CN116135807A - Surface treatment method of glass hollow microsphere, glass hollow microsphere obtained by method and application of glass hollow microsphere - Google Patents
Surface treatment method of glass hollow microsphere, glass hollow microsphere obtained by method and application of glass hollow microsphere Download PDFInfo
- Publication number
- CN116135807A CN116135807A CN202111363793.XA CN202111363793A CN116135807A CN 116135807 A CN116135807 A CN 116135807A CN 202111363793 A CN202111363793 A CN 202111363793A CN 116135807 A CN116135807 A CN 116135807A
- Authority
- CN
- China
- Prior art keywords
- glass hollow
- hollow microspheres
- surface treatment
- microspheres
- composite material
- 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.)
- Pending
Links
- 239000004005 microsphere Substances 0.000 title claims abstract description 115
- 239000011521 glass Substances 0.000 title claims abstract description 72
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000004381 surface treatment Methods 0.000 title claims abstract description 27
- 239000002131 composite material Substances 0.000 claims abstract description 58
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000011282 treatment Methods 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims abstract description 4
- 238000012216 screening Methods 0.000 claims abstract description 3
- 229920005989 resin Polymers 0.000 claims description 16
- 239000011347 resin Substances 0.000 claims description 16
- 239000011159 matrix material Substances 0.000 claims description 11
- 229910052783 alkali metal Inorganic materials 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 150000001340 alkali metals Chemical class 0.000 claims description 5
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 5
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 2
- 239000004593 Epoxy Substances 0.000 claims 1
- 229920000098 polyolefin Polymers 0.000 claims 1
- 229920001296 polysiloxane Polymers 0.000 claims 1
- 229920002635 polyurethane Polymers 0.000 claims 1
- 238000010306 acid treatment Methods 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000001556 precipitation Methods 0.000 description 15
- 239000006260 foam Substances 0.000 description 14
- 238000007654 immersion Methods 0.000 description 13
- 239000006261 foam material Substances 0.000 description 9
- 239000011734 sodium Substances 0.000 description 8
- 238000002386 leaching Methods 0.000 description 7
- 239000002253 acid Substances 0.000 description 6
- 230000006835 compression Effects 0.000 description 6
- 238000007906 compression Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000003513 alkali Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 229910001413 alkali metal ion Inorganic materials 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000010335 hydrothermal treatment Methods 0.000 description 4
- 230000007774 longterm Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- -1 alkali metal alkaline earth metal Chemical class 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000002671 adjuvant Substances 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003090 exacerbative effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
- C03C23/008—Other surface treatment of glass not in the form of fibres or filaments comprising a lixiviation step
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C11/00—Multi-cellular glass ; Porous or hollow glass or glass particles
- C03C11/002—Hollow glass particles
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/28—Glass
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses a surface treatment method of glass hollow microspheres, the glass hollow microspheres obtained by the method, a composite material containing the glass hollow microspheres and a preparation method thereof. The surface treatment method comprises the steps of carrying out water treatment on the glass hollow microspheres; wherein, the water treatment method comprises the following steps: and mixing the glass hollow microspheres with water, stirring, filtering, drying, and screening to remove agglomerated particles to obtain the glass hollow microspheres after surface treatment. The scheme disclosed by the invention can at least solve the problems of environmental protection, stability, strength and the like of a composite material containing the glass hollow microspheres and the like caused by acid treatment of the glass hollow microspheres in the prior art.
Description
Technical Field
The invention relates to the technical field of composite materials. More particularly, it relates to a surface treatment method of glass hollow microspheres, glass hollow microspheres obtained by the method and applications thereof.
Background
With the rapid development of modern technology, composite materials are widely used in lightweight designs of structural and functional materials. The hollow microsphere composite material (also called as composite foam material) is a closed cell foam material obtained by mixing, forming and curing a hollow microsphere filler and matrix resin, and is an effective scheme for lightening the composite material. The composite foam has a cavity structure which is formed by a plurality of air pockets enclosed in hollow microspheres, and the spherical shell of the microspheres can play a role in mechanical reinforcement of the composite material and has higher strength and modulus. In addition, in the forming process, the composite foam material can avoid the defect that technological parameters are difficult to control in the forming process of the chemical foam material, and the size and the distribution of bubbles are controlled by adjusting the density and the filling quantity of the hollow balls, so that the density and the mechanical property of the material are regulated and controlled to meet different purposes. However, the addition of hollow microspheres introduces a large number of interfaces into the composite foam material compared to conventional foam structures. In addition to affecting the immediate performance of the composite foam, the interface state can also significantly affect the interface bonding in use and in storage in high temperature, high pressure and high humidity environments, and further result in performance decay of the composite foam. Therefore, from the viewpoints of long-term service performance and environmental suitability, it is important to develop a composite foam material stability study.
The glass hollow microsphere is easy to mold, high in compressive strength, easy to disperse and fill on the surface, and widely used as a hollow filler of composite foam. To achieve low density, the loading of microspheres is typically large, with interface problems not being negligible. However, from the standpoint of manufacturability and economy, the alkali metal alkaline earth metal components are added in the preparation process of the glass hollow microspheres, which not only leads to poor wettability of the microspheres with the resin, but also leads to easy dissolution of the alkali metal alkaline earth metal components in water environment, thereby destroying the interface between the microspheres and the resin matrix and exacerbating performance attenuation. The application number is 202010389519.9, the surface acid leaching treatment is carried out on the glass hollow microspheres, alkali on the surfaces of the microspheres is removed, and the durability of the glass hollow microspheres is improved. Acid treatment presents environmental issues such as post-treatment of acid solutions. Therefore, a more environment-friendly method for removing alkali on the surface of the microsphere and improving the stability of the composite material is needed to be found.
Disclosure of Invention
Based on the above-mentioned shortcomings, the present invention aims to provide a surface treatment method for glass hollow microspheres, glass hollow microspheres obtained by the method, composite materials containing the glass hollow microspheres and a preparation method thereof, so as to at least solve the environmental protection problem existing in the prior art when the glass hollow microspheres are subjected to acid treatment, and improve the stability, strength and other stability problems of the composite materials containing the glass hollow microspheres.
In one aspect, the present invention provides a surface treatment method of glass hollow microspheres, the method comprising the steps of subjecting the glass hollow microspheres to water treatment;
wherein, the water treatment method comprises the following steps:
and mixing the glass hollow microspheres with water, stirring, filtering, drying, and screening to remove agglomerated particles to obtain the glass hollow microspheres after surface treatment.
Further, the glass hollow microspheres are glass hollow microspheres containing alkali metal and/or alkaline earth metal.
In the method, the glass hollow microspheres are treated by water immersion, so that the alkaline metal on the surfaces of the glass hollow microspheres is removed, and the further precipitation of the alkaline metal ions is reduced. The method can achieve the degree of acid treatment, and is environment-friendly and pollution-free. Further, the temperature of the mixing is 1-90 ℃; and/or
The volume ratio of the glass hollow microspheres to the water is 1:1-1:40, preferably 1:5-1:20.
Further, the stirring and filtering times are 1-3 times; the time is 3-48 hours, preferably 6-24 hours.
Further, the stirring is mechanical stirring, and is used for dispersing the glass hollow microspheres in water.
Further, the water is one of deionized water, tap water and distilled water.
In a further aspect, the present invention provides a surface-treated glass hollow microsphere obtained by the surface treatment method as described in the first object above.
In yet another aspect, the present invention provides a method of preparing a high strength composite material, the method comprising the steps of:
and mixing the raw materials comprising the resin matrix and the glass hollow microspheres subjected to surface treatment, and molding to obtain the composite material.
The glass hollow microsphere after surface treatment is used as filler and is compounded with a resin matrix to form the composite material. After the composite material is exposed in water environment, the precipitation of alkali metal ions of microspheres in the composite material is reduced, so that the attenuation degree of the composite material is further weakened, and the long-term service performance and stability of the composite material are improved.
Further, the resin matrix is selected from one or more of epoxy resin, polyurethane, polyolefin and silicone resin.
Further, in the composite material, the volume content of the glass hollow microspheres subjected to surface treatment is 0.01-96%, preferably 40-70%.
It will be appreciated that in this embodiment, the raw materials may also contain some conventional adjuvants. Selection of specific adjuvants one skilled in the art can arrange according to the specific choice of resin matrix. Such as curing agents, diluents, accelerators, coupling agents, and the like.
Further, the preparation method comprises the following steps:
mixing a resin matrix with the mixture of the glass hollow microspheres subjected to surface treatment, and carrying out vacuum defoaming;
pouring the mixture into a mold, and vacuum defoaming;
and curing to obtain the composite material.
Further, the mixture is subjected to vacuum deaeration treatment prior to use.
Further, the vacuum defoaming mode is replaced by vacuum vibration defoaming, and the times are 3 times.
On the other hand, the invention also provides the high-strength composite material prepared by the preparation method.
The beneficial effects of the invention are as follows:
in the surface treatment method of the glass hollow microsphere provided by the invention, the glass hollow microsphere is subjected to surface water immersion to remove alkali, so that Na on the surface of the glass hollow microsphere is removed 2 The alkaline components such as O and the like are separated out, so that the further separation of alkali metal ions is reduced, and the stability of the microsphere is improved. The method can directly obtain a series of stable glass hollow microspheres through controlling the water immersion treatment time, the treatment times, the treatment water quantity and the heating temperature. In addition, the method provided by the invention is suitable for all different types of glass hollow microspheres containing alkali metal and/or alkaline earth metal.
According to the invention, the composite material obtained by compounding the microsphere and the resin matrix is obtained after alkali is removed by water immersion, and after the composite material is exposed in water environment, the precipitation of alkali metal ions of the microsphere in the composite foam is reduced, and accordingly, the attenuation degree of the performance of the composite foam is obviously reduced, so that the composite material has better usability and storage stability.
Drawings
The following describes the embodiments of the present invention in further detail with reference to the drawings.
FIG. 1 shows the process flow of the present invention for glass hollow microsphere surface treatment and further use in the preparation of composites with resins.
FIG. 2 shows XRF test results of microspheres and blank microspheres after water treatment in example 1 of the present invention.
FIG. 3 shows the NaO microspheres before and after water immersion in example 1 of the present invention 2 The content is reduced.
Fig. 4 shows the results of the secondary precipitation amount of the microsphere Na before and after the secondary water immersion in example 1 of the present invention.
Fig. 5 shows the instant compression and hydrothermal and damp-heat compression strength diagrams of composite foam formed by glass hollow microspheres and blank glass hollow microspheres after water immersion in example 1 of the present invention.
Detailed Description
In order to more clearly illustrate the present invention, the present invention will be further described with reference to preferred embodiments and the accompanying drawings. Like parts in the drawings are denoted by the same reference numerals. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and that this invention is not limited to the details given herein.
In this embodiment, the hollow glass microsphere may be commercially available, or may be realized by referring to the technical scheme disclosed in the chinese patent publication of application No. 201210056295.5 entitled "a method for preparing hollow glass microsphere with soft chemistry and the hollow glass microsphere prepared and application thereof". The density of the glass hollow microsphere is 0.30g/cm 3 Model T30, granularity of 20-80 μm, and deionized water.
In the embodiment of the invention, the surface treatment of the glass hollow microsphere and the process flow for further using the glass hollow microsphere in the preparation of the composite material by compounding the glass hollow microsphere with resin are shown in the figure 1.
Some performance testing methods: carrying out XRF characterization on the content of microsphere elements; icp detects the alkali metal ion precipitation amount of the composite foam material; performance, uniaxial compression performance. For stability experiments, the stability characterization used employed was a change in performance after 100 ℃ hydrothermal treatment; the storage stability was changed by a wet heat treatment at 80℃and a humidity of 93%.
Example 1
The surface treatment of the hollow microspheres in this example is as follows:
controlling the volume ratio of the glass hollow microspheres (T30) to deionized water to be 1:15, mechanically stirring for 8 hours at room temperature, filtering, repeating for three times, and drying; sieving to remove agglomerated particles. The soaking solution was subjected to an icp test and compared with the pickling 1h disclosed in the chinese patent application No. 202010389519.9, and the results are shown in table 1. XRF testing was performed on both the blank microspheres and the water treated microspheres, and the results are shown in figure 2. Leaching for 1h, the precipitation amount of the microsphere Na is 5419 mug/g, table1, the total precipitation amount of the Na of the water leaching microsphere is 5345 mug/g, and the acid leaching effect is basically achieved. Microsphere NaO after water immersion as described in FIG. 3 2 The content is reduced by 11%.
Table 1: na content variation in the water immersed microsphere solution of this example
In order to further test the alkali removal effect on the surface of the hollow microsphere, respectively carrying out water leaching treatment on the blank microsphere and the microsphere after water leaching, controlling the volume ratio of the microsphere to deionized water to be 1:30, mechanically stirring for 1h at room temperature, and carrying out icp analysis on the obtained aqueous solution. As shown in FIG. 4, the secondary precipitation amount of Na in the microspheres after water immersion is obviously reduced, and the stability is improved.
Finally, the preparation process of the composite foam material is carried out: uniformly mixing several reagents of epoxy resin E51, TDE85, methyl hexahydrophthalic anhydride, N-dimethylbenzylamine and KH560 according to the mass ratio of 100:100:228.5:4.3:4.3, respectively adding the blank glass hollow microspheres and the glass hollow microspheres subjected to water immersion treatment, wherein the adding ratio of the glass hollow microspheres accounts for 58% of the volume ratio of the composite material, and heating and curing at 80 ℃, 120 ℃ and 160 ℃ for 2 hours, 2 hours and 4 hours respectively. After cooling, the corresponding composite material is obtained. The resultant composite foam materials were then subjected to respective hydrothermal treatments at 100℃and a humidity of 93% at 80℃and, after 12 hours, the uniaxial compression property was changed, and the results were shown in FIG. 5. The compression strength of the composite foam formed by the blank microspheres is reduced by 22.3% after hydrothermal treatment, and the strength is reduced by 17.0% after damp-heat treatment; the instant strength of the composite foam formed by the microspheres is almost unchanged after water immersion, but the performance is reduced by only 5.9% after hydrothermal treatment, the use stability is obviously improved, the performance is reduced by only 3.8% after wet heat treatment, and the storage stability is obviously improved. In a word, the long-term service performance and stability of the composition are improved. Meanwhile, the icp test is carried out on the hydrothermal soaking liquid, and the result is shown in figure 5, the Na precipitation amount of the composite foam formed by the microspheres after water immersion is reduced by 31.6% compared with that of the composite foam formed by the blank microspheres, which shows that the microspheres after water immersion not only obviously reduce the precipitation of alkali metal of the microspheres, but also further reduce the precipitation of alkali metal of the microspheres in the formed composite foam, thereby improving the long-term stability of the composite foam.
Examples 2 to 12
Examples 2-12 the specific implementation procedure was carried out as in example 1, with specific differences and the resulting composite material performance parameters as shown in table 2 (wherein the molding conditions for the composite materials of different resin matrices were followed by the conventional curing conditions for the corresponding resins).
TABLE 2 preparation conditions and Performance parameters of glass hollow microsphere composites in examples 2-12
Note that: ion secondary precipitation rate: under the same conditions, the Na precipitation amount of the water immersed microsphere after the water immersed microsphere is immersed again is the ratio of the Na precipitation amount of the blank microsphere.
Comparative example 1
T30 glass hollow microspheres are adopted, acid leaching treatment is adopted, acid liquor is hydrochloric acid with the volume ratio of 1mol/L, the microspheres and the acid liquor are 1:1.5, mechanical stirring treatment is carried out for 1h, and then filtration and drying are carried out for standby. The preparation method and the material proportion of the composite material are the same as in example 2. The compression strength attenuation rate of the obtained composite material after the hydrothermal environment treatment is 6.82%; the reduction rate of sodium ion precipitation (compared with the composite material corresponding to untreated microspheres) of the composite material after the hydrothermal environment treatment is 28.1%.
It should be understood that the foregoing examples of the present invention are provided merely for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention, and that various other changes and modifications may be made therein by one skilled in the art without departing from the spirit and scope of the present invention as defined by the appended claims.
Claims (10)
1. A surface treatment method of glass hollow microspheres is characterized by comprising the step of carrying out water treatment on the glass hollow microspheres;
wherein, the water treatment method comprises the following steps:
and mixing the glass hollow microspheres with water, stirring, filtering, drying, and screening to remove agglomerated particles to obtain the glass hollow microspheres after surface treatment.
2. The surface treatment method according to claim 1, wherein the temperature of the mixing is 1 to 90 ℃; and/or
The volume ratio of the glass hollow microspheres to the water is 1:1-1:40.
3. The surface treatment method according to claim 1, wherein the number of stirring and filtering is 1 to 3; the time is 3-48h.
4. The surface treatment method according to claim 1, wherein the glass hollow microspheres are alkali metal and/or alkaline earth metal-containing glass hollow microspheres.
5. Surface-treated glass hollow microspheres obtained by the surface treatment method according to any one of claims 1 to 4.
6. The preparation method of the high-strength composite material is characterized by comprising the following steps of:
mixing the raw materials comprising the resin matrix and the glass hollow microspheres subjected to surface treatment according to claim 5, and forming to obtain the composite material.
7. The method according to claim 6, wherein the resin matrix is one or more selected from the group consisting of epoxy, polyurethane, polyolefin, and silicone.
8. The method according to claim 6, wherein the glass hollow microspheres after surface treatment have a volume content of 0.01-96%, preferably 40-70%.
9. The preparation method according to claim 6, characterized in that the preparation method comprises the steps of:
mixing a resin matrix with the mixture of the glass hollow microspheres subjected to surface treatment, and carrying out vacuum defoaming;
pouring the mixture into a mold, and vacuum defoaming;
and curing to obtain the composite material.
10. A high strength composite material prepared by the method of any one of claims 6-9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111363793.XA CN116135807A (en) | 2021-11-17 | 2021-11-17 | Surface treatment method of glass hollow microsphere, glass hollow microsphere obtained by method and application of glass hollow microsphere |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111363793.XA CN116135807A (en) | 2021-11-17 | 2021-11-17 | Surface treatment method of glass hollow microsphere, glass hollow microsphere obtained by method and application of glass hollow microsphere |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116135807A true CN116135807A (en) | 2023-05-19 |
Family
ID=86326783
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111363793.XA Pending CN116135807A (en) | 2021-11-17 | 2021-11-17 | Surface treatment method of glass hollow microsphere, glass hollow microsphere obtained by method and application of glass hollow microsphere |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116135807A (en) |
-
2021
- 2021-11-17 CN CN202111363793.XA patent/CN116135807A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111534055B (en) | Composite material based on modified hollow glass microspheres and preparation method thereof | |
| CN101428962B (en) | Reinforcing method for ultra-thin lithium alumina silicate glass | |
| CN110078515A (en) | A kind of preparation method of graphene oxide modified carbon fiber enhancing carbon/silicon carbide ceramic matrix composite | |
| CN109370133B (en) | Method for reinforcing polymethyl methacrylate by cellulose | |
| CN108911607B (en) | Assembled wall material and preparation method thereof | |
| CN113072314A (en) | Treatment method of household garbage incineration fly ash | |
| CN112679763A (en) | Carbon fiber resin matrix composite material and preparation method thereof | |
| CN101709130A (en) | Ultra-low density solid buoyant material and manufacture method | |
| CN116444945A (en) | High-heat-conductivity hollow boron nitride microsphere composite polymer material and preparation method thereof | |
| CN111161901B (en) | Method for treating radioactive iodine waste | |
| CN115594505A (en) | Bulletproof ceramic material and preparation method thereof | |
| CN116135807A (en) | Surface treatment method of glass hollow microsphere, glass hollow microsphere obtained by method and application of glass hollow microsphere | |
| Liu et al. | Preparation of a cenosphere curing agent and its application to foam concrete | |
| CN115319883B (en) | Three-period minimum curved surface structure geopolymer and preparation method thereof | |
| CN109354448B (en) | Method for preparing light foam concrete by using municipal solid waste incineration slag | |
| CN100335664C (en) | Shielded Pb-base composite materials with high-energy ray and production thereof | |
| CN111690242B (en) | High-temperature-resistant acid-resistant UV (ultraviolet) protective film and preparation method thereof | |
| CN108296477A (en) | A kind of 3D printing precoated sand and preparation method thereof | |
| CN113733353A (en) | Production process of super-durable building concrete | |
| CN113881247A (en) | Surface grafting modification treatment method for anti-settling boron carbide powder | |
| CN116535812A (en) | Composite material based on interface reinforced glass hollow microspheres and preparation method thereof | |
| CN115180867B (en) | Targeted sulfate corrosion-resistant preservative with spherical shell structure and preparation method and application thereof | |
| CN114276497B (en) | Paraffin-modified styrene-acrylate-siloxane core-shell phase-change emulsion and preparation method and application thereof | |
| CN115959873B (en) | High-ductility concrete with high bending toughness and preparation method thereof | |
| CN116690742B (en) | Bamboo wood modification method for co-production of aragonite type nano calcium carbonate |
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 |