * | 2017-06-12 | 2017-09-22 | 凡闰司（苏州）环保科技有限公司 | A kind of low temperature synthesizes the method and silicon carbide products of high-specific-surface mesoporous carborundum |
| CN108219486A (en) * | 2017-12-29 | 2018-06-29 | 常州市鼎日环保科技有限公司 | A kind of high Humid Area asphalt anti-stripping agent of saliferous |
-
2018
- 2018-09-17 CN CN201811078339.8A patent/CN109354026A/en not_active Withdrawn
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5091271A (en) * | 1988-10-05 | 1992-02-25 | Teijin Limited | Shaped silion carbide-eased ceramic article |
| CN1730392A (en) * | 2005-06-16 | 2006-02-08 | 复旦大学 | Large aperture capacity silicon oxide vesicle, foamed material and process for preparing the same |
| CN101214965A (en) * | 2008-01-11 | 2008-07-09 | 北京化工大学 | Preparation method and application of macropore-mesoporous silicon dioxide hollow micro-sphere |
| CN103157450A (en) * | 2013-04-08 | 2013-06-19 | 南开大学 | Method for preparing efficient, environment-friendly and functional meso-porous silicon ball |
| CN103923614A (en) * | 2014-04-18 | 2014-07-16 | 北京科技大学 | Preparation method of orderly porous matrix shaping composite phase change material |
| CN104190444A (en) * | 2014-09-15 | 2014-12-10 | 安徽工业大学 | Preparation method of sulphated mesoporous SiO2 colloidal sphere catalyst for synthesizing biodiesel |
| CN107188181A (en) * | 2017-06-12 | 2017-09-22 | 凡闰司（苏州）环保科技有限公司 | A kind of low temperature synthesizes the method and silicon carbide products of high-specific-surface mesoporous carborundum |
| CN108219486A (en) * | 2017-12-29 | 2018-06-29 | 常州市鼎日环保科技有限公司 | A kind of high Humid Area asphalt anti-stripping agent of saliferous |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113198468A (en) * | 2021-04-27 | 2021-08-03 | 中国科学院上海高等研究院 | Modified mesoporous material and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Gai et al. | Uniform and size-tunable mesoporous silica with fibrous morphology for drug delivery | |
| CN102633464B (en) | Method for preparing SiO2 aerogel heat insulating composite through adhesive slip casting | |
| CN110483799B (en) | Controllable preparation method based on covalent organic framework and energy storage application thereof | |
| Su et al. | A controllable soft-templating approach to synthesize mesoporous carbon microspheres derived from d-xylose via hydrothermal method | |
| CN102418168A (en) | Porous-particle-doped polyimide hollow fibrous membrane, preparation method thereof, and application thereof | |
| CN106395837A (en) | Method for preparing silicon dioxide aerogel | |
| CN104860304A (en) | High specific surface area of silicon oxide hybridized graphene aerogel and production method thereof | |
| CN110203938A (en) | A kind of method and its application preparing multi-stage porous silicon dioxide ultrafine powder body for template based on glucan | |
| CN109179519A (en) | A kind of NiMnO3Porous nano ball material and its preparation method and application | |
| CN113292735B (en) | Simple preparation method of hollow ZIF-8 material | |
| CN110257019A (en) | A kind of phase change composite material and preparation method thereof with photo-thermal converting function | |
| CN109354026A (en) | A kind of preparation method of the uniform mesoporous silicon foam material in aperture | |
| CN107022102A (en) | Monodisperse mesoporous silica preparation method and nanocomposite foaming agent, preparation method and application | |
| CN108440767A (en) | It is a kind of that nanometer Au is combined to the new method for preparing Au@MOF composite materials with porous MOF | |
| CN106904604B (en) | A kind of carbon aerogels and preparation method thereof | |
| CN102020283A (en) | Preparation method of silicon dioxide nano hollow sphere with adjustable inner diameter | |
| CN108314089A (en) | A kind of porous flower-shaped α-Fe2O3The synthetic method of self-assembled nanometer material | |
| CN115608423A (en) | Gold nanocluster with silicon-based mesoporous molecular sieve inner packaging precise structure and preparation method thereof | |
| CN105540618B (en) | A kind of sodium bicarbonate and preparation method thereof and application of the sodium bicarbonate in expanded material | |
| Zhang et al. | Template-free synthesis of silica ellipsoids | |
| CN102303910B (en) | Method for preparing uniform-spherical trimanganese tetroxide | |
| CN108640661A (en) | A kind of preparation method of porous oxide ceramics | |
| CN105948117A (en) | Hydrothermal method for preparing HfO2 nano-particles | |
| CN112479223A (en) | Low-silicon nano sheet SAPO-34 molecular sieve and preparation method and application thereof | |
| CN1317233C (en) | Silica aerogel powder moulding method adopting gel injection molding method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20190219 |