CN112897898A - Method for improving mechanical strength of hollow glass microsphere and obtained hollow glass microsphere - Google Patents
Method for improving mechanical strength of hollow glass microsphere and obtained hollow glass microsphere Download PDFInfo
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- CN112897898A CN112897898A CN202010389530.5A CN202010389530A CN112897898A CN 112897898 A CN112897898 A CN 112897898A CN 202010389530 A CN202010389530 A CN 202010389530A CN 112897898 A CN112897898 A CN 112897898A
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- 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
- C03C23/007—Other surface treatment of glass not in the form of fibres or filaments by thermal treatment
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- 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
- C03C23/0095—Solution impregnating; Solution doping; Molecular stuffing, e.g. of porous glass
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Abstract
The invention discloses a method for improving the mechanical strength of hollow glass microspheres and the obtained hollow glass microspheres. The method for improving the mechanical strength of the hollow glass microsphere comprises the following steps: carrying out acid leaching treatment on the hollow glass microspheres; and carrying out heat treatment on the hollow glass microspheres subjected to acid leaching. According to the method, the surface of the hollow glass microsphere is subjected to acid leaching to remove alkali, and then heat treatment is carried out, so that the influence of the existence of alkaline oxides and defects on the surface of the hollow glass microsphere on the mechanical property and the surface state of the hollow glass microsphere is overcome, and the mechanical strength of the hollow glass microsphere is improved.
Description
Technical Field
The invention relates to the technical field of powder materials. More particularly, it relates to a method for improving the mechanical strength of hollow glass microspheres and the hollow glass microspheres obtained by the method.
Background
The rapid development of scientific technology has put higher demands on the comprehensive performance of high-end equipment, wherein light weight is an important consideration. For the application in many fields, the light weight of the base material is an important requirement for improving the comprehensive performance of the equipment. Light weight can generally be achieved by selecting low density functional materials or introducing hollow structures. From the viewpoint of functionality and mechanical strength of the material, the selection range of the low-density material is limited; the introduction of hollow structures has a greater range of applicability. The foamed structure in general can reduce the density through the hollow pores, but can significantly reduce the strength of the material. To make up for this deficiency, introducing closed cells through hollow microspheres is an effective way to increase strength on the premise of reducing density. The reason is that the spherical shell of the hollow microsphere can reinforce the pore wall of the foam pore, and the reduction of the mechanical property is relieved.
The hollow glass microspheres are a filler with low density and high strength, and are a composite material based on the hollow glass microspheres, high in specific strength and low in cost, so that the hollow glass microspheres are an important way for realizing light weight of functional and structural materials. For the hollow glass microsphere composite material, in order to reduce the density of the composite material as much as possible, a large proportion of hollow glass microspheres needs to be filled. Because the hollow glass microspheres are powder with micron-sized particle size and a thin spherical shell structure, the mechanical property difference with a polymer matrix is large, and the structural strength and the stability of the composite material can be obviously influenced by large-proportion filling of the hollow glass microspheres. Specifically, hollow glass microspheres directly form a weak zone inside the lightweight composite material, resulting in a weakening of the performance of the composite material. On the other hand, besides being used as a filler, the hollow glass microsphere can also be used as a low-density carrier of a micro-nano functional material, so that the obtained composite microsphere is endowed with low density and floatability, and the hollow glass microsphere is also required to have high structural strength. Therefore, both as a lightweight filler and a lightweight carrier, the hollow thin-walled structure is the source of its lightweight properties, which are lost by the destruction of the hollow structure.
In order to improve the strength of the hollow glass microspheres, the thickness of the spherical shell can be increased by reducing the ratio of the inner diameter to the outer diameter, but the density of the hollow microspheres is increased, which is not favorable for light weight.
Therefore, finding a proper method for processing the hollow glass microsphere shell has important significance in optimizing the mechanical property and the structural stability of the hollow glass microsphere shell on the premise of keeping the density.
Disclosure of Invention
The invention aims to provide a method for improving the mechanical strength of hollow glass microspheres, which overcomes the influence of the existence of alkaline oxides and defects on the surfaces of the hollow glass microspheres on the mechanical properties and the surface states of the hollow glass microspheres by carrying out surface acid leaching for removing alkali and then carrying out heat treatment on the hollow glass microspheres, thereby improving the mechanical strength of the hollow glass microspheres.
Another object of the present invention is to provide a hollow glass microsphere obtained by the above method.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for improving the mechanical strength of hollow glass microspheres, comprising the steps of:
carrying out acid leaching treatment on the hollow glass microspheres;
and carrying out heat treatment on the hollow glass microspheres subjected to acid leaching.
In a preferred embodiment of the present invention, the step of acid-washing the hollow glass microspheres further comprises: carrying out flotation on the hollow glass microspheres; so as to remove solid microspheres and other impurities in the hollow glass microspheres.
In this preferred embodiment, preferably, the flotation comprises the steps of:
mixing hollow glass microspheres with a solvent, stirring uniformly, standing for layering, taking an upper floating material, filtering, and drying for later use.
Preferably, the volume ratio of the hollow glass microspheres to the solvent is 1: 1-1: 10; as understood by the skilled in the art, the proportion of the solvent is enough for the flotation of the hollow glass microspheres, the volume ratio of the solvent can be theoretically infinitely high, but the factors such as the solvent cost, the operation convenience and the like need to be considered; if the volume ratio of the solvent is too low, the purpose of floating the low-density hollow glass microspheres on the surface of the solvent and floating the high-density microspheres and fragments at the bottom cannot be achieved, so the volume ratio of the low-density hollow glass microspheres to the high-density microspheres to the fragments is limited, and the volume ratio of the hollow glass microspheres to the solvent is preferably 1: 1-1: 10; for example 1:1 in the examples.
Preferably, the solvent is selected from ethanol, water or a mixture of the two. The solvent is selected to be free from chemical bond reaction with the surface of the hollow glass microsphere and easy to dry and remove.
In a preferred embodiment of the present invention, the step of acid-washing the hollow glass microspheres comprises: mixing the hollow glass microspheres with an acid solution, filtering, cleaning and drying; and sieving to remove agglomerated particles.
In this preferred embodiment, preferably, the acid in the acid solution is selected from organic or inorganic acids; more preferably an inorganic acid.
Preferably, the acid comprises one or a combination of two or more of acetic acid, hydrochloric acid, sulfuric acid and nitric acid.
Preferably, the acid solution has a concentration of: 0.01 mol/L-2 mol/L; more preferably 0.1mol/L to 1 mol/L.
Preferably, the mixing treatment is achieved by mixing and stirring; it may also be achieved by other conventional mixing means, such as ultrasonic vibration after mixing, etc.
Preferably, the time of the mixing treatment is 1min to 240 min; more preferably 5 to 60 min.
Preferably, the volume of the hollow glass microspheres treated with the acid solution is 10cm per liter3～1000cm3(ii) a More preferably 50cm3～500cm3。
Preferably, the solvent for washing is ethanol.
In a preferred embodiment of the present invention, the step of heat-treating the acid-washed hollow glass microspheres comprises: and (3) carrying out high-temperature heating treatment on the acidified hollow glass microspheres, and then screening to remove agglomerated particles.
In the preferred embodiment, the temperature of the high-temperature heating treatment is preferably 360 to 650 ℃; more preferably 400-650 ℃.
Preferably, the time of the high-temperature heating treatment is 1-48 h; more preferably 6 to 24 hours.
In a preferred embodiment of the present invention, the hollow glass microspheres after acid washing and/or heat treatment are stored in a dry environment for use. The dry environment may be provided by a drying oven or the like.
In a preferred embodiment of the present invention, the method for improving the mechanical strength of hollow glass microspheres comprises the steps of:
carrying out flotation on the hollow glass microspheres: mixing hollow glass microspheres with a solvent, stirring uniformly, standing for layering, taking an upper floating material, filtering, and drying for later use;
acid washing the floated hollow glass microspheres: mixing the hollow glass microspheres with an acid solution, and then filtering and drying; sieving to remove agglomerated particles;
carrying out heat treatment on the pickled hollow glass microspheres: and (3) carrying out high-temperature heating treatment on the acidified hollow glass microspheres, and then screening to remove agglomerated particles.
In a second aspect, the present invention provides a hollow glass microsphere obtained by the above process.
The invention has the following beneficial effects:
the invention carries out surface acid leaching on the hollow glass microspheres to remove alkali, and Na on the surfaces of the hollow glass microspheres2Separating out alkaline components such as O and the like; and when the high-temperature treatment is carried out, the Si-OH bonds on the surface of the microsphere shell are changed into Si-O-Si, and the addition of the O-Si-O bonds optimizes the surface structure of the hollow microsphere, reduces the surface defects of the microsphere shell and improves the mechanical strength of the hollow glass microsphere.
In addition, when the surface treatment method of the present invention is used, the composition and the surface state of the spherical shell can be directly adjusted by controlling the pickling time, the acid concentration, the heating temperature and the time. More importantly, the method provided by the invention is suitable for all different types of hollow glass microspheres containing alkali metal and/or alkaline earth metal, and the improved hollow glass microspheres with different properties are obtained.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 shows an SEM image of the whole blank hollow glass microspheres of example 5.
Figure 2 shows a photograph of a cross section of the shell wall of the hollow glass microsphere of example 5.
FIG. 3 shows a photograph of a cross section of the wall of the acid-washed hollow glass microsphere shell of example 5.
FIG. 4 shows a photograph of a cross-section of the shell wall of the heated hollow glass microsphere after acid washing in example 5.
FIG. 5 shows the compressive strength of hollow glass microspheres (the volume viability of the microspheres at 30 MPa) at different stages of the treatment in example 5.
Detailed Description
In order to make the technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
It is noted that all numerical designations of the invention (e.g., temperature, time, concentration, weight, and the like, including ranges for each) may generally be approximations that vary (+) or (-) by increments of 0.1 or 1.0, as appropriate. All numerical designations should be understood as preceded by the term "about".
Example 1
In this example, the method of the present invention was used to treat the self-made hollow glass microspheres
The invention relates to a self-made hollow glass microsphere, which is prepared according to patent 201210056295.5 'a soft chemical preparation method of a hollow glass microsphere, the prepared hollow glass microsphere and application thereof'. The density of the hollow glass microsphere is 0.38g/cm3The granularity is 20-80 mu m; the acid used in the acidification treatment is 0.1mol/L sulfuric acid.
The steps of surface treatment of the hollow microspheres in this example are as follows:
firstly, carrying out hollow glass microsphere flotation: mixing the hollow glass microspheres with ethanol in a volume ratio of 1:1, standing for layering, taking an upper-layer floating material, filtering, and drying for later use.
And then carrying out acid leaching treatment on the floated hollow glass microspheres: preparing 1mol/L hydrochloric acid solution, controlling the volume ratio of the hollow glass microspheres to the acid solution to be 1:1, mechanically stirring for 30min, filtering, cleaning with ethanol, drying, screening to remove agglomerated particles, and putting into a dryer for later use.
And finally, carrying out heat treatment on the hollow glass microspheres: and putting the hollow glass microspheres subjected to acid leaching into a muffle furnace, heating for 10 hours at 650 ℃, cooling, collecting, and putting into a dryer for later use.
Examples 2 to 15
The specific implementation steps are carried out as in example 1, with the specific distinguishing conditions shown in table 1:
table 1 examples changes in the surface treatment conditions of hollow glass microspheres
Description of the drawings: in the column of hollow glass microsphere types, firstly, the hollow glass microspheres are self-made microspheres; ② products of Yali science and technology Limited of Chinese; ③ is a product of new materials of Chinese Huaxing company Limited; fourthly, the product is a product of 3M company; fifthly, the product is a new material science and technology company Limited of the Maanshan institute of Medium Steel group. It is understood that the method of measuring pressure for a survival rate of 90% or more by volume is referred to in patent 201410196976.0 "a method of measuring isostatic strength of hollow glass beads".
FIG. 1 shows an overall SEM image of untreated hollow glass microspheres of example 5; FIG. 2 is a photograph showing a cross-sectional view of the shell wall of an untreated glass microsphere in example 5; FIG. 3 shows a photograph of a cross section of the shell wall of the acid-leached hollow glass microspheres of example 5; FIG. 4 shows a photograph of a cross-section of the shell wall of the heated hollow glass microsphere after acid leaching in example 5. It can be seen from the comparison of fig. 1-4 that after the acid leaching treatment, alkaline particles on the surface of the microsphere are separated out, the surface of the microsphere has more Si-OH bonds, when the microsphere is broken, burrs are likely to appear on the cross section of the hollow glass microsphere (fig. 3), and after the heating treatment, Si-O-Si bonds are formed on the surface of the microsphere, and the cross section of the hollow glass microsphere is relatively flat (fig. 4).
FIG. 5 is a graph of the compressive strength of hollow glass microspheres (the volumetric viability of the microspheres at 30 MPa) at various stages of the treatment in example 5. In the test, a true density meter is used for testing the true density of the hollow glass microspheres, inert fluid is used as a medium, the true density of the hollow glass microspheres is tested again after being pressurized at 30MPa, and the volume survival rate of the microspheres is measured according to the change of the true density before and after the pressure (refer to patent 201410196976.0, "a method for measuring isostatic pressure resistance of hollow glass microspheres"). In fig. 5, the compressive strength of the hollow glass microspheres subjected to acid leaching is reduced, mainly because after the acid leaching treatment, alkaline particles on the surfaces of the microspheres are precipitated by acid, microscopic defects exist on the surfaces of the microspheres, the volume survival rate of the hollow glass microspheres is reduced, and after the heating treatment, chemical bonds on the surfaces of the microspheres are rearranged to form more Si-O-Si bonds, so that the compressive strength is increased, and the volume survival rate of the microspheres is increased.
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that other variations or modifications may be made on the basis of the above description, and all embodiments may not be exhaustive, and all obvious variations or modifications may be included within the scope of the present invention.
Claims (10)
1. A method for improving the mechanical strength of hollow glass microspheres is characterized by comprising the following steps:
carrying out acid leaching treatment on the hollow glass microspheres;
and carrying out heat treatment on the hollow glass microspheres subjected to acid leaching.
2. The method of claim 1, wherein the step of acid leaching the hollow glass microspheres further comprises: carrying out flotation on the hollow glass microspheres;
preferably, the flotation comprises the following steps:
mixing hollow glass microspheres with a solvent, stirring uniformly, standing for layering, taking an upper floating material, filtering, and drying for later use;
preferably, the volume ratio of the hollow glass microspheres to the solvent is 1: 1-1: 10.
3. The method of claim 2, wherein the solvent is selected from the group consisting of ethanol, water, and a mixture thereof.
4. The method of claim 1, wherein the step of acid leaching the hollow glass microspheres comprises: mixing the hollow glass microspheres with an acid solution, and then filtering and drying; and sieving to remove agglomerated particles.
5. The method according to claim 4, wherein the acid in the acid solution is selected from the group consisting of organic or inorganic acids;
preferably, the acid comprises one or a combination of two or more of acetic acid, hydrochloric acid, sulfuric acid and nitric acid.
6. The method of claim 4, wherein the acid solution has a concentration of: 0.01mol/L to 2 mol/L.
7. The method according to claim 4, wherein the time of the mixing treatment is 1min to 240 min;
preferably, the volume of the hollow glass microspheres treated with the acid solution per liter is 10cm3～1000cm3；
Preferably, the solvent for washing is ethanol.
8. The method of claim 1, wherein the step of heat treating the acid-leached hollow glass microspheres comprises: carrying out high-temperature heating treatment on the hollow glass microspheres subjected to acid leaching, and then screening to remove agglomerated particles;
preferably, the temperature of the high-temperature heating treatment is 360-650 ℃;
preferably, the time of the high-temperature heating treatment is 1-48 h.
9. The method according to any one of claims 1 to 8, wherein the hollow glass microspheres after acid leaching and/or heat treatment are stored in a dry environment for use.
10. Hollow glass microspheres obtained by a process according to any one of claims 1 to 9.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114525104A (en) * | 2022-03-07 | 2022-05-24 | 郑州圣莱特空心微珠新材料有限公司 | Polysulfide sealant, preparation method and application thereof |
| CN114804658A (en) * | 2022-05-19 | 2022-07-29 | 陕西科技大学 | Environment-friendly and efficient glass microsphere brightening method |
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| US3972720A (en) * | 1974-03-01 | 1976-08-03 | Ppg Industries, Inc. | Phase separatable borosilicate glass compositions |
| CN1569710A (en) * | 2004-05-11 | 2005-01-26 | 武汉理工大学 | Process for preparing antibacterial fabric with high strength |
| CN101648776A (en) * | 2008-08-14 | 2010-02-17 | 比亚迪股份有限公司 | Method for improving strength of glass |
| CN103626401A (en) * | 2013-12-03 | 2014-03-12 | 汕头超声显示器（二厂）有限公司 | Touch screen glass chemical secondary strengthening method |
| CN104291688A (en) * | 2014-09-03 | 2015-01-21 | 宁波市合鑫玻璃科技有限公司 | Processing technology for single-sheet cesium potassium fireproof glass |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| GB597591A (en) * | 1945-07-12 | 1948-01-29 | Holophane Co Inc | Shock-resistant glass and a process of making the same |
| US3972720A (en) * | 1974-03-01 | 1976-08-03 | Ppg Industries, Inc. | Phase separatable borosilicate glass compositions |
| CN1569710A (en) * | 2004-05-11 | 2005-01-26 | 武汉理工大学 | Process for preparing antibacterial fabric with high strength |
| CN101648776A (en) * | 2008-08-14 | 2010-02-17 | 比亚迪股份有限公司 | Method for improving strength of glass |
| CN103626401A (en) * | 2013-12-03 | 2014-03-12 | 汕头超声显示器（二厂）有限公司 | Touch screen glass chemical secondary strengthening method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114525104A (en) * | 2022-03-07 | 2022-05-24 | 郑州圣莱特空心微珠新材料有限公司 | Polysulfide sealant, preparation method and application thereof |
| CN114804658A (en) * | 2022-05-19 | 2022-07-29 | 陕西科技大学 | Environment-friendly and efficient glass microsphere brightening method |
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