CN103964707A - Method of improving fluidity of hollow glass bead powder - Google Patents

Method of improving fluidity of hollow glass bead powder Download PDF

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Publication number
CN103964707A
CN103964707A CN201410196965.2A CN201410196965A CN103964707A CN 103964707 A CN103964707 A CN 103964707A CN 201410196965 A CN201410196965 A CN 201410196965A CN 103964707 A CN103964707 A CN 103964707A
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China
Prior art keywords
hollow glass
glass micropearl
powder
glass bead
fluidity
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Pending
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CN201410196965.2A
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Chinese (zh)
Inventor
钟舜
张敬杰
严开祺
杨岩峰
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Technical Institute of Physics and Chemistry of CAS
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Technical Institute of Physics and Chemistry of CAS
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Priority to CN201410196965.2A priority Critical patent/CN103964707A/en
Publication of CN103964707A publication Critical patent/CN103964707A/en
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Abstract

The invention belongs to the technical field of inorganic powder material surface treatment and in particular relates to a method of improving the fluidity of hollow glass bead powder. The method is characterized by comprising the steps of dissolving an alkaline matter in water to prepare an alkaline solution with a certain concentration, adding the hollow glass bead powder in the alkaline solution, mixing for a certain time, filtering, washing, and drying to obtain the hollow glass bead powder with good fluidity. The method is non-toxic, is low in cost and is simple in operation. With the adoption of the method, the fluidity of the hollow glass bead powder after treating is obviously improved, and meanwhile, the true density and the compression strength of a hollow glass bead are little influenced.

Description

A kind of method that improves hollow glass micropearl powder fluidity
Technical field
The invention belongs to inorganic powder material technical field of surface, particularly a kind of method of improving hollow glass micropearl powder fluidity.
Background technology
Hollow glass micropearl is a kind of novel inorganic powder body material growing up in nearest twenty or thirty year, and main component is basic metal or alkaline earth borosilicate, and particle is hollow ball shape structure, and particle diameter arrives between hundreds of micron at several microns.Many excellent properties such as the miniature spherical hollow structure of this uniqueness of hollow glass micropearl makes it have that density is little, good fluidity, thermal conductivity are low, good insulation preformance, compressive strength is large, chemical stability is good.Therefore, hollow glass micropearl has been widely used in the fields such as petrochemical complex, coatings industry, material of construction, emulsion explosive, fire-retardant material, and hollow glass micropearl also reaches its maturity in the application in the most advanced and sophisticated national defence fields such as deep diving exploration and space flight and aviation simultaneously.Thus, hollow glass micropearl has huge market potential and wide application prospect.In theory, spherical hollow glass micropearl particle has good mobility, but due to a large amount of silicon hydroxyls of surface existence, without the hollow glass micropearl product of any processing in long-term storage and transportation, easily absorb gradually airborne moisture and lose flowability gradually, finally harden together, this will have a strong impact on the further use of hollow glass micropearl, so be necessary in advance hollow glass micropearl to be carried out to certain processing to improve its mobility.
At present, also less about the research that improves hollow glass micropearl mobility, existing research is mainly by realizing at the coated one deck organism in hollow glass micropearl surface.In Chinese patent CN103232170A, announce a kind of method that prevents hollow glass micropearl moisture absorption caking.The method is by hollow glass micropearl being immersed in trimethoxy chlorosilane solution, thereby the organic group of introducing hydrophobic nature on hollow glass micropearl surface reaches the object that prevents the hollow glass micropearl moisture absorption and improve its mobility.But the method exists organism used to have the deficiencies such as the higher and operation relative complex of certain toxicity, cost, so be necessary to seek a kind of more simple method that improves efficiently hollow glass micropearl powder fluidity.
Hollow glass micropearl carries out in surface-functionalized process, alkaline solution also can be used to hollow glass micropearl powder to carry out pre-treatment, as Chinese patent CN103566977A, CN102964878A and CN102311233A, but their object is just in order to remove the greasy dirt on hollow glass micropearl surface or to increase the quantity of surperficial activity hydroxy, instead of improve the mobility of hollow glass micropearl powder.
Summary of the invention
The object of the invention is to overcome in prior art the defect that exists organism used while improving hollow glass micropearl mobility to have the higher and operation relative complex of certain toxicity, cost, a kind of method that can improve hollow glass micropearl powder fluidity is provided, the method is nontoxic, cost is low, simple to operate, through the mobility of present method hollow glass micropearl powder after treatment be improved significantly, true density and the compressive strength impact of present method on hollow glass micropearl is simultaneously very little.
The object of the invention is to be achieved by following technical solution:
A kind of method that improves hollow glass micropearl powder fluidity, it is characterized in that, use that alkaline matter is soluble in water is mixed with certain density basic solution, hollow glass micropearl powder is joined in this basic solution, stir certain hour, after filtering, rinsing, put into baking oven and dry certain hour, obtain the hollow glass micropearl powder of good fluidity.
Further technical scheme of the present invention is, hollow glass micropearl is joined in the basic solution preparing, temperature maintains 20~30 DEG C, stir 5~30 minutes with the rotating speeds of 600~1200 revs/min, with filter screens more than 800 orders, hollow glass micropearl is leached again, then use solvent as the flushings such as water, methyl alcohol, ethanol or acetone 1-20 time, put into baking oven and be warming up to 50~120 DEG C, more than being incubated 0.5 hour, to dry out solvent, after oven dry, obtain the hollow glass micropearl powder of good fluidity.
Described alkaline matter is sodium hydroxide, lithium hydroxide, potassium hydroxide and the calcium hydroxide etc. that alkalescence is stronger.The volumetric molar concentration of the basic solution of preparation should be between 0.05~0.5 mol/L, and concentration is too low, and treatment effect is not obvious; Excessive concentration easily causes the fragmentation of hollow glass micropearl particle and the decline of compressive strength.
Described hollow glass micropearl powder refers to the hollow glass micropearl powder of Lower alrali content, does not comprise the common hollow glass micropearl powder of flyash and high alkali content.
The mobility of described hollow glass micropearl powder is to weigh by the size at the slope of repose of powder, and the described good mobility of hollow glass micropearl powder requires its slope of repose to be less than 30 °.The present invention tests the slope of repose of hollow glass micropearl powder with reference to the injection method specifying in standard GB/T/T6609.23.
Through the present invention's hollow glass micropearl powder after treatment, except having good mobility, density and the compressive strength of hollow glass micropearl almost do not change.The true density of hollow core glass microballon of the present invention and compressive strength test are all carried out according to the regulation in national military standard GJB3594.
Beneficial effect of the present invention:
Because the main component of hollow glass micropearl is borosilicate, so it has been generally acknowledged that alkaline solution can produce certain corrasion to hollow glass micropearl, reduce the compressive strength of hollow glass micropearl.The invention has the advantages that and find to use the alkaline solution of suitable concn to soak the regular hour to hollow glass micropearl, can't produce significantly impact to the true density of hollow glass micropearl and compressive strength, the mobility of hollow glass micropearl powder has obtained obvious raising simultaneously.
Research according to the article (Kouassi, S.S., J.Andji, et al.Ceramics-Silikaty.2010,54:235.) of 235 pages of " ceramics " magazine the 54th volumes in 2010 to reaction mechanism between alkali and silicate glass, the OH in alkaline solution -after the Si-O-Si network destroying in hollow glass micropearl, can in solution, form some insolubless, be mainly silicate and the carbonate of alkaline-earth metal, and these insolubless can further be deposited on glass surface and form one deck coating film.By further infrared spectrum characterization, research finds that the wetting ability of this layer of coating film is poorer than the original surface of glass.Therefore, by reducing the water absorbability of hollow glass micropearl particle surface after alkaline solution treatment of hollow glass bead, reduce the intergranular clinging power of hollow glass micropearl, and then improve the mobility of hollow glass micropearl powder.
Technique of the present invention is simple, efficiency is high, cost is low, is improved significantly through the mobility of present method hollow glass micropearl powder after treatment, and true density and the compressive strength impact of present method on hollow glass micropearl is simultaneously very little.Can withstand long-term storage and transportation process and moisture absorption caking does not occur through the hollow glass micropearl product of processing of the present invention.
Embodiment
Below in conjunction with embodiment, the invention will be further described but not limit the scope of the invention.
Embodiment 1
50 grams of prepared T30 series high-performance hollow glass micropearl samples of Chinese Academy of Sciences's physics and chemistry are joined in the aqueous sodium hydroxide solution that 500 ml concns are 0.05 mol/L, temperature maintains approximately 25 DEG C, stir 30 minutes with the rotating speeds of 1200 revs/min, with 800 object filter screens, hollow glass micropearl is leached again, then use deionized water rinsing 1 time, put into baking oven and be warming up to 120 DEG C, be incubated 2 hours to dry out solvent, after oven dry, obtaining slope of repose is the hollow glass micropearl powder of the good fluidity of 24 °.
Embodiment 2
50 grams of prepared T30 series high-performance hollow glass micropearl samples of Chinese Academy of Sciences's physics and chemistry are joined in the potassium hydroxide aqueous solution that 500 ml concns are 0.1 mol/L, temperature maintains approximately 25 DEG C, stir 20 minutes with the rotating speeds of 1000 revs/min, with 800 object filter screens, hollow glass micropearl is leached again, then use washed with methanol 5 times, put into baking oven and be warming up to 100 DEG C, be incubated 0.5 hour to dry out solvent, after oven dry, obtaining slope of repose is the hollow glass micropearl powder of the good fluidity of 23 °.
Embodiment 3
50 grams of prepared T30 series high-performance hollow glass micropearl samples of Chinese Academy of Sciences's physics and chemistry are joined in the lithium hydroxide aqueous solution that 500 ml concns are 0.2 mol/L, temperature maintains approximately 25 DEG C, stir 15 minutes with the rotating speeds of 800 revs/min, with 800 object filter screens, hollow glass micropearl is leached again, then use alcohol flushing 10 times, put into baking oven and be warming up to 80 DEG C, be incubated 1 hour to dry out solvent, after oven dry, obtaining slope of repose is the hollow glass micropearl powder of the good fluidity of 23.5 °.
Embodiment 4
50 grams of prepared T30 series high-performance hollow glass micropearl samples of Chinese Academy of Sciences's physics and chemistry are joined in the aqueous sodium hydroxide solution that 500 ml concns are 0.1 mol/L, temperature maintains approximately 25 DEG C, stir 20 minutes with the rotating speeds of 1000 revs/min, with 800 object filter screens, hollow glass micropearl is leached again, then use acetone rinsing 5 times, put into baking oven and be warming up to 80 DEG C, be incubated 1 hour to dry out solvent, after oven dry, obtaining slope of repose is the hollow glass micropearl powder of the good fluidity of 22.5 °.
Embodiment 5
50 grams of prepared T30 series high-performance hollow glass micropearl samples of Chinese Academy of Sciences's physics and chemistry are joined in the potassium hydroxide aqueous solution that 500 ml concns are 0.05 mol/L, temperature maintains approximately 25 DEG C, stir 30 minutes with the rotating speeds of 800 revs/min, with 800 object filter screens, hollow glass micropearl is leached again, then use deionized water rinsing 3 times, put into baking oven and be warming up to 120 DEG C, be incubated 2 hours to dry out solvent, after oven dry, obtaining slope of repose is the hollow glass micropearl powder of the good fluidity of 24.5 °.
Embodiment 6
50 grams of prepared T30 series high-performance hollow glass micropearl samples of Chinese Academy of Sciences's physics and chemistry are joined in the lithium hydroxide aqueous solution that 500 ml concns are 0.3 mol/L, temperature maintains approximately 25 DEG C, stir 10 minutes with the rotating speeds of 800 revs/min, with 800 object filter screens, hollow glass micropearl is leached again, then use acetone rinsing 15 times, put into baking oven and be warming up to 50 DEG C, be incubated 0.5 hour to dry out solvent, after oven dry, obtaining slope of repose is the hollow glass micropearl powder of the good fluidity of 23.5 °.
Embodiment 7
50 grams of prepared T40 series high-performance hollow glass micropearl samples of Chinese Academy of Sciences's physics and chemistry are joined in the aqueous sodium hydroxide solution that 500 ml concns are 0.25 mol/L, temperature maintains approximately 25 DEG C, stir 10 minutes with the rotating speeds of 800 revs/min, with 800 object filter screens, hollow glass micropearl is leached again, then use acetone rinsing 15 times, put into baking oven and be warming up to 50 DEG C, be incubated 0.5 hour to dry out solvent, after oven dry, obtaining slope of repose is the hollow glass micropearl powder of the good fluidity of 23.5 °.
Embodiment 8
50 grams of prepared T40 series high-performance hollow glass micropearl samples of Chinese Academy of Sciences's physics and chemistry are joined in the potassium hydroxide aqueous solution that 500 ml concns are 0.1 mol/L, temperature maintains approximately 25 DEG C, stir 20 minutes with the rotating speeds of 1000 revs/min, with 800 object filter screens, hollow glass micropearl is leached again, then use washed with methanol 5 times, put into baking oven and be warming up to 85 DEG C, be incubated 0.5 hour to dry out solvent, after oven dry, obtaining slope of repose is the hollow glass micropearl powder of the good fluidity of 23 °.
Embodiment 9
50 grams of prepared T40 series high-performance hollow glass micropearl samples of Chinese Academy of Sciences's physics and chemistry are joined in the lithium hydroxide aqueous solution that 500 ml concns are 0.2 mol/L, temperature maintains approximately 25 DEG C, stir 10 minutes with the rotating speeds of 800 revs/min, with 800 object filter screens, hollow glass micropearl is leached again, then use alcohol flushing 15 times, put into baking oven and be warming up to 60 DEG C, be incubated 1.5 hours to dry out solvent, after oven dry, obtaining slope of repose is the hollow glass micropearl powder of the good fluidity of 24.5 °.
Embodiment 10
50 grams of prepared T40 series high-performance hollow glass micropearl samples of Chinese Academy of Sciences's physics and chemistry are joined in the aqueous sodium hydroxide solution that 500 ml concns are 0.1 mol/L, temperature maintains approximately 25 DEG C, stir 20 minutes with the rotating speeds of 1000 revs/min, with 800 object filter screens, hollow glass micropearl is leached again, then use deionized water rinsing 5 times, put into baking oven and be warming up to 100 DEG C, be incubated 2.5 hours to dry out solvent, after oven dry, obtaining slope of repose is the hollow glass micropearl powder of the good fluidity of 23.5 °.
Embodiment 11
50 grams of prepared T40 series high-performance hollow glass micropearl samples of Chinese Academy of Sciences's physics and chemistry are joined in the potassium hydroxide aqueous solution that 500 ml concns are 0.5 mol/L, temperature maintains approximately 25 DEG C, stir 5 minutes with the rotating speeds of 600 revs/min, with 800 object filter screens, hollow glass micropearl is leached again, then use alcohol flushing 20 times, put into baking oven and be warming up to 80 DEG C, be incubated 2.5 hours to dry out solvent, after oven dry, obtaining slope of repose is the hollow glass micropearl powder of the good fluidity of 23 °.
Embodiment 12
50 grams of prepared T40 series high-performance hollow glass micropearl samples of Chinese Academy of Sciences's physics and chemistry are joined in the lithium hydroxide aqueous solution that 500 ml concns are 0.5 mol/L, temperature maintains approximately 25 DEG C, stir 10 minutes with the rotating speeds of 800 revs/min, with 800 object filter screens, hollow glass micropearl is leached again, then use washed with methanol 20 times, put into baking oven and be warming up to 50 DEG C, be incubated 2 hours to dry out solvent, after oven dry, obtaining slope of repose is the hollow glass micropearl powder of the good fluidity of 23.5 °.
Embodiment 13
In order to characterize the variation of hollow glass micropearl sample mobility before and after alkaline solution is processed, experiment is used powder general performance test to measure the slope of repose of hollow glass micropearl sample before and after basic solution is processed, and test result as shown in Table 1 and Table 2.T30 series high-performance hollow glass micropearl is after the alkaline solution described in embodiment 1 to 6 is processed as can be seen from Table 1, and its powder slope of repose has been reduced between 22.5 °-24.5 ° by 32.5 °; T40 series high-performance hollow glass micropearl is after the alkaline solution described in embodiment 7 to 12 is processed as can be seen from Table 2, and its powder slope of repose has been reduced between 23 °-24.5 ° by 33.5 °.This illustrates that selected T30 and T40 series high-performance hollow glass micropearl are after alkaline solution of the present invention is processed, and its mobility is all significantly improved.
Hollow glass micropearl is not caused to obvious corrasion in order to verify that alkaline solution in the present invention is processed, measuring the breakage rate under true density and the 12 MPa hydrostaticpressures of hollow glass micropearl sample before and after alkaline solution is processed, the results are shown in Table 1 and table 2.Can find out that from test result wherein T30 and T40 series hollow glass micropearl sample are after alkaline solution of the present invention is processed, the variation of their true density and breakage rate is all very little, and this illustrates that alkaline solution treating processes of the present invention does not cause the fragmentation of obvious hollow glass micropearl particle and the considerable change of hollow glass micropearl particle compressive strength.
Breakage rate before and after the processing of table 1 alkaline solution under the slope of repose of T30 series high-performance hollow glass micropearl powder, true density, 12 MPa hydrostaticpressures
Sample T30 Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6
Slope of repose (degree) 32.5° 24° 23° 23.5° 22.5° 24.5° 23.5°
True density (g/cm 3) 0.3035 0.3056 0.3064 0.3045 0.3048 0.3055 0.3054
Breakage rate (%) 17.2 16.5 16.2 16.7 16.6 16.9 16.1
Breakage rate before and after the processing of table 2 alkaline solution under the slope of repose of T40 series high-performance hollow glass micropearl powder, true density, 12 MPa hydrostaticpressures
Sample T40 Embodiment 7 Embodiment 8 Embodiment 9 Embodiment 10 Embodiment 11 Embodiment 12
Slope of repose (degree) 33.5° 23.5° 23° 24.5° 23.5° 23° 23.5°
True density (g/cm 3) 0.4064 0.4045 0.4055 0.4065 0.4058 0.4084 0.4075
Breakage rate (%) 5.1 4.5 4.7 4.4 4.6 4.2 4.3

Claims (5)

1. one kind is improved the method for hollow glass micropearl powder fluidity, it is characterized in that using that alkaline matter is soluble in water is mixed with certain density basic solution, hollow glass micropearl powder is joined in this basic solution, stir certain hour, filter, rinse post-drying, obtain the hollow glass micropearl powder of good fluidity.
2. the method for raising hollow glass micropearl powder fluidity according to claim 1, is characterized in that described alkaline matter is sodium hydroxide, lithium hydroxide, potassium hydroxide or calcium hydroxide; The volumetric molar concentration of the basic solution of preparation is 0.05~0.5 mol/L.
3. the method for raising hollow glass micropearl powder fluidity according to claim 1, is characterized in that described hollow glass micropearl powder being joined in this basic solution, and temperature maintains 20~30 DEG C, churning time 5~30 minutes.
4. the method for raising hollow glass micropearl powder fluidity according to claim 1, is characterized in that described rinse solvent is water, methyl alcohol, ethanol or acetone.
5. the method for raising hollow glass micropearl powder fluidity according to claim 1, is characterized in that described bake out temperature is 50~120 DEG C.
CN201410196965.2A 2014-05-12 2014-05-12 Method of improving fluidity of hollow glass bead powder Pending CN103964707A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108863092A (en) * 2018-08-30 2018-11-23 浙江省交通运输科学研究院 A kind of glass microballoon and preparation method thereof of self assembly surface layer microcellular structure
CN113502026A (en) * 2021-07-09 2021-10-15 山东鲁泰控股集团有限公司石墨烯高分子复合材料研发中心 Composition for light environment-friendly PVC pipe fitting and preparation method thereof

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Publication number Priority date Publication date Assignee Title
US4540629A (en) * 1982-04-08 1985-09-10 Pq Corporation Hollow microspheres with organosilicon-silicate walls
CN1097440A (en) * 1993-07-15 1995-01-18 张敬鳌 Metal coating material
CN101160266A (en) * 2005-02-24 2008-04-09 詹姆斯哈迪国际财金公司 Alkali resistant glass compositions
CN102381844A (en) * 2011-07-26 2012-03-21 西安工程大学 Method for modifying hollow glass microspheres by chemical precipitation process
CN102583973A (en) * 2012-03-06 2012-07-18 中国科学院理化技术研究所 Soft chemical preparation method for hollow glass micro-balloon, prepared hollow glass micro-balloon and application thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4540629A (en) * 1982-04-08 1985-09-10 Pq Corporation Hollow microspheres with organosilicon-silicate walls
CN1097440A (en) * 1993-07-15 1995-01-18 张敬鳌 Metal coating material
CN101160266A (en) * 2005-02-24 2008-04-09 詹姆斯哈迪国际财金公司 Alkali resistant glass compositions
CN102381844A (en) * 2011-07-26 2012-03-21 西安工程大学 Method for modifying hollow glass microspheres by chemical precipitation process
CN102583973A (en) * 2012-03-06 2012-07-18 中国科学院理化技术研究所 Soft chemical preparation method for hollow glass micro-balloon, prepared hollow glass micro-balloon and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108863092A (en) * 2018-08-30 2018-11-23 浙江省交通运输科学研究院 A kind of glass microballoon and preparation method thereof of self assembly surface layer microcellular structure
CN113502026A (en) * 2021-07-09 2021-10-15 山东鲁泰控股集团有限公司石墨烯高分子复合材料研发中心 Composition for light environment-friendly PVC pipe fitting and preparation method thereof

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