CN-122010410-A - Preparation method of magnetic hollow glass beads

Abstract

The invention discloses a preparation method of magnetic hollow glass beads, and belongs to the technical field of functional material preparation. The method comprises the following steps of mixing various glass forming raw materials, melting the raw materials into glass liquid at 1400-1600 ℃, carrying out water quenching, crushing and grading to obtain magnetic glass powder, mixing the magnetic glass powder and paste according to a mass ratio of 1:1-2.5, simultaneously adding sodium dodecyl benzene sulfonate, forming magnetic precursor particles through spray granulation, placing the precursor particles into a negative pressure spheroidizing furnace, foaming and spheroidizing, carrying out hydrofluoric acid surface etching on the obtained microbeads to form a sand grinding layer, coating a barium ferrite magnetization layer, and separating and collecting the magnetic glass particles through a specific gravity sorting method to obtain the magnetic glass microbeads.

Inventors

• ZHONG ZHAOJIN
• ZHANG ZHENGYI
• XU JIAXIN
• ZHOU JUNJIE
• JIAO JINXU
• DONG WEIYONG
• WANG HUAWEN
• PENG XIAOBO

Assignees

• 中建材玻璃新材料研究院集团有限公司
• 中国建材集团有限公司

Dates

Publication Date

20260512

Application Date

20260205

Claims (5)

1. 1. The preparation method of the magnetic hollow glass microsphere is characterized by comprising the following steps of: Step 1, mixing various glass forming raw materials, melting into glass liquid at 1400-1600 ℃, and obtaining magnetic glass powder after water quenching, crushing and grading; Step 2, mixing magnetic glass powder and paste according to a mass ratio of 1:1-2.5, simultaneously adding sodium dodecyl benzene sulfonate accounting for 0.1-0.5% of the mass of the magnetic glass powder, and forming magnetic precursor particles through spray granulation; And step 3, placing the precursor particles in a negative pressure spheroidizing furnace, completing foaming and spheroidizing treatment under the process conditions of 1200-1400 ℃ and 0.02-0.08MPa, then carrying out hydrofluoric acid surface etching on the obtained microbeads to form a sand grinding layer, coating a barium ferrite magnetization layer, and finally separating and collecting by a specific gravity sorting method to obtain the magnetic glass microbeads.
2. 2. The preparation method of the magnetic hollow glass microsphere according to claim 1, wherein the glass forming raw materials comprise, by weight, 58-60 parts of quartz sand, 14-18 parts of boric acid, 9-12 parts of calcium carbonate, 8-12 parts of sodium carbonate, 1-2 parts of mirabilite and 8-10 parts of ferroferric oxide.
3. 3. The preparation method of the magnetic hollow glass microsphere according to claim 1, wherein the paste comprises, by weight, 2-6 parts of starch, 2-6 parts of cellulose and 80-90 parts of deionized water.
4. 4. The method for preparing the magnetic hollow glass beads according to claim 1, wherein the density of the magnetic glass beads is 0.68-0.98g/cm 3 and the saturation magnetization is 29-42emu/g.
5. 5. The method for preparing the magnetic hollow glass beads according to claim 1, wherein the etching process parameters are that the temperature is 20-40 ℃ and the time is 1-5min, and the concentration of hydrofluoric acid is 3-6wt%.

Description

Preparation method of magnetic hollow glass beads Technical Field The invention belongs to the technical field of functional material preparation, and particularly relates to a preparation method of magnetic hollow glass beads. Background The hollow glass microsphere is a micron-sized glass spherical material with a hollow structure, and has a series of excellent characteristics of low density, excellent heat and sound insulation performance, high and low temperature resistance, good electrical insulation, high thermal stability, chemical corrosion resistance and the like. Based on the characteristics, the hollow glass microspheres can be used as functional filler to be applied to resin-based composite materials, such as deep sea buoyancy materials, high-performance heat insulation materials and the like, can be used for preparing low-density cement paste and drilling fluid in the field of building materials, and is beneficial to solving the technical problems in deep well cementation and drilling, and in addition, the material has wide application potential in special functional materials such as aerospace ablation protection, hydrogen storage media, electromagnetic shielding and the like. The magnetic hollow glass bead is a multifunctional composite material prepared by introducing magnetic components (such as ferroferric oxide) through a surface modification or integrated composite mode on the basis of retaining the characteristics of the hollow glass bead. The material has the light weight, heat insulation and good dispersibility of the hollow glass beads and the external field magnetic response characteristic of the magnetic material, so that the application range of the material in the high technical fields of targeted conveying, separation and recovery, intelligent sensing and the like is remarkably expanded. At present, the common methods for magnetically modifying hollow glass beads mainly comprise surface modification technologies such as a hydrothermal method, a magnetron sputtering method and an electroless plating method. Although the methods have the characteristics, the method has obvious limitations such as good uniformity of a coating layer by a hydrothermal method, long reaction period and low efficiency, high equipment cost and complex process of a magnetron sputtering method, and relatively low cost of an electroless plating method, and the obtained magnetic layer has weak bonding strength and is easy to fall off, so that the magnetic performance is unstable. In addition, the traditional integrated preparation process such as a powder melting method, a template method and the like also commonly has the problems of uneven magnetic distribution, difficult cooperative regulation and control of the density and magnetic performance of the microbeads, higher preparation cost and the like. Therefore, in order to solve the problems, the invention provides a preparation method of magnetic hollow glass beads. Disclosure of Invention The invention aims to overcome the defects of the prior art and provides a preparation method of magnetic hollow glass beads. The aim of the invention can be achieved by the following technical scheme: The preparation method of the magnetic hollow glass microsphere comprises the following steps: Step 1, mixing various glass forming raw materials, melting into glass liquid at 1400-1600 ℃, and obtaining magnetic glass powder after water quenching, crushing and grading; Step 2, mixing magnetic glass powder and paste according to a mass ratio of 1:1-2.5, simultaneously adding sodium dodecyl benzene sulfonate accounting for 0.1-0.5% of the mass of the magnetic glass powder, and forming magnetic precursor particles through spray granulation; And step 3, placing the precursor particles in a negative pressure spheroidizing furnace, completing foaming and spheroidizing treatment under the process conditions of 1200-1400 ℃ and 0.02-0.08MPa, then carrying out hydrofluoric acid surface etching on the obtained microbeads to form a sand grinding layer, coating a barium ferrite magnetization layer, and finally separating and collecting by a specific gravity sorting method to obtain the magnetic glass microbeads. More optimally, the glass forming raw materials comprise, by weight, 58-60 parts of quartz sand, 14-18 parts of boric acid, 9-12 parts of calcium carbonate, 8-12 parts of sodium carbonate, 1-2 parts of mirabilite and 8-10 parts of ferroferric oxide. More preferably, the paste is composed of, by weight, 2-6 parts of starch, 2-6 parts of cellulose, and 80-100 parts of deionized water. More optimally, the density of the magnetic glass beads is 0.68-0.98g/cm 3, and the saturation magnetization is 29-42emu/g. More optimally, the etching process parameters are that the temperature is 20-40 ℃ and the time is 1-5min, wherein the concentration of hydrofluoric acid is 3-6wt%. The invention has the beneficial effects that: The preparation method of the magnetic hollow glass microsphere