CN107245159A - A kind of Preparation method and use of silica constructing super-drainage melamine sponge - Google Patents
A kind of Preparation method and use of silica constructing super-drainage melamine sponge Download PDFInfo
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- CN107245159A CN107245159A CN201710363886.XA CN201710363886A CN107245159A CN 107245159 A CN107245159 A CN 107245159A CN 201710363886 A CN201710363886 A CN 201710363886A CN 107245159 A CN107245159 A CN 107245159A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/40—Impregnation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08L61/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08L61/28—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08J2361/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08J2361/28—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
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- Organic Chemistry (AREA)
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- Polymers & Plastics (AREA)
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- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention provides a kind of Preparation method and use of silica constructing super-drainage melamine sponge, step is as follows:Step 1, the cleaning of melamine sponge:Melamine sponge is dipped in hydrochloric acid and cleaned, and is washed with water to neutrality, is dried;Step 2, preparation VTES aqueous dispersions:VTES is added in deionized water, is sufficiently stirred for obtaining VTES aqueous dispersions;Step 3, prepare silica constructing super-drainage melamine sponge:Melamine sponge in step 1 is dipped in the VTES aqueous dispersions in step 2, is added dropwise after ammoniacal liquor, drying obtains silica constructing super-drainage melamine sponge.Base material of the invention used is melamine sponge, abundance, cheap.
Description
Technical field
The present invention relates to a kind of preparation method and its usage of silica constructing super-drainage melamine sponge, belong to environment
Functional material preparing technical field.
Background technology
Oil is one of most important energy in the world, but during the exploitation, transport and storage in oil often
Occurs the incident of leakage of oil, the leakage of oil can bring huge economic impact to fishery, marine aquaculture and tourist industry.Mesh
The preceding administering method on Oil spills mainly has:Situ combustion method, fence intercept method, biological degradation method, adsorption method of separation etc..
Wherein, it is one of most economical, effective method to handle oil spilling with oil absorption material, therefore enjoys the extensive concern of scientific research personnel.Mesh
The new material of the preceding field of scientific study on " separation of water oil " is gradually developed.This kind of material is general coarse by structured surface
Structure and surface katakinetomere are modified to reach the super-hydrophobic/super-oleophilic performance of material.However, material prepare Cost Problems with
Complex procedures problem is the difficult point of urgent need to resolve.
Melamine (melamine) aerated plastics is a kind of low-density, high opens sky rate, flexible foamed plastics.Because possessing brilliance
Anti-flammability, sound absorption properties and thermal insulation, be widely used in having improvement tonequality, control noise, the construction industry of heat-insulation and heat-preservation demand, work
The fields such as industry, the vehicles, space flight and aviation, electromechanics, household electrical appliances, electronic product, garment fabric, daily cleaning product.Contact after naked light
The coke layer of densification is formed on the surface of burner body so as to block burning, no drip, non-toxic gas release, smoke density is small, from
Fiery self-extinguishment.Superpower acoustical absorptivity:It is up to more than 95% percent opening and enables the deep layers of the entrance foams of sound wave easily and effectively
And be changed into the shock energy of grid and be consumed and sponge, and effectively eliminate back wave.Well insulated heat insulating ability:Its percent opening
Up to more than 95%, three dimensional network structure makes the convection heat transfer' heat-transfer by convection of air effectively be blocked.Temperature tolerance is strong:Suitable long-term work
Under the conditions of -165 DEG C to 180 DEG C, and without decomposition and metaboly.Non-toxic sanitary security:Its stable chemical constitution and friendship
Conjuncted system makes it have the chemical stability of uniqueness, fully meets country on interior decoration, commodity and vehicles noise reduction
Deng field.Ultralight porous, being used repeatedly property based on melamine sponge and it is cheap the advantages of, can conduct
The base material of water-oil separating material is used, and coarse constructing is carried out on its surface and reaches ultra-hydrophobicity with the modification of surface low energy, and
Applied to water-oil separating engineering.
The present invention makes full use of resource, using low density porous melamine sponge as base material, is dredged on its surface
Water silica is constructed, and the material shows excellent ultra-hydrophobicity, and show in water surface quick adsorption greasy dirt,
It is a kind of sorbing material for being used to have good prospect in terms of water-oil separating.
The content of the invention
It is an object of the invention to provide a kind of preparation method of silica constructing super-drainage melamine sponge, first will
Melamine sponge carries out pickling;Secondly, VTES (VTES) aqueous dispersions are prepared;Finally, dioxy is prepared
SiClx constructing super-drainage melamine sponge;And by a variety of characterization methods, disclose the pattern and performance of composite, utilize
Adsorb removal capacity of the composite to greasy dirt in water body obtained by oils experimental study.
The technical solution adopted by the present invention is:
A kind of preparation method of silica constructing super-drainage melamine sponge, is carried out as steps described below:
Step 1, the cleaning of melamine sponge:Melamine sponge is dipped in hydrochloric acid and cleaned, and be washed with water to
After neutrality, drying;
Step 2, preparation VTES aqueous dispersions:VTES is added to deionization
In water, it is sufficiently stirred for obtaining VTES aqueous dispersions;
Step 3, prepare silica constructing super-drainage melamine sponge:Melamine sponge in step 1 is dipped in
In VTES aqueous dispersions in step 2, it is added dropwise after ammoniacal liquor, drying obtains silica constructing super-drainage
Melamine sponge.
In step 1, used concentration of hydrochloric acid solution is 0~1mol L-1, soaking temperature is 10~50 DEG C, soak time
For 0.5~5h.
In step 1, described washing is to use deionized water or distilled water or hot water wash.
In step 1,5~8h is dried at used 40~60 DEG C.
In step 2, the volume ratio of used VTES and deionized water is 1~10:100.
In step 3, the volume ratio of used ammoniacal liquor and VTES is 1~3:10, the ammoniacal liquor
Concentration is 5~15mol L-1。
In step 3, the drying temperature is 25~45 DEG C, and keeps 1~4h.
The greasy dirt that prepared silica constructing super-drainage melamine sponge is used in adsorbed water body, on the water surface
Diesel oil.
Beneficial effect:
(1) present invention base material used is melamine sponge, abundance, cheap.
(2) silica constructing super-drainage melamine sponge made from has high porosity, extremely-low density, height absorption
Amount, quick adsorption, the performance such as chemical stability is strong, regeneration reusing is good.
(3), can be oily in adsorbed water body in view of the excellent performance of the silica constructing super-drainage melamine sponge
Dirty field is widely used.
(4) preparation method of the invention is simple and easy to apply, flow is shorter, easy controlled operation, suitable for industrialized production, uses.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of base material melamine sponge in embodiment 1;
Fig. 2 is the scanning electron microscope (SEM) photograph of the silica constructing super-drainage melamine sponge prepared in embodiment 1;
Fig. 3 is the contact angle figure of silica constructing super-drainage melamine sponge and pictorial diagram prepared in embodiment 1.
Embodiment
The invention will be further described below in conjunction with the accompanying drawings:
Embodiment 1:
Melamine sponge is dipped in 0.5mol L-1Keep 1h to be cleaned at 10 DEG C in aqueous hydrochloric acid solution, and spend
After ionized water or distilled water or hot wash to neutrality, 5h is dried at 60 DEG C;Then, VTES aqueous dispersions are prepared:By VTES with
The volume ratio of water is 5:100 mixing, and under magnetic stirring apparatus strong stirring to uniform dispersion liquid;Finally, will be clear in step 1
Melamine sponge after washing is dipped in the dispersion liquid in step 2, and ammoniacal liquor (5~15mol L are added dropwise-1, it is 2 with VTES volume ratios:
10) VTES hydrolysis, is carried out at 35 DEG C, and keeps 2h, 80 DEG C of drying are warming up to afterwards, you can obtain silica constructing super-drainage
Melamine sponge.
Fig. 1 is the scanning electron microscope (SEM) photograph of unpickled melamine sponge, it can be clearly seen that melamine sponge surface has
Substantial amounts of impurity, it may be possible to the remnants of foaming agent in melamine sponge preparation process, therefore surface acid-washing, with necessity
Property;
Fig. 2 is the scanning electron microscope (SEM) photograph of silica constructing super-drainage melamine sponge, clearly it can be seen that having a large amount of
Silicon ball be completely coated with melamine sponge surface, in preparation process, not only constructed coarse surface texture, simultaneously
The surface katakinetomere of the vinyl silicon ball of formation;
Fig. 3 is the contact angle figure and pictorial diagram of silica constructing super-drainage melamine sponge, is connect by water droplet static state
Feeler figure, it can be seen that the composite has reached excellent ultra-hydrophobicity, and pictorial diagram indicates melamine sea
Silk floss is from water wetted material to the transformation of super hydrophobic material.
Embodiment 2:
Melamine sponge is dipped in 0mol L-1In aqueous hydrochloric acid solution at 50 DEG C keep 5h cleaned, and spend from
After sub- water or distilled water or hot wash to neutrality, 8h is dried at 40 DEG C;Then, VTES aqueous dispersions are prepared:By VTES and water
Volume ratio be 1:100 mixing, and under magnetic stirring apparatus strong stirring to uniform dispersion liquid;Finally, it will be cleaned in step 1
Melamine sponge afterwards is dipped in the dispersion liquid in step 2, and ammoniacal liquor (5~15mol L are added dropwise-1, it is 1 with VTES volume ratios:10),
VTES hydrolysis is carried out at 25 DEG C, and keeps 4h, 80 DEG C of drying are warming up to afterwards, you can obtain silica constructing super-drainage trimerization
Cyanamide sponge.
Embodiment 3:
Melamine sponge is dipped in 1mol L-1Keep 0.5h to be cleaned at 10 DEG C in aqueous hydrochloric acid solution, and spend
After ionized water or distilled water or hot wash to neutrality, 5h is dried at 60 DEG C;Then, VTES aqueous dispersions are prepared:By VTES with
The volume ratio of water is 10:100 mixing, and under magnetic stirring apparatus strong stirring to uniform dispersion liquid;Finally, by step 1
Melamine sponge after cleaning is dipped in the dispersion liquid in step 2, and ammoniacal liquor (5~15mol L are added dropwise-1, it is 3 with VTES volume ratios:
10) VTES hydrolysis, is carried out at 45 DEG C, and keeps 1h, you can silica constructing super-drainage melamine sponge is obtained.
2nd, with reference to specific implementation example, the present invention will be further described:
Adsorbed water body greasy dirt performance evaluation is carried out by the following method in specific embodiment in the present invention:In deionized water
Middle a certain amount of oil of addition, such as light oil (diesel oil), heavy oil (dichloroethanes), with the silica constructing super-drainage three of certain mass
Poly cyanamid sponge carries out greasy dirt adsorption experiment.Its oil absorption QeIt is calculated as follows:
Wherein MoAnd M (g)e(g) it is respectively silica constructing super-drainage melamine sponge initial mass and adsorption saturation
Gross mass.
Experimental example 1:First, 50mL deionized water is gone in beaker, and addition takes 50mL diesel oil thereto, by 0.1g
Silica constructing super-drainage melamine sponge be placed in equipped with oil water mixture, after saturation to be adsorbed, take out, and claim it
Quality, oil absorption is can obtain by calculating.As a result show:Silica constructing super-drainage melamine sponge is to water surface
Light oil there is good absorption property.
Experimental example 2:First, 50mL deionized water is gone in beaker, and addition takes 50mL dichloroethanes thereto, will
0.1g silica constructing super-drainage melamine sponge is placed in equipped with oil water mixture, and tweezer is needed to use in adsorption process
Sponge is in contact by son with dichloroethanes, is easy to after absorption, saturation to be adsorbed, takes out, and claims its quality, can be obtained by calculating
To oil absorption.As a result show:Silica constructing super-drainage melamine sponge has good absorption to the heavy oil under water body
Performance.
Experimental example 3:First, 50mL deionized water is gone in beaker, and addition takes 50mL dichloroethanes thereto, will
0.1g silica constructing super-drainage melamine sponge is placed in equipped with oil water mixture, and tweezer is needed to use in adsorption process
Sponge is in contact by son with dichloroethanes, is easy to after absorption, saturation to be adsorbed, takes out, and claims its quality, can be obtained by calculating
To oil absorption.After the dichloroethanes for extruding the absorption of silica constructing super-drainage melamine sponge, drying is weighed.Repeat with
Upper process 10 times, and show excellent recycling performance.
Claims (8)
1. a kind of preparation method of silica constructing super-drainage melamine sponge, it is characterised in that enter as steps described below
OK:
Step 1, the cleaning of melamine sponge:Melamine sponge is dipped in hydrochloric acid and cleaned, and is washed with water to neutrality
Afterwards, dry;
Step 2, preparation VTES aqueous dispersions:VTES is added to deionized water
In, it is sufficiently stirred for obtaining VTES aqueous dispersions;
Step 3, prepare silica constructing super-drainage melamine sponge:Melamine sponge in step 1 is dipped in step 2
In VTES aqueous dispersions in, be added dropwise ammoniacal liquor after, drying, obtain silica constructing super-drainage melamine
Amine sponge.
2. a kind of preparation method of silica constructing super-drainage melamine sponge according to claim 1, its feature
It is, in step 1, used concentration of hydrochloric acid solution is 0~1mol L-1, soaking temperature is 10~50 DEG C, and soak time is
0.5~5h.
3. a kind of preparation method of silica constructing super-drainage melamine sponge according to claim 1, its feature
It is, in step 1, described washing is to use deionized water or distilled water or hot water wash.
4. a kind of preparation method of silica constructing super-drainage melamine sponge according to claim 1, its feature
It is, in step 1,5~8h is dried at used 40~60 DEG C.
5. a kind of preparation method of silica constructing super-drainage melamine sponge according to claim 1, its feature
It is, in step 2, the volume ratio of used VTES and deionized water is 1~10:100.
6. a kind of preparation method of silica constructing super-drainage melamine sponge according to claim 1, its feature
It is, in step 3, the volume ratio of used ammoniacal liquor and VTES is 1~3:10, the concentration of the ammoniacal liquor
For 5~15mol L-1。
7. a kind of preparation method of silica constructing super-drainage melamine sponge according to claim 1, its feature
It is, in step 3, the drying temperature is 25~45 DEG C, and keeps 1~4h.
8. silica constructing super-drainage melamine sponge prepared by the method described in claim 1~7 any one is used for
The purposes of greasy dirt in adsorbed water body.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107987311A (en) * | 2017-12-27 | 2018-05-04 | 淮阴工学院 | A kind of preparation method of hydrophobicity melamine sponge enhancing polysilsesquioxane composite aerogel |
CN108465460A (en) * | 2018-05-17 | 2018-08-31 | 江苏大学 | A kind of preparation method of super-hydrophobic sponge sorbing material |
CN109364888A (en) * | 2018-10-04 | 2019-02-22 | 南京航空航天大学溧水仿生产业研究院有限公司 | The preparation method of bionic super-hydrophobic absorption sponge |
CN110773137A (en) * | 2019-10-22 | 2020-02-11 | 同济大学 | Silicon dioxide nanorod-melamine foam compound and preparation method thereof |
CN116425553A (en) * | 2023-02-10 | 2023-07-14 | 浙江理工大学 | Preparation method for preparing heat-insulating boron nitride foam by in-situ vapor deposition |
CN116514556A (en) * | 2023-02-10 | 2023-08-01 | 浙江理工大学 | Preparation method of lightweight heat-insulating boron nitride foam |
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CN104771936A (en) * | 2015-03-19 | 2015-07-15 | 南京工业大学 | Preparation method of high oil absorption sponge for oil-water separation |
CN105542221A (en) * | 2015-12-18 | 2016-05-04 | 河南大学 | Wear-resistant super-hydrophobic super-lipophilic polyurethane sponge and preparation method and application thereof in oil-water continuous separation |
CN105801903A (en) * | 2016-03-17 | 2016-07-27 | 中国船舶重工集团公司第七二五研究所 | Preparation method and corrosion-preventing implementation method of super-hydrophobic sponge material |
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CN104324524A (en) * | 2014-11-21 | 2015-02-04 | 中国科学院新疆理化技术研究所 | Preparation method of super-hydrophobic, super-oleophylic and ultralight sponge |
CN104771936A (en) * | 2015-03-19 | 2015-07-15 | 南京工业大学 | Preparation method of high oil absorption sponge for oil-water separation |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107987311A (en) * | 2017-12-27 | 2018-05-04 | 淮阴工学院 | A kind of preparation method of hydrophobicity melamine sponge enhancing polysilsesquioxane composite aerogel |
CN108465460A (en) * | 2018-05-17 | 2018-08-31 | 江苏大学 | A kind of preparation method of super-hydrophobic sponge sorbing material |
CN109364888A (en) * | 2018-10-04 | 2019-02-22 | 南京航空航天大学溧水仿生产业研究院有限公司 | The preparation method of bionic super-hydrophobic absorption sponge |
CN110773137A (en) * | 2019-10-22 | 2020-02-11 | 同济大学 | Silicon dioxide nanorod-melamine foam compound and preparation method thereof |
CN116425553A (en) * | 2023-02-10 | 2023-07-14 | 浙江理工大学 | Preparation method for preparing heat-insulating boron nitride foam by in-situ vapor deposition |
CN116514556A (en) * | 2023-02-10 | 2023-08-01 | 浙江理工大学 | Preparation method of lightweight heat-insulating boron nitride foam |
CN116514556B (en) * | 2023-02-10 | 2024-07-23 | 浙江理工大学 | Preparation method of lightweight heat-insulating boron nitride foam |
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