CN103101919A - Method for preparing ultrafine crystalline silica by using quartz tailings - Google Patents
Method for preparing ultrafine crystalline silica by using quartz tailings Download PDFInfo
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- CN103101919A CN103101919A CN2013100608436A CN201310060843A CN103101919A CN 103101919 A CN103101919 A CN 103101919A CN 2013100608436 A CN2013100608436 A CN 2013100608436A CN 201310060843 A CN201310060843 A CN 201310060843A CN 103101919 A CN103101919 A CN 103101919A
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Abstract
The invention relates to a method for preparing ultrafine crystalline silica by using quartz tailings. The method comprises steps of: (1) uniformly mixing quartz tailings and deionized water, stirring, filtering and discharging a filtrate; and (2) adding a grinding aid in the quartz tailings, conducting wet grinding to obtain a ground slurry, then washing to obtain a filter cake, and drying to a constant weight to obtain the ultrafine crystalline silica. The method has the advantages of simple operation, low cost and good repeatability, and is suitable for mass production. The excellent ultrafine crystalline silica prepared by the invention has particle size close to nanometer level, moisture content far less than the white carbon black, and a good prospect of application. The method provided by the invention changes waste into valuables by processing quartz tailings into a silicon micro powder, so as to reduce a problem of environmental pollution caused by discharge of quartz tailings.
Description
Technical field
The invention belongs to the preparation field of earth silicon material, particularly a kind of method of utilizing quartz tail sand to prepare ultra-fine powdered quartz.
Background technology
The annual quartz tail sand discharge capacity of China approximately has 1,000 ten thousand tons, and discharging is a large amount of quartz tail sands so, directly cause the adverse consequencess such as serious environmental pollution, cultivated land occupancy, river course reservoir silt up.For protection of the environment and take full advantage of Mineral resources, the comprehensive utilization of quartz tail sand becomes inexorable trend.The quartz tail sand composition is mainly SiO
2, further processing can prepare silicon powder.
Silicon powder is a kind of ultra tiny SiO
2Material is divided into two kinds of unformed and crystal types, is widely used in the fields such as electronic material, polymer composite, plastics, coating, rubber, pigment, pottery, tackiness agent, glass reinforced plastic, pharmaceutical carrier, makeup and anti-biotic material.Wherein, unformed SiO
2Namely be white carbon black, its surface with hydroxyl, is ultramicro powder, and particle diameter is generally 20～60nm, and specific surface area is large, is the present the highest a kind of superfine powdery material of output of large-scale industrial production in the world.Preparation method's comparative maturity, be generally two kinds of dry method and wet methods at present, and complex process needs specific installation, and production cost is high, also easily brings environmental pollution.And unformed SiO
2The adsorbed hydroxyl content is high, easily reunites, and therefore bad dispersibility is used and be subject to limitation.In recent years, crystal type SiO
2Material is low because of its adsorbed hydroxyl content, and dispersing property is better than unformed SiO
2And more and more come into one's own.Compare ultra-fine crystal type SiO with amorphous silica
2Material has following advantage: 1. cost is compared lowlyer with amorphous silica, and working condition is more easy to control, is fit to scale operation; 2. narrow particle size distribution, easily control, and is uniformly dispersed, and is difficult for reuniting; 3. water content is low, and surface hydroxyl is few; 4. purity is high, and impurity is few, more easily obtains the high-purity superfine powder.So crystal type nanometer SiO
2Become the upgrading type material of amorphous silica.
The silicon powder of conventional physical method preparation is generally all in micron level at present, and patent CN102070150A grinds quartz sand by grind grading, is easy to large-scale production, but the silica powder granularity is about 2 μ m.Other silicon powder of the following level of micron adds follow-up separating step on general basis of grinding, patent CN101659393 is by wet grinding, ultra-sonic dispersion, superfine grinding, the technique of centrifugation classification obtains super-fine silicon micro-powder, epigranular, but this method complex process, and in classification process, the super-fine silicon micro-powder proportion is little, cost is high, and efficient is low.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method of utilizing quartz tail sand to prepare ultra-fine powdered quartz, and the method has simple to operate, and cost is low, good reproducibility, mass producible characteristics; The present invention prepares good ultra-fine crystal formation silicon-dioxide, and particle diameter is near Nano grade, and water content has a good application prospect much smaller than white carbon black; The present invention is turned waste into wealth, and quartz tail sand is processed into silicon powder, has reduced the problem of environmental pollution that the quartz tail sand discharging causes.
A kind of method of utilizing quartz tail sand to prepare ultra-fine powdered quartz of the present invention comprises:
(1) quartz tail sand and deionized water are mixed, stir, filter, abandon filtrate;
(2) add grinding aid in above-mentioned quartz tail sand, carry out wet grinding, get the grinding disposed slurry, then washing is filtered, and obtains filter cake, is dried to constant weight, namely gets ultra-fine powdered quartz.
The mass ratio 1:3 of quartz tail sand and deionized water in described step (1), repeated washing 3-5 time.
In described step (1), churning time is 60-120min.
In described step (2), grinding aid is sodium laurylsulfonate or sodium oleate, and the amount of grinding aid is the 0.5-2% of quartz tail sand quality.
In described step (2), wet grinding device is the impact grinding of high energy nanometer.
In described step (2), the wet grinding time is 6-8h, and treatment capacity is 500g.
Washing in described step (2) is acid solution washing 2-3 time, and then deionized water wash is 3-4 time.
The acid solution washing be the hydrochloric acid soln of 0.1mol/L in described step (2), mixes stirring 1-2h, removal waste liquid with silica powder after grinding.
Drying temperature in described step (2) is 100-120 ℃.
In described step (2), the mean particle size of the ultra-fine powdered quartz of gained is of a size of 200 ± 30nm.
Beneficial effect
(1) the present invention has simple to operately, and cost is low, good reproducibility, mass producible characteristics;
(2) the present invention prepares good ultra-fine crystal formation earth silicon material, and granularity is near Nano grade, and water content has a good application prospect much smaller than white carbon black;
(3) the present invention is turned waste into wealth, and quartz tail sand is processed into silicon powder, has reduced the problem of environmental pollution that the quartz tail sand discharging causes.
Description of drawings
Fig. 1 is the process flow sheet of embodiment 1;
Fig. 2 is the X-ray diffractogram of the ultra-fine powdered quartz of embodiment 1 gained;
Fig. 3 is the TGA figure of the ultra-fine powdered quartz of embodiment 1 gained;
Fig. 4 is the N of the ultra-fine powdered quartz of embodiment 1 gained
2Adsorption curve figure;
Fig. 5 is the TEM figure of the ultra-fine powdered quartz of embodiment 1 gained;
Fig. 6 is the TEM figure of the ultra-fine powdered quartz of embodiment 1 gained;
Fig. 7 is the TEM figure of the ultra-fine powdered quartz of embodiment 1 gained.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
(1) quartz tail sand pre-treatment: get the 500g quartz tail sand, press quartz tail sand: deionized water quality ratio=1:3 mixes, and mechanical stirring washing 60min filters, and abandons waste liquid, washs as stated above three times.
(2) grind: adding massfraction in the quartz tail sand that washing is completed is 1% sodium laurylsulfonate, with high energy nanometer impact grinding wet grinding 6h, gets the slip after grinding.
(3) washing: the 0.1mol/L hydrochloric acid soln washed twice of the slip after grinding, deionized water wash three times filters to get filter cake.
(4) drying: filter cake is dried to constant weight under 110 ℃ of conditions in air dry oven, namely gets ultra-fine crystal formation earth silicon material.
The transmission electron microscope picture of the superfine silicon dioxide material that scheme 1 makes is seen Fig. 5, and the median size that is estimated particle by figure is about 220nm.The X ray diffracting spectrum of sample is seen Fig. 2, calculates size and the TEM picture gained sizableness of gained by the Scherrer formula.The TGA figure of sample sees Fig. 3, and percentage of water loss is in 1.5%.The N of sample
2Adsorption curve figure sees Fig. 4, and the BET specific surface area is 15m
2/ g.
Embodiment 2
(1) quartz tail sand pre-treatment: get the 500g quartz tail sand, press quartz tail sand: deionized water quality ratio=1:3 mixes, and mechanical stirring washing 60min filters, and abandons waste liquid, washs as stated above three times.
(2) grind: adding massfraction in the quartz tail sand that washing is completed is 1% sodium laurylsulfonate, with high energy nanometer impact grinding wet grinding 7h, gets the slip after grinding.
(3) washing: the 0.1mol/L hydrochloric acid soln washed twice of the slip after grinding, deionized water wash three times filters to get filter cake.
(4) drying: filter cake is dried to constant weight under 110 ℃ of conditions in air dry oven, namely gets ultra-fine crystal formation earth silicon material.
The transmission electron microscope picture of the superfine silicon dioxide material that scheme 2 makes is seen Fig. 6, and the median size that is estimated particle by figure is about 200nm.
Embodiment 3
(1) quartz tail sand pre-treatment: get the 500g quartz tail sand, press quartz tail sand: deionized water quality ratio=1:3 mixes, and mechanical stirring washing 60min filters, and abandons waste liquid, washs as stated above three times.
(2) grind: adding massfraction in the quartz tail sand that washing is completed is 1% sodium laurylsulfonate, with high energy nanometer impact grinding wet grinding 8h, gets the slip after grinding.
(3) washing: the 0.1mol/L hydrochloric acid soln washed twice of the slip after grinding, deionized water wash three times filters to get filter cake.
(4) drying: filter cake is dried to constant weight under 110 ℃ of conditions in air dry oven, namely gets ultra-fine crystal formation earth silicon material.
The transmission electron microscope picture of the superfine silicon dioxide material that scheme 3 makes is seen Fig. 7, and the median size that is estimated particle by figure is about 180nm.
Claims (10)
1. method of utilizing quartz tail sand to prepare ultra-fine powdered quartz comprises:
(1) quartz tail sand and deionized water are mixed, stir, filter, abandon filtrate;
(2) add grinding aid in above-mentioned quartz tail sand, carry out wet grinding, get the grinding disposed slurry, then washing is filtered, and obtains filter cake, is dried to constant weight, namely gets ultra-fine powdered quartz.
2. a kind of method of utilizing quartz tail sand to prepare ultra-fine powdered quartz according to claim 1 is characterized in that:
The mass ratio 1:3 of quartz tail sand and deionized water in described step (1), repeated washing 3-5 time.
3. a kind of method of utilizing quartz tail sand to prepare ultra-fine powdered quartz according to claim 2 is characterized in that:
In described step (1), churning time is 60-120min.
4. a kind of method of utilizing quartz tail sand to prepare ultra-fine powdered quartz according to claim 1 is characterized in that:
In described step (2), grinding aid is sodium laurylsulfonate or sodium oleate, and the amount of grinding aid is the 0.5-2% of quartz tail sand quality.
5. a kind of method of utilizing quartz tail sand to prepare ultra-fine powdered quartz according to claim 1 is characterized in that:
In described step (2), wet grinding device is the impact grinding of high energy nanometer.
6. a kind of method of utilizing quartz tail sand to prepare ultra-fine powdered quartz according to claim 1 is characterized in that:
In described step (2), the wet grinding time is 6-8h.
7. a kind of method of utilizing quartz tail sand to prepare ultra-fine powdered quartz according to claim 1 is characterized in that:
Washing in described step (2) is acid solution washing 2-3 time, and then deionized water wash is 3-4 time.
8. a kind of method of utilizing quartz tail sand to prepare ultra-fine powdered quartz according to claim 7 is characterized in that:
The acid solution washing be the hydrochloric acid soln of 0.1mol/L in described step (2), mixes stirring 1-2h, removal waste liquid with silica powder after grinding.
9. a kind of method of utilizing quartz tail sand to prepare ultra-fine powdered quartz according to claim 1 is characterized in that:
Drying temperature in described step (2) is 100-120 ℃.
10. a kind of method of utilizing quartz tail sand to prepare ultra-fine powdered quartz according to claim 1 is characterized in that:
In described step (2), the mean particle size of the ultra-fine powdered quartz of gained is of a size of 200 ± 30nm.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104925818A (en) * | 2015-07-13 | 2015-09-23 | 田辉明 | High-purity quartz powder producing technology and device utilizing quartz mill tailings |
| CN107597301A (en) * | 2017-09-08 | 2018-01-19 | 芜湖悠派护理用品科技股份有限公司 | A kind of zeolite grinds preprocess method |
| CN108249450A (en) * | 2018-01-19 | 2018-07-06 | 华南理工大学 | A kind of method that chemolysis auxiliary mechanical lapping prepares spherical ultra-fine quartz particles |
| CN109135346A (en) * | 2018-09-05 | 2019-01-04 | 中建材蚌埠玻璃工业设计研究院有限公司 | Modified silicon powder of a kind of high pure and ultra-fine and preparation method thereof |
| CN112374504A (en) * | 2020-11-05 | 2021-02-19 | 黄运雷 | Process for manufacturing nano silicon dioxide by physical method |
| CN113416592A (en) * | 2021-05-24 | 2021-09-21 | 广西大学 | Preparation method of hydrophilic corn insulating oil modified by nano magnesium oxide |
Citations (1)
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| CN102674376A (en) * | 2012-04-19 | 2012-09-19 | 田辉明 | Production method of quartz tailing purification |
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2013
- 2013-02-27 CN CN2013100608436A patent/CN103101919A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102674376A (en) * | 2012-04-19 | 2012-09-19 | 田辉明 | Production method of quartz tailing purification |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104925818A (en) * | 2015-07-13 | 2015-09-23 | 田辉明 | High-purity quartz powder producing technology and device utilizing quartz mill tailings |
| CN104925818B (en) * | 2015-07-13 | 2017-01-25 | 黄冈师范学院 | High-purity quartz powder producing technology and device utilizing quartz mill tailings |
| CN107597301A (en) * | 2017-09-08 | 2018-01-19 | 芜湖悠派护理用品科技股份有限公司 | A kind of zeolite grinds preprocess method |
| CN108249450A (en) * | 2018-01-19 | 2018-07-06 | 华南理工大学 | A kind of method that chemolysis auxiliary mechanical lapping prepares spherical ultra-fine quartz particles |
| CN109135346A (en) * | 2018-09-05 | 2019-01-04 | 中建材蚌埠玻璃工业设计研究院有限公司 | Modified silicon powder of a kind of high pure and ultra-fine and preparation method thereof |
| CN112374504A (en) * | 2020-11-05 | 2021-02-19 | 黄运雷 | Process for manufacturing nano silicon dioxide by physical method |
| CN112374504B (en) * | 2020-11-05 | 2023-01-24 | 黄运雷 | Process for manufacturing nano silicon dioxide by physical method |
| CN113416592A (en) * | 2021-05-24 | 2021-09-21 | 广西大学 | Preparation method of hydrophilic corn insulating oil modified by nano magnesium oxide |
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Application publication date: 20130515 |