CN111807375B - Preparation of nano silicon dioxide by impact flow - Google Patents
Preparation of nano silicon dioxide by impact flow Download PDFInfo
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- CN111807375B CN111807375B CN202010632834.XA CN202010632834A CN111807375B CN 111807375 B CN111807375 B CN 111807375B CN 202010632834 A CN202010632834 A CN 202010632834A CN 111807375 B CN111807375 B CN 111807375B
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- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention provides a preparation method for preparing nano silicon dioxide by an impinging stream method, which comprises the following steps: (1) preparing silicon dioxide colloid into silicon dioxide emulsion; (2) placing the silicon dioxide emulsion in a high-pressure jet device for spraying, forming a turbulent fluid system after spraying to form nano atomized liquid drops, and simultaneously starting freezing airflow to purge the nano atomized liquid drops to quickly solidify the formed nano liquid drops; (3) and collecting the cured nano silicon dioxide product, and heating to normal temperature and normal pressure under reduced pressure to obtain the final nano silicon dioxide product. The impact flow method for preparing the nano silicon dioxide has low cost and simple operation, greatly improves the product quality and yield, can accurately control the water content in the product, and is beneficial to industrial production.
Description
Technical Field
The invention relates to the technical field of nano-silica preparation, in particular to a method for preparing nano-silica by adopting an impinging stream method and a preparation method thereof.
Background
Silica has an irreplaceable role in industrial applications. The silicon dioxide is amorphous powder, has excellent reinforcing property, stability, thixotropy and thickening property due to high activity of the silicon dioxide, and is widely applied to various industries such as rubber, plastics, paint, medicine, daily chemical industry and the like. The high-quality silicon dioxide is mainly produced by a gas phase method at present, and the process is monopolized by foreign production of giant degussel, cabot, mountain de. Because the production process of the fumed silica is complex, the cost is high, the conditions are harsh, although enterprises can produce fumed silica products in China, the fumed silica cannot be produced in large scale due to various technical and equipment requirements, and meanwhile, the quality of the fumed silica in China has a great gap with the quality of like products in China. Therefore, the precipitation method is still the main technique in the field of silica production in China.
The preparation process of the silicon dioxide by the precipitation method is simple and low in required cost, but the nano-scale product cannot be produced due to the limitation of the production method. In order to obtain excellent performances which are comparable to the performance, more domestic researches are focused on the technical modification of precipitated silica products. The modification method mainly has two directions: firstly, adding a surfactant to modify the hydroxyl on the surface of the white carbon black; the other method is to carbonize the surface of the white carbon black to obtain high dispersion and hydrophobic property. Because other substances are added in the modification, the finally formed product deviates from the normal property of the silicon dioxide, and can only be exclusively applied to a special field, and the application of the silicon dioxide is limited in some aspects. A patent of modifying carbon-coated silica surface such as a patent of modifying carbon-coated silica surface by coating carbon nanotubes on silica surface introduced in patent CN105836749, a patent of modifying silica surface hydroxyl by using a surfactant and a polymer material reported in patent CN110746794, and the like; a few scientific research units are involved in the improvement of the production mode, for example, the production process adopts a method of adding a surfactant to reduce the influence of metal ions, such as adding surfactant sodium dodecyl benzene sulfonate, polyethylene glycol 6000 and the like in the production process mentioned in the thesis of controllable preparation and application of nano white carbon black of beijing university of chemical industry. However, the introduction of the added surfactant is easy to cause secondary pollution in the production process. Therefore, the research of preparing the micro-nano silicon dioxide by adopting a new technology in the process of preparing the silicon dioxide by a precipitation method has great production value.
The impinging stream technique was first proposed by Elperin and was subsequently greatly developed in Tamir research. The fluids colliding with each other not only have large relative movement speed, but also can generate a mixing area with high turbulent motion intensity at the collision position, so that the mixing intensity and the mass transfer coefficient of the impinging stream equipment are far beyond those of the traditional chemical equipment. Through research for many years, the impinging stream technology is applied to various fields such as powder drying, gas absorption, liquid-liquid extraction, particle preparation and the like. In industrial application, the impinging stream equipment has the advantages of simple structure, convenient operation and wide application prospect. The principle is that two opposite phase fluids collide at high speed, so that a high-speed turbulent collision region is formed between the accelerating tubes, the axial speed of the fluid on a collision surface approaches zero and is converted into radial flow, particles can penetrate into the opposite flow continuously and reach a maximum value at the moment of starting penetration, and then the energy is dispersed from the maximum size to the minimum size through the formation, interaction and extinction of vortexes under the action of turbulence. In brief, the ordered fluid flow forms individual vortices which interact with each other to split into smaller vortices, and the smaller vortices then continue to interact with each other, and so on, which has the advantages of continuously radiating energy points to the inside of the material in an all-round and three-dimensional manner, continuously cascading, no energy is concentrated at a certain point in space, and the existence of turbulence enables mechanical energy, chemical energy or other forms of energy to be fully applied to the microscopic size, so as to realize the internal transfer of energy. The turbulent bed invented in patent CN107720869 fully utilizes the principle of turbulence energy cascade dispersion, and the prepared turbulent bed has smaller volume and higher treatment efficiency; the patent CN209849102 discloses a forced turbulent mineralization reaction device, which utilizes a turbulent generator to generate turbulent flow, and converts mechanical energy into forced shearing force, thereby improving the efficiency of flotation mineralization reaction; the turbulence generating structure disclosed in patent CN209663879 gives full play to the advantages of turbulence, improves the utilization rate of energy, and is safe and fast. It has been proved that impinging stream is one of the most effective methods for strengthening the phase-to-phase transfer, especially the outer diffusion transfer process, and the transfer coefficient can be improved by several times to dozens of times compared with the common method, and the characteristic is in general concern. In recent years, the use of this characteristic for the preparation of ultrafine powders and the like has shown great potential applications, and research in this field is rapidly growing.
At present, in the prior art, a precipitation method-impinging stream reaction is adopted to prepare silicon dioxide with smaller particle size, sodium silicate and sulfuric acid are usually directly added into an impinging stream reactor to prepare the silicon dioxide through reaction in the impinging stream reactor, and the silicon dioxide prepared by the method has the advantages of difficult particle size reaching the nanometer level, easy agglomeration and uneven particle size distribution.
In the prior art, CN103588210A provides a method for preparing nano-silica, which comprises adding solution a (or solution B) into an impinging stream reactor, adjusting the pH value to 4-10 with solution B (or solution a), suction-filtering, washing the filter cake with washing solution C, drying, and calcining to obtain nano-silica. Wherein: a is a solution of a silicon-containing compound, a surfactant, alcohols and water; b is a solution containing an acidifying agent, alcohols and water; c is a solution containing alcohol or acetone or the combination thereof, a surfactant and water. According to the invention, the nano silicon dioxide is prepared by carrying out chemical reaction in the impinging stream reactor, the crude product is dried by blowing air and is calcined in the muffle furnace, and the silicon dioxide with the particle size of 40-90nm is prepared, but the silicon dioxide prepared by the method is easy to agglomerate and uneven in particle size distribution, and various surfactants are added, so that secondary pollution in the production process is easily caused, and the operation flow is complex.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
In order to solve the problem that the precipitation method can not prepare the nano-scale silicon dioxide, impinging stream is introduced into production, energy is dispersed and exerted to the maximum through the action of shearing force, micro liquid drops are formed through continuous shearing, and cascade energy finally reaches the preparation condition of nano-scale silicon dioxide particles. The invention adopts an impinging stream method to atomize the silica emulsion into liquid drops on the basis of preparing silica colloid by a precipitation method, simultaneously introduces liquefied carbon dioxide to carry out purging separation, and finally prepares a nano-grade silica product after decompression and temperature rise. The operation flow is shown in fig. 1.
The problem solved by the invention is realized by the following steps:
the invention provides a preparation method for preparing nano silicon dioxide by an impinging stream method, which comprises the following steps:
(1) preparing silicon dioxide colloid into silicon dioxide emulsion;
(2) placing the silicon dioxide emulsion in a high-pressure jet device for spraying, forming a turbulent fluid system after spraying to form nano atomized liquid drops, and simultaneously starting freezing airflow to purge the nano atomized liquid drops to quickly solidify the formed nano liquid drops;
(3) collecting the solidified nano particles, and obtaining the nano silicon dioxide after reducing pressure and raising temperature to normal temperature and normal pressure.
In the invention, turbulent cascade energy transfer is utilized to convert kinetic energy of the silicon dioxide dilute solution into shearing force to continuously act on silicon dioxide liquid drops, energy is dispersed in a cascade mode to form nano-scale liquid drops, and the nano-silicon dioxide is rapidly cooled and solidified into solid particles under the blowing of freezing airflow to finally prepare the nano-silicon dioxide.
In some embodiments of the present invention, in the step (1), the conductivity of the silica colloid is 0.5-5 us/cm. If the conductivity of the adopted silicon dioxide colloid is too large, the prepared nano silicon dioxide has non-uniform particle size distribution and wider particle size distribution.
In some embodiments of the invention, in step (1), the silica emulsion has a concentration of 3-15% (w/w).
In some embodiments of the invention, the high-pressure fluidic device comprises two high-pressure lance heads, the high-pressure lance heads being 180 °.
In some embodiments of the invention, the high-pressure jet apparatus comprises three high-pressure lance tips at 120 °.
In some embodiments of the invention, the mouth diameter of the lance tip is 1-2mm and the distance between the mouths is 1-4 mm.
In some embodiments of the invention, the high pressure fluidic device has an injection pressure of 1-15 MPa.
In some embodiments of the invention, the refrigerated gas stream is liquid carbon dioxide.
In some embodiments of the invention, the liquid carbon dioxide temperature is from-40 ℃ to 60 ℃.
In some embodiments of the invention, the chilled gas stream purge pressure is 1 to 10 MPa.
Compared with the prior art, the invention has the advantages that:
(1) the method is characterized in that a precipitation method is utilized to prepare silica colloid, turbulent cascade energy transfer is utilized to convert the kinetic energy of silica emulsion into shearing force to continuously act on silica droplets, energy is dispersed in a cascade manner to form nano-scale droplets, a nano-silica product is finally prepared under the sweeping of freezing airflow, impinging flow can produce nano-scale silica, and the cost, equipment, process flow requirements and the like are greatly reduced compared with those of a gas phase method.
(2) The nano silicon dioxide prepared by the invention has small particle size, uniform particle size, narrower particle size distribution and easily controlled size, is quickly cured under the blowing of freezing airflow and is not easy to agglomerate.
(3) The production operation of the invention is simple and safe, and is easy to control.
(4) The product quality and yield are greatly improved, the water content in the product can be accurately controlled, other substances are not introduced, and the product purity is high.
Drawings
FIG. 1 is a process flow diagram of the impinging stream method for preparing nano-silica;
FIG. 2 is a schematic view of a lance head of the high pressure fluidic apparatus;
FIG. 3 is a schematic diagram of the normal-impact correlation of two high-pressure gun heads of the high-pressure jet device;
FIG. 4 is a schematic view of the high-pressure jet device for evenly dividing and oppositely jetting three high-pressure gun heads;
FIG. 5 is a transmission electron micrograph of the nano-silica prepared in example 3 of the present invention.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The present invention is further illustrated by the following examples, but the embodiments of the invention are not limited to the following examples, and equivalent variations or modifications of the method according to the present invention should be considered within the scope of the present invention.
Example 1
Adding water into silica colloid with the conductivity of 1us/cm to prepare 3% silica emulsion, and uniformly stirring. And transferring the uniformly stirred silicon dioxide emulsion into high-pressure jet devices of two high-pressure gun heads, and controlling the jet pressure to be 1MPa, the distance between the gun heads to be 1mm and the caliber to be 2 mm. And opening a gun head switch to jet the two silicon dioxide emulsions. During the opposite injection, the gun head rifling makes the jet flow be injected in a spiral shape, the impulse is increased, the two spiral jet flows are collided and then subjected to energy conversion, and the two liquid flows are emitted outwards in a turbulent flow mode to form atomized nano liquid drops. And simultaneously starting liquid carbon dioxide to purge and atomize the nano liquid drops, wherein the temperature of the liquid carbon dioxide is-40 ℃, the purging pressure is 1MPa, so that the formed nano liquid drops are rapidly solidified, collecting the solidified nano silicon dioxide product, and reducing the pressure and raising the temperature to normal temperature and normal pressure to obtain the final nano silicon dioxide product with the particle size range of 19-27 nm. The water content was 24%.
Example 2
Adding water into silica colloid with conductivity of 5us/cm to prepare 10% silica emulsion, and stirring uniformly. And transferring the uniformly stirred silicon dioxide emulsion into high-pressure jet devices of two high-pressure gun heads, and controlling the jet pressure to be 3MPa, the distance between the gun heads to be 2mm and the caliber to be 1 mm. And opening a gun head switch to jet the two silicon dioxide emulsions. During the opposite injection, the gun head rifling makes the jet flow be injected in a spiral shape, the impulse is increased, the two spiral jet flows are collided and then subjected to energy conversion, and the two liquid flows are emitted outwards in a turbulent flow mode to form atomized nano liquid drops. And simultaneously starting liquid carbon dioxide to purge and atomize the nano liquid drops, wherein the temperature of the liquid carbon dioxide is-50 ℃, the purging pressure is 2MPa, so that the formed nano liquid drops are rapidly solidified, collecting the solidified nano silicon dioxide product, and reducing the pressure and raising the temperature to normal temperature and normal pressure to obtain the final nano silicon dioxide product, wherein the particle size range is 30-37nm, and the water content is 22%.
Example 3
Adding water into silica colloid with conductivity of 5us/cm to prepare 15% silica emulsion, and stirring uniformly. And transferring the uniformly stirred silicon dioxide emulsion into high-pressure jet devices of two high-pressure gun heads, and controlling the spraying pressure to be 5MPa, the distance between the gun heads to be 2mm and the caliber to be 1.5 mm. And opening a gun head switch to jet the two silicon dioxide emulsions. During the opposite injection, the gun head rifling makes the jet flow be injected in a spiral shape, the impulse is increased, the two spiral jet flows are collided and then subjected to energy conversion, and the two liquid flows are emitted outwards in a turbulent flow mode to form atomized nano liquid drops. And simultaneously starting liquid carbon dioxide to purge and atomize the nano liquid drops, wherein the temperature of the liquid carbon dioxide is-40 ℃, the purging pressure is 3MPa, so that the formed nano liquid drops are rapidly solidified, collecting the solidified nano silicon dioxide product, and reducing the pressure and raising the temperature to normal temperature and normal pressure to obtain the final nano silicon dioxide product, wherein the particle size range is 20-25nm, and the water content is 19%.
Example 4
Adding water into silica colloid with conductivity of 0.5us/cm to prepare 8% silica emulsion, and stirring well. And transferring the uniformly stirred silicon dioxide emulsion into high-pressure jet devices of three high-pressure gun heads, and controlling the spraying pressure to be 2MPa, the distance between the gun heads to be 4mm and the caliber to be 2 mm. And opening a gun head switch to spray the three strands of silicon dioxide emulsion. During the opposite injection, the gun head rifling makes the jet flow be injected in a spiral shape, the impulse is increased, the three strands of spiral jet flows are subjected to energy conversion after collision, and the three strands of liquid are emitted outwards in a turbulent flow mode to form atomized nano liquid drops. And simultaneously starting liquid carbon dioxide to purge and atomize the nano liquid drops, wherein the temperature of the liquid carbon dioxide is-60 ℃, the purging pressure is 5MPa, so that the formed nano liquid drops are rapidly solidified, collecting the solidified nano silicon dioxide product, and reducing the pressure and raising the temperature to normal temperature and normal pressure to obtain the final nano silicon dioxide product, wherein the particle size range is 27-33nm, and the water content is 24%.
Example 5
Adding water into silica colloid with the conductivity of 1us/cm to prepare 15% silica emulsion, and uniformly stirring. And transferring the uniformly stirred silicon dioxide emulsion into high-pressure jet devices of three high-pressure gun heads, and controlling the jet pressure to be 15MPa, the distance between the gun heads to be 4mm and the caliber to be 1 mm. And opening a gun head switch to spray the three strands of silicon dioxide emulsion. During the opposite injection, the gun head rifling makes the jet flow be injected in a spiral shape, the impulse is increased, the three strands of spiral jet flows are subjected to energy conversion after collision, and the three strands of liquid are emitted outwards in a turbulent flow mode to form atomized nano liquid drops. And simultaneously starting liquid carbon dioxide to purge and atomize the nano liquid drops, wherein the temperature of the liquid carbon dioxide is-60 ℃, the purging pressure is 1MPa, so that the formed nano liquid drops are rapidly solidified, collecting the solidified nano silicon dioxide product, and reducing the pressure and raising the temperature to normal temperature and normal pressure to obtain the final nano silicon dioxide product, wherein the particle size range is 35-40nm, and the water content is 21%.
Example 6
Adding water into silica colloid with conductivity of 5us/cm to prepare 15% silica emulsion, and stirring uniformly. And transferring the uniformly stirred silicon dioxide emulsion into high-pressure jet devices of three high-pressure gun heads, and controlling the spraying pressure to be 10MPa, the distance between the gun heads to be 2mm and the caliber to be 2 mm. And opening a gun head switch to spray the three strands of silicon dioxide emulsion. During the opposite injection, the gun head rifling makes the jet flow be injected in a spiral shape, the impulse is increased, the three strands of spiral jet flows are subjected to energy conversion after collision, and the three strands of liquid are emitted outwards in a turbulent flow mode to form atomized nano liquid drops. And simultaneously starting liquid carbon dioxide to purge and atomize the nano liquid drops, wherein the temperature of the liquid carbon dioxide is-40 ℃, the purging pressure is 4MPa, so that the formed nano liquid drops are rapidly solidified, collecting the solidified nano silicon dioxide product, and reducing the pressure and raising the temperature to normal temperature and normal pressure to obtain the final nano silicon dioxide product, wherein the particle size range is 31-38nm, and the water content is 18%.
It should be noted that the silica colloid described in the above embodiments can be prepared by a precipitation method in the prior art, in which sodium silicate and sulfuric acid are used as raw materials to prepare the silica colloid.
Comparative example 1
CN103588210A the preparation method of example 1 is used for preparing nano-silica, so as to obtain the nano-silica with the particle size of 60-90nm and the water content of 30%.
Comparative example 2
Preparing the silica colloid with the conductivity of 10us/cm into 2 percent silica emulsion, and uniformly stirring. And transferring the uniformly stirred silicon dioxide emulsion into high-pressure jet devices of two high-pressure gun heads, and controlling the jet pressure to be 1MPa, the distance between the gun heads to be 1mm and the caliber to be 2 mm. And opening a gun head switch to jet the two silicon dioxide emulsions. During the opposite injection, the gun head rifling makes the jet flow be injected in a spiral shape, the impulse is increased, the two spiral jet flows are collided and then subjected to energy conversion, and the two liquid flows are emitted outwards in a turbulent flow mode to form atomized nano liquid drops. And simultaneously starting liquid carbon dioxide to purge and atomize the nano liquid drops, wherein the temperature of the liquid carbon dioxide is-40 ℃, the purging pressure is 1MPa, so that the formed nano liquid drops are rapidly solidified, collecting the solidified nano silicon dioxide product, and reducing the pressure and raising the temperature to normal temperature and normal pressure to obtain the final nano silicon dioxide product, wherein the particle size range is 35-60nm, and the water content is 24%.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents and are included in the scope of the present invention.
Claims (8)
1. The impact flow method for preparing the nano silicon dioxide is characterized in that: the preparation method for preparing the nano silicon dioxide by the impinging stream method comprises the following steps:
(1) adding water into a silicon dioxide colloid to prepare a silicon dioxide emulsion, wherein the conductivity of the silicon dioxide colloid is 0.5-5 us/cm, and the concentration of the silicon dioxide emulsion is 3-15% (w/w); the silica colloid is prepared by adopting a precipitation method and taking sodium silicate and sulfuric acid as raw materials;
(2) placing the silicon dioxide emulsion in a high-pressure jet device for spraying, forming a turbulent fluid system after spraying to form nano atomized liquid drops, and simultaneously starting freezing airflow to purge the nano atomized liquid drops to quickly solidify the formed nano liquid drops;
(3) collecting the solidified nano particles, and obtaining the nano silicon dioxide after reducing pressure and raising temperature to normal temperature and normal pressure.
2. The impact flow method for preparing nano-silica according to claim 1, wherein: the high-pressure jet device comprises two high-pressure gun heads, and the high-pressure gun heads are 180 degrees.
3. The impact flow method for preparing nano-silica according to claim 1, wherein: the high-pressure jet device comprises three high-pressure gun heads, and the high-pressure gun heads are 120 degrees.
4. The impact flow method for preparing nano-silica according to claim 2 or 3, wherein: the caliber of the muzzle of the high-pressure gun head is 1-2mm, and the muzzle distance is 1-4 mm.
5. The impact flow method for preparing nano-silica according to any one of claims 1 to 3, wherein: the injection pressure of the high-pressure jet device is 1-15 MPa.
6. The impact flow method for preparing nano-silica according to claim 1, wherein: the refrigerated gas stream is liquid carbon dioxide.
7. The impact flow method for preparing nano-silica according to claim 6, wherein: the temperature of the liquid carbon dioxide is minus 40 ℃ to minus 60 ℃.
8. The impact flow method for preparing nano-silica according to claim 6, wherein: the blowing pressure of the freezing airflow is 1-10 MPa.
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| CN1814344A (en) * | 2005-02-05 | 2006-08-09 | 中国石油化工股份有限公司 | Impact flow reactor for liquid-phase reaction |
| CN101863479B (en) * | 2010-06-25 | 2012-07-11 | 应城市东诚有机硅有限公司 | Method for preparing silica aerogel by supercritical drying with high-pressure liquid medium |
| CN103588210A (en) * | 2012-08-17 | 2014-02-19 | 东莞市长安东阳光铝业研发有限公司 | Preparation method of nano silicon dioxide |
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| CN1814344A (en) * | 2005-02-05 | 2006-08-09 | 中国石油化工股份有限公司 | Impact flow reactor for liquid-phase reaction |
| CN101863479B (en) * | 2010-06-25 | 2012-07-11 | 应城市东诚有机硅有限公司 | Method for preparing silica aerogel by supercritical drying with high-pressure liquid medium |
| CN103588210A (en) * | 2012-08-17 | 2014-02-19 | 东莞市长安东阳光铝业研发有限公司 | Preparation method of nano silicon dioxide |
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