CN104860324A - Method for controlling dispersion particle size of fumed silica - Google Patents
Method for controlling dispersion particle size of fumed silica Download PDFInfo
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- CN104860324A CN104860324A CN201510241684.9A CN201510241684A CN104860324A CN 104860324 A CN104860324 A CN 104860324A CN 201510241684 A CN201510241684 A CN 201510241684A CN 104860324 A CN104860324 A CN 104860324A
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Abstract
The invention discloses a method for controlling dispersion particle size of fumed silica. Commercial fumed silica is prepared into an aqueous solution with concentration which is 4wt%-25wt%; the aqueous solution is sheared for 1-15 min at the shearing linear velocity of 9.64m/s-27m/s; or the aqueous solution is ultrasonically dispersed for 1-15 min under the ultrasonic powder of 9.5-950W. On the premise that the concentration of the commercial fumed silica is 4wt%-25wt%, shearing force, ultrasonic force, dispersion time and concentration of fumed silica and the like are comprehensively utilized to realize dispersion of the commercial fumed silica and effective control of the particle size; the dispersion particle size of the fumed silica is controlled to be 130-240 nm.
Description
Technical field
The invention belongs to the preparation field of chemical power source material, be specifically related to a kind of method controlling aerosil dispersion particle diameter.
Background technology
The gelation of sulfuric acid electrolyte is the important development direction of analysing valve control type lead-acid accumulator battery, and application aerosil is the first-selection of current each store battery producer as jelling agent.Aerosil has very high chemical purity and very strong thixotropy, and it obtains primary particles by combustion and pyrolysis silane in oxyhydrogen flame, and particulate becomes containing 10 through perikinetic aggregation
4individual or more high number SiO
4a shape primary particle of unit, in process of cooling, these primary particles define aggregate, are combined into larger aggregate again after aggregate surface sclerosis through Van der Waals force, and this is the pattern that commodity aerosil presents usually.Through shearing or shear the dispersed particle that combination of ultrasound can only obtain a certain size, dispersion particle diameter difference determines the difference of particle surface silicone hydroxyl kind and quantity, therefore strongly have impact on the gelling characteristic of aerosil and the battery performance after adding store battery, control first committed step that aerosil dispersion particle diameter becomes the excellent colloid storage battery of processability.
Importance about aerosil particle diameter is realized already (Gen ten, M. etc.,
j Solid State Electrochem.2014,18,2469 – 2479; Chen, M. etc.,
electrochimica Acta2015,164,243 – 251; Chen, M. etc.,
j. Power Sources2008,181,161-171; Kamiya, H. etc.,
j. Am. Ceram. Soc.2000,83,287-293), but they be all according to Electronic Speculum shooting primary partical or primary particle consider these unit size (10-50nm) (Park, J. etc.,
j. Non-Crystalline Solids2005,351,2352 – 2357; Sun, C. etc.,
applied Mechanics Materials2012,110-116,514-518; Chen, M. etc.,
j. Power Sources2008,181,161-171; Kamiya, H. etc.,
j. Am. Ceram. Soc.2000,83,287-293).This does not seriously conform to practical application, because commodity aerosil can only destroy the Van der Waals force be bonded to each other through mechanical force, namely dispersion can only obtain aggregate as above, and particle diameter is at this moment between 100-300nm.The disconnection of this theory and practice causes not having clear and definite knowledge to instruct so far to the pre-treating technology of this key of dispersion, has a strong impact on the practical application even hindering aerosil.
The present invention in depth studies through system, determine on the important factor basis of commodity aerosils effect at clear and definite mechanical dispersion particle diameter, summarize the means such as comprehensive utilization shearing force, ultrasonic force, jitter time, aerosil concentration, the dispersion to commodity aerosil and the effective control to particle diameter can be realized.
Summary of the invention
The invention reside in for the deficiencies in the prior art, a kind of method that effectively can control aerosil dispersion particle diameter is provided.The method is when to be mixed with concentration be the aqueous solution of 4wt% ~ 25wt% to commodity aerosil, and comprehensive utilization shearing force, ultrasonic force, jitter time etc., effectively can control the dispersion particle diameter of aerosil at 130nm ~ 240nm.
For achieving the above object, the present invention adopts following technical scheme:
Control the method for aerosil dispersion particle diameter: commodity aerosil is mixed with the aqueous solution that concentration is 4wt% ~ 25wt%, under shear line speed is 9.64 m/s ~ 27 m/s, shears 1 minute ~ 15 minutes; Or again under ultrasonic power is 9.5W ~ 950W, ultrasonic disperse 1 minute ~ 15 minutes; Obtained dispersion size controlling 130nm ~ 240nm(particles distribution instrument measure and through the process of concentration extrapotation) aerosil.
The application adopts the high-speed shearing machine that is made up of stators and rotators or clarifixator to shear.
The application adopts the ultrasonic grinder be made up of ultra-sonic generator to carry out ultrasonic disperse.
The present invention fully utilizes the means such as shearing force, ultrasonic force, jitter time, aerosil concentration, be used alone shearing force or conbined usage to shear and ultrasonic force, choose reasonable aerosil concentration, in described jitter time, the dispersion particle diameter of aerosil can be controlled well at 130nm ~ 240nm.
Condition test:
1) silica concentration change is on the impact of aerosil dispersion particle diameter
Weighing concentration is respectively the aqueous silica solution of 4wt% ~ 25wt%, and fixed shear linear velocity is under 15.5 m/s, shears 3 minutes.The dispersion particle diameter of aerosil with aerosil concentration change as shown in Figure 1.Along with aerosil concentration increases, dispersion particle diameter reduces.
2) change of shear line speed is on the impact of the dispersion particle diameter of aerosil
Weighing concentration is the aqueous silica solution of 15wt%, and fixed shear linear velocity is under 12 ~ 24 m/s respectively, shears 3 minutes.The dispersion particle diameter of aerosil with shear line speed change as shown in Figure 2.Along with shear line speed increases, aerosil dispersion particle diameter reduces.
3) change of shear time is on the impact of the dispersion particle diameter of aerosil
Weighing concentration is the aqueous silica solution of 15wt%, and fixed shear linear velocity is under 15.5 m/s, shears 3 ~ 15 minutes respectively.The dispersion particle diameter of aerosil with shear time change as shown in Figure 3.Along with shear time increases, aerosil dispersion particle diameter slightly reduces.
4) change of ultrasonic time is on the impact of the dispersion particle diameter of aerosil
Weighing concentration is the aqueous silica solution of 15wt%, under fixed shear linear velocity is 15.5 m/s, shears after 3 minutes, then combining ultrasonic dispersion, ultrasonic 1 ~ 9 minute of difference under 665W power.The dispersion particle diameter of aerosil with ultrasonic time change as shown in Figure 4.Along with ultrasonic time increases, aerosil dispersion particle diameter reduces.Can obtain under ultrasound condition than shearing less aerosil dispersion particle diameter.
5) change of ultrasonic power is on the impact of the dispersion particle diameter of aerosil
Weighing concentration is the aqueous silica solution of 15wt%, under fixed shear linear velocity is 15.5 m/s, shears after 3 minutes, then combining ultrasonic dispersion, and fixing ultrasonic power is respectively under 450W ~ 900W, ultrasonic 5 minutes.The dispersion particle diameter of aerosil with ultrasonic power change as shown in Figure 5.Along with ultrasonic power increases, aerosil dispersion particle diameter slightly reduces.
remarkable advantage of the present invention is:
(1) the present invention on purpose improves the pre-treating technology of commodity aerosil, the means such as comprehensive utilization shearing force, ultrasonic force, jitter time, aerosil concentration, achieve effective control of the dispersion particle diameter to silicon-dioxide, thus greatly affect jelling agent character and colloid battery performance;
(2) concentration by strengthening aerosil increases interparticle collision, thus obtains less particle diameter, and this method does not increase production cost, only changes concentration conditions simply, just can obtain good additional dispersion effect, possess progress significantly.
Accompanying drawing explanation
Fig. 1 is fixed shear linear velocity is 15.5 m/s, and under shearing 3 minutes conditions, aerosil concentration is on the impact of dispersion particle diameter;
Fig. 2 is fixed air aerosil concentration is 15.0wt%, and under shearing 3 minutes conditions, shear line speed is on the impact of dispersion particle diameter;
Fig. 3 is fixed air aerosil concentration is 15.0wt%, and shear line speed is under 15.5 m/s conditions, and shear time is on the impact of dispersion particle diameter;
Fig. 4 is fixed air aerosil concentration is 15.0wt%, and shear line speed is 15.5 m/s down cuts after 3 minutes, then fixes ultrasonic disperse under 665W power, and ultrasonic time is on the impact of dispersion particle diameter;
Fig. 5 is fixed air aerosil concentration is 15.0wt%, and shear line speed is 15.5 m/s down cuts after 3 minutes, then ultrasonic disperse is under 5 minutes, and ultrasonic power is on the impact of dispersion particle diameter.
Embodiment
The present invention's the following example further illustrates the present invention, but protection scope of the present invention is not limited to the following example.
embodiment 1
Commodity aerosil being mixed with concentration is the 4wt% aqueous solution, and under shear line speed is 9.64 m/s, shear 1 minute, the dispersion particle diameter of the aerosil after process is 240 ± 5 nm.
embodiment 2
Commodity aerosil being mixed with concentration is the 20wt% aqueous solution, and under shear line speed is 27 m/s, shear 10 minutes, the dispersion particle diameter of the aerosil after process is 150 ± 3 nm.
embodiment 3
Commodity aerosil being mixed with concentration is the 15.0wt% aqueous solution, under shear line speed is 15.5m/s, shears after 3 minutes; Again under ultrasonic power is 855W, ultrasonic disperse 5 minutes, the dispersion particle diameter of the aerosil after process is 130 ± 2 nm.
The foregoing is only a part of embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (3)
1. control a method for aerosil dispersion particle diameter, it is characterized in that: commodity aerosil is mixed with the aqueous solution that concentration is 4wt% ~ 25wt%, under shear line speed is 9.64 m/s ~ 27 m/s, shear 1 minute ~ 15 minutes; Or again under ultrasonic power is 9.5W ~ 950W, ultrasonic disperse 1 minute ~ 15 minutes; Obtained dispersion size controlling is at the aerosil of 130nm ~ 240nm.
2. the method for control aerosil according to claim 1 dispersion particle diameter, is characterized in that: adopt the high-speed shearing machine that is made up of stators and rotators or clarifixator to shear.
3. the method for control aerosil dispersion particle diameter according to claim 1, is characterized in that: adopt the ultrasonic grinder be made up of ultra-sonic generator to carry out ultrasonic disperse.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510241684.9A CN104860324A (en) | 2015-05-13 | 2015-05-13 | Method for controlling dispersion particle size of fumed silica |
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| CN201510241684.9A CN104860324A (en) | 2015-05-13 | 2015-05-13 | Method for controlling dispersion particle size of fumed silica |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106356570A (en) * | 2016-09-27 | 2017-01-25 | 天能电池集团有限公司 | Preparation method of colloid mother solution for lead storage battery |
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| CN103280602A (en) * | 2013-05-08 | 2013-09-04 | 超威电源有限公司 | Colloidal electrolyte for lead-acid storage battery and preparation method of colloidal electrolyte |
| CN103969157A (en) * | 2014-05-29 | 2014-08-06 | 福州大学 | Method of testing gel time of gelled electrolyte |
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2015
- 2015-05-13 CN CN201510241684.9A patent/CN104860324A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103280602A (en) * | 2013-05-08 | 2013-09-04 | 超威电源有限公司 | Colloidal electrolyte for lead-acid storage battery and preparation method of colloidal electrolyte |
| CN103969157A (en) * | 2014-05-29 | 2014-08-06 | 福州大学 | Method of testing gel time of gelled electrolyte |
Non-Patent Citations (1)
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| 孙小祥等: "不同制备条件下气相二氧化硅胶体电解液的性能研究", 《中国化学会第十三届胶体与界面化学会议论文摘要集》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106356570A (en) * | 2016-09-27 | 2017-01-25 | 天能电池集团有限公司 | Preparation method of colloid mother solution for lead storage battery |
| CN106356570B (en) * | 2016-09-27 | 2019-06-25 | 天能电池集团有限公司 | A kind of preparation method of lead storage battery colloid mother liquor |
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Application publication date: 20150826 |