CN111495291A - Continuous production equipment for integration of synthesis and modification of nano material and method thereof - Google Patents
Continuous production equipment for integration of synthesis and modification of nano material and method thereof Download PDFInfo
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- CN111495291A CN111495291A CN202010527180.4A CN202010527180A CN111495291A CN 111495291 A CN111495291 A CN 111495291A CN 202010527180 A CN202010527180 A CN 202010527180A CN 111495291 A CN111495291 A CN 111495291A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J14/00—Chemical processes in general for reacting liquids with liquids; Apparatus specially adapted therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/28—Moving reactors, e.g. rotary drums
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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
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention relates to a continuous production device and a method for integration of synthesis and modification of a nano material, wherein the continuous production device comprises an outer barrel, an inner barrel and a disc which are sequentially arranged from outside to inside, the outer barrel, the inner barrel and the disc are coaxially arranged, a barrel cover is rotatably arranged at an opening at the upper end of the outer barrel, a liquid outlet pipe orifice is formed at one side of the lower part of the outer barrel, a flow guide hole communicated with the outer barrel is arranged at the bottom of the inner barrel, the disc and the inner barrel are fixedly arranged together, and the disc and the inner barrel are rotatably arranged in the outer barrel; the upper end surface of the disc forms a first surface, and the inner side wall of the inner cylinder forms a second surface. The invention has the advantages that: the surface modification reaction liquid is spread to form a longitudinal film, and the reaction liquid forms a film in the horizontal direction, so that the defect that the nano-particle crystal is generated due to too short retention time of the nano-reaction liquid of the common film reactor is overcome.
Description
Technical Field
The invention relates to a continuous production device and a method for integration of synthesis and modification of a nano material, and relates to the field of continuous flow reactors.
Background
In recent years, with the development of nanotechnology, nanomaterials and their corresponding preparation techniques have become the mainstream direction in the scientific and technological development in the world today, and are also one of the main research hotspots in scientific research today. Nanotechnology is of no doubt as an emerging scientific technology with the most potential for market applications. In recent years, nanotechnology has achieved a great deal of research and development efforts and technological breakthroughs in different fields, such as advanced materials, biomedicine, catalysts, electronics and pharmaceutical fields; and continuously expand new fields such as energy, water treatment, agriculture and forestry; simultaneously, nanotechnology is combined with other emerging fields, such as quantum information systems, neuromorphic engineering, synthesis, and system biology; the fields of continuous generation, such as spintronics, surface plasmon photonics, metamaterials, molecular nanosystems, and the like.
Under the wide application prospect of the nano-particles, the means for synthesizing the nano-particles at present still mainly synthesizes the nano-particles in a small scale in a laboratory, and mainly synthesizes the nano-particles by a physical method and a chemical method, and the nano-particles prepared by the physical method are mostly large in particle size and wide in distribution range, so that the nano-particles meeting the application purpose are difficult to realize; the nano particles prepared by the chemical method have small production scale, the preparation process is difficult to control, and the amplification production of the nano particles is difficult to realize although the product purity is generally higher. There are also many deficiencies in the nanoparticle size that can be generated from industrially used reaction vessels for preparing nanoparticles. Therefore, it is important to develop an apparatus that can realize the scaled-up production of nanoparticles.
At present, nanoparticles with smaller sizes are mainly prepared in an organic solvent, and the prepared nanoparticles have good dispersion performance in the organic solvent, but the water solubility of the nanoparticles is generally poor. However, in the fields of drug carriers and medical diagnosis, nanoparticles must have good water solubility if low biotoxicity and high bioavailability are to be achieved, and thus the surface of nanoparticles is modified to achieve good water solubility. At present, there are two methods for surface modification of nanoparticles, one is to add surface modification molecules to perform surface modification while synthesizing nanoparticles, and the other is to combine nanoparticles with surface modification molecules to realize surface modification after synthesizing nanoparticles. The synthesis of the two schemes is mainly realized in a flask in a laboratory and an industrial reaction kettle at present, the synthesis in the laboratory has complete surface modification and good water solubility, but the industrial amplification production is still difficult to realize; the preparation of the nano particles with incomplete surface modification in an industrial reaction kettle is difficult to obtain nano particles with uniform size, complete structure and complete surface modification.
The continuous flow reactor is widely applied in process intensification and can be used for preparing nano particles, and compared with the traditional kettle type batch reactor, the continuous flow microreactor for preparing nano particles at present has the advantages of high-speed mixing, high-efficiency heat transfer, narrow distribution of reactant retention time, good repeatability, quick system response, convenient operation and control, almost no amplification effect, small amount of on-line chemicals, high safety performance and the like. However, most of the existing continuous flow reactors are based on a microchannel technology, the channels of the microchannel continuous flow reactors with simple structures are completely laminar, and the mass transfer and heat transfer efficiency in fluid is not ideal, so that the uniformity of products is poor; the microchannel reactor with a complex structure can generate partial turbulence as much as possible through the channel design to reduce the thickness of a laminar layer, but the design can also cause the increase of fluid resistance, so that the equipment cost is increased, and the increase of the fluid flow speed is restricted to influence the yield. However, the most deadly of the reactors showed reaction residence times of typically less than 20 seconds, and most reactions could not be completed in such a short time. This also makes the applicability of such reactors very narrow. Therefore, the development of a continuous production apparatus integrating the synthesis and surface modification of nanocrystal materials is the focus of current research.
Disclosure of Invention
In order to overcome the problems that the preparation of nano particles is difficult to amplify and the reaction residence time of a film continuous flow reactor is short at present, the invention provides continuous production equipment and a method integrating synthesis of nano crystal materials and surface modification, which can realize industrial amplified production and solve the problems of difficult control of particle size and crystallinity and the like caused by too short residence time of reaction liquid in a common film reactor. The technical scheme of the invention is as follows:
the continuous production equipment for integration of synthesis and modification of the nano material comprises an outer barrel, an inner barrel and a disc which are sequentially arranged from outside to inside, wherein the outer barrel, the inner barrel and the disc are coaxially arranged, a barrel cover is rotatably arranged at an opening at the upper end of the outer barrel, a liquid outlet pipe orifice is formed at one side of the lower part of the outer barrel, a flow guide hole communicated with the outer barrel is formed at the bottom of the inner barrel, the disc and the inner barrel are fixedly arranged together, and the disc and the inner barrel are rotatably arranged in the outer barrel; the up end of disc forms first surface, and the inside wall of interior barrel forms the second surface, installs first feed liquor unit and second feed liquor unit on this cover, first feed liquor unit with first surface corresponding, second feed liquor unit with the second surface corresponding.
The first surface is densely distributed with annular grooves, and all the annular grooves are concentrically arranged.
The lower part of the disc is provided with a stud, the stud is arranged along the vertical direction, the upper end of the stud is arranged on the disc, and the lower end of the stud sequentially penetrates through the bottom of the inner cylinder and the bottom of the outer cylinder and then is driven by a driving mechanism; the stud is fixedly connected with the inner cylinder body and is in running fit with the outer cylinder body.
The driving mechanism comprises a motor, a belt, a driving roller and a driven roller, the driving roller is installed on a rotating shaft of the motor, the driven roller is installed after the lower end of the stud penetrates through the bottom of the outer barrel, and the driven roller is in transmission fit with the driving roller through the belt.
A conical guide plate is arranged at the bottom inside the inner cylinder body, and the guide hole is formed in the lower end of the conical guide plate; the flow guide holes are three arc-shaped holes arranged along the circumferential direction of the bottom of the inner barrel, and a space is formed between every two adjacent arc-shaped holes.
The first liquid inlet unit comprises two first liquid inlet pipes, the upper ends of the two first liquid inlet pipes are located outside the outer barrel, the lower ends of the two first liquid inlet pipes extend into the inner portion of the inner barrel, the lower ends of the two first liquid inlet pipes stretch into the inner portion of the inner barrel and then are close to each other, and a space is formed between the lower ends of the two first liquid inlet pipes and the first surface.
The second liquid inlet unit comprises a second liquid inlet pipe, the upper end of the second liquid inlet pipe is located outside the outer cylinder, the lower end of the second liquid inlet pipe extends into the inner portion of the inner cylinder and then is bent, and the bent section of the second liquid inlet pipe points to the side wall of the inner cylinder.
The cylinder cover is provided with a handle and a lock catch, and two sides of the handle are respectively provided with the lock catch; an observation window is arranged on the cylinder cover close to the first liquid inlet unit.
A method for integrated continuous production of nanocrystalline material synthesis and surface modification, comprising the steps of:
(1) injecting two reaction liquids of the nanocrystal material to be synthesized onto a disc in an inner cylinder body through two first liquid inlet pipes at a preset speed, wherein the outer cylinder body is fixed, and the inner cylinder body and the disc coaxially rotate;
(2) two kinds of reaction liquid injected through the two first liquid inlet pipes are rapidly pulled into thin films on the disc, and then the thin films formed by the two kinds of reaction liquid are mixed, because the thin films of the two kinds of reaction liquid are in a uniform concentration environment, crystal nuclei with uniform size are formed;
(3) due to the action of the centrifugal force of the disc, the mixed film flows along the radial direction of the disc, and meanwhile, redundant reaction precursors can continue to grow on the original crystal nucleus;
(4) injecting the surface modification reaction liquid onto the inner side wall of the inner cylinder through a second liquid inlet pipe, and spreading the surface modification reaction liquid into a longitudinal film on the inner side wall of the inner cylinder; when the films of the two reaction liquids are thrown away from the disc, the films and the surface modification reaction liquid film on the inner side wall of the inner cylinder body are subjected to surface modification reaction and curing to obtain the surface-modified nano crystal particles with uniform particle size.
And (5) allowing the nano-crystal particles to flow into the outer barrel through the flow guide hole at the bottom of the inner barrel, and flow out of the outer barrel through the liquid outlet pipe orifice of the outer barrel.
The invention has the advantages that:
1. the two rotating surfaces spread the reaction liquid into transverse and longitudinal micro-thin films respectively, so that the concentration gradient of the reaction liquid in each direction is greatly reduced, on one hand, the reaction precursor is highly uniform, and on the other hand, the mass transfer and heat transfer efficiency inside the liquid film is also enhanced.
2. The nanoparticle precursor nucleates in the micro-film on the first surface and generates original crystal nuclei with uniform particle sizes. In the longitudinal micro-film on the second surface, the precursor with uniform concentration can be uniformly adsorbed and grown on the original crystal nucleus, so that the particle size of the generated nano-particles is highly uniform.
3. The design of the second surface greatly increases the residence time of the continuous flow reactor, so that the reaction is more complete and the crystallinity of the nano material is higher.
4. The integrated design of nanoparticle synthesis and surface modification enables the surface modifier added in the second surface to be modified on the surface of the nanoparticles in real time, and the occurrence of nanoparticle agglomeration is avoided.
Drawings
Fig. 1 is a sectional view of the main structure of the present invention.
Fig. 2 is a schematic view showing a connection relationship between the inner cylinder and the outer cylinder in fig. 1.
Fig. 3 is a top view of the disk of fig. 1.
Fig. 4 is a schematic view of the structure of the cartridge cover of fig. 1.
Detailed Description
The invention will be further described with reference to specific embodiments, and the advantages and features of the invention will become apparent as the description proceeds. These examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.
Referring to fig. 1 to 4, the present invention relates to an integrated continuous production equipment for nanomaterial synthesis and modification, which comprises an outer cylinder 1, an inner cylinder 3 and a disc 6, which are sequentially arranged from outside to inside, wherein the outer cylinder 1, the inner cylinder 3 and the disc 6 are coaxially arranged, a cylinder cover 2 is rotatably arranged at an opening at the upper end of the outer cylinder 1, a liquid outlet pipe opening 9 is formed at one side of the lower part of the outer cylinder 1, a flow guide hole 10 communicated with the outer cylinder 1 is arranged at the bottom of the inner cylinder 3, the disc 6 and the inner cylinder 3 are fixedly arranged together, and the rotatably arranged 1 is arranged in the outer cylinder; the upper end face of disc 6 forms first surface, and the interior lateral wall of interior barrel 3 forms the second surface, installs first feed liquor unit and second feed liquor unit on this cover 2, first feed liquor unit with first surface corresponding, the second feed liquor unit with the second surface corresponding.
As shown in fig. 3, the first surface is densely packed with annular grooves 14, all of which are concentrically arranged.
The lower part of the disc 6 is provided with a stud 7, the stud 7 is arranged along the vertical direction, the upper end of the stud 7 is arranged on the disc 6, and the lower end of the stud passes through the bottom of the inner cylinder 3 and the bottom of the outer cylinder 1 in sequence and then is driven by a driving mechanism; the stud 7 is fixedly connected with the inner cylinder 3, the stud 7 is in running fit with the outer cylinder 1, the inner cylinder 3 and the disc 6 rotate together, and the outer cylinder 1 is fixed.
The driving mechanism is a conventional driving mechanism and comprises a motor, a belt, a driving roller and a driven roller, the driving roller is installed on a rotating shaft of the motor, the driven roller is installed after the lower end of the stud penetrates through the bottom of the outer barrel, and the driven roller is in transmission fit with the driving roller through the belt.
A conical guide plate 8 is arranged at the bottom inside the inner cylinder 3, and the guide hole 10 is arranged at the lower end of the conical guide plate 8; specifically, the flow guide holes 10 are three arc-shaped holes arranged along the circumferential direction of the bottom of the inner cylinder 3, and a space is formed between every two adjacent arc-shaped holes.
The first liquid inlet unit comprises two first liquid inlet pipes 5 for injecting reaction liquid, the upper ends of the two first liquid inlet pipes 5 are positioned outside the outer barrel body 1, the lower ends of the two first liquid inlet pipes extend to the inside of the inner barrel body 3, the lower ends of the two first liquid inlet pipes 5 extend into the inner barrel body and then are close to each other, and a distance of 1cm is formed between the lower ends of the two first liquid inlet pipes and the first surface.
The second liquid inlet unit comprises a second liquid inlet pipe 4 for injecting surface modification reaction liquid, the upper end of the second liquid inlet pipe is positioned outside the outer cylinder, the lower end of the second liquid inlet pipe extends into the inner part of the inner cylinder and then is bent, and the bending section of the second liquid inlet pipe points to the side wall of the inner cylinder.
The cylinder cover 2 is provided with a handle 13 and a lock catch 11, and two sides of the handle are respectively provided with a lock catch; an observation window 12 is provided on the cylinder cover 2 near the first liquid inlet unit.
The invention also relates to a method for the integrated continuous production of nanocrystalline material synthesis and surface modification, comprising the steps of:
(1) injecting two reaction liquids of the nanocrystal material to be synthesized onto a disc in an inner cylinder body through two first liquid inlet pipes at a preset speed, wherein the outer cylinder body is fixed, and the inner cylinder body and the disc coaxially rotate;
(2) two kinds of reaction liquid injected through the two first liquid inlet pipes are rapidly pulled into thin films on the disc, and then the thin films formed by the two kinds of reaction liquid are mixed, so that crystal nuclei with uniform size are formed because the thin films of the two kinds of reaction liquid are in a uniform concentration environment; the annular grooves on the disc can effectively promote the reaction liquid to flow radially with high-efficiency turbulence, so that the growth of the nano crystal particles is highly uniform; the residence time of the reaction liquid on the inner side wall of the inner cylinder body can be adjusted by changing the rotating speed of the inner cylinder body and the injection speed of the reaction liquid.
(3) Due to the action of the centrifugal force of the disc, the mixed film flows along the radial direction of the disc, and meanwhile, redundant reaction precursors can continue to grow on the original crystal nucleus;
(4) injecting the surface modification reaction liquid onto the inner side wall of the inner cylinder through a second liquid inlet pipe, and spreading the surface modification reaction liquid into a longitudinal film on the inner side wall of the inner cylinder; when the films of the two reaction liquids are thrown away from the disc, the films and the surface modification reaction liquid film on the inner side wall of the inner cylinder body are subjected to surface modification reaction and curing. The nano crystal particles formed by the reaction have high specific surface area and surface energy, and the surface atoms of unsaturated bonds on the surface are added, so that the nano crystal particles and the surface modification reaction solution can quickly react, and the nano crystal particles with modified surfaces and uniform particle sizes are obtained.
And (5) allowing the nano-crystal particles to flow into the outer barrel through the flow guide hole at the bottom of the inner barrel, and flow out of the outer barrel through the liquid outlet pipe orifice of the outer barrel.
Claims (10)
1. The continuous production equipment for integration of synthesis and modification of the nano material is characterized by comprising an outer barrel, an inner barrel and a disc which are sequentially arranged from outside to inside, wherein the outer barrel, the inner barrel and the disc are coaxially arranged, a barrel cover is rotatably arranged at an opening at the upper end of the outer barrel, a liquid outlet pipe orifice is formed at one side of the lower part of the outer barrel, a flow guide hole communicated with the outer barrel is formed at the bottom of the inner barrel, the disc and the inner barrel are fixedly arranged together, and the disc and the inner barrel are rotatably arranged in the outer barrel; the up end of disc forms first surface, and the inside wall of interior barrel forms the second surface, installs first feed liquor unit and second feed liquor unit on this cover, first feed liquor unit with first surface corresponding, second feed liquor unit with the second surface corresponding.
2. The integrated continuous production equipment for synthesis and modification of nanometer materials as claimed in claim 1, wherein the first surface is densely distributed with annular grooves, and all the annular grooves are concentrically arranged.
3. The integrated continuous production equipment for synthesis and modification of nano-materials according to claim 1 or 2, wherein the lower part of the disc is provided with a stud, the stud is arranged along the vertical direction, the upper end of the stud is arranged on the disc, and the lower end of the stud is driven by a driving mechanism after sequentially penetrating through the bottom of the inner cylinder and the bottom of the outer cylinder; the stud is fixedly connected with the inner cylinder body and is in running fit with the outer cylinder body.
4. The integrated continuous production equipment for nanomaterial synthesis and modification according to claim 3, wherein the driving mechanism comprises a motor, a belt, a driving roller and a driven roller, the driving roller is installed on a rotating shaft of the motor, the driven roller is installed after the lower end of the stud penetrates through the bottom of the outer cylinder body, and the driven roller is in transmission fit with the driving roller through the belt.
5. The integrated continuous production equipment for nanomaterial synthesis and modification according to claim 1, wherein a conical flow guide plate is installed at the bottom inside the inner cylinder, and the flow guide hole is arranged at the lower end of the conical flow guide plate; the flow guide holes are three arc-shaped holes arranged along the circumferential direction of the bottom of the inner barrel, and a space is formed between every two adjacent arc-shaped holes.
6. The continuous production equipment for integration of synthesis and modification of the nano-materials according to claim 1 or 5, wherein the first liquid inlet unit comprises two first liquid inlet pipes, the upper ends of the two first liquid inlet pipes are positioned outside the outer cylinder, the lower ends of the two first liquid inlet pipes extend into the inner cylinder, and the lower ends of the two first liquid inlet pipes extend into the inner cylinder, are close to each other and form a space with the first surface.
7. The integrated continuous production equipment for synthesis and modification of nano-materials according to claim 1 or 5, wherein the second liquid inlet unit comprises a second liquid inlet pipe, the upper end of the second liquid inlet pipe is positioned outside the outer cylinder, the lower end of the second liquid inlet pipe extends into the inner cylinder and then is bent, and the bent section of the second liquid inlet pipe points to the side wall of the inner cylinder.
8. The integrated continuous production equipment for synthesis and modification of nano-materials according to claim 1, wherein a handle and a lock catch are installed on the cylinder cover, and a lock catch is respectively arranged on two sides of the handle; an observation window is arranged on the cylinder cover close to the first liquid inlet unit.
9. A method for integrated continuous production of nanocrystalline material synthesis and surface modification, comprising the steps of:
(1) injecting two reaction liquids of the nanocrystal material to be synthesized onto a disc in an inner cylinder body through two first liquid inlet pipes at a preset speed, wherein the outer cylinder body is fixed, and the inner cylinder body and the disc coaxially rotate;
(2) two kinds of reaction liquid injected through the two first liquid inlet pipes are rapidly pulled into thin films on the disc, and then the thin films formed by the two kinds of reaction liquid are mixed, so that crystal nuclei with uniform size are formed because the thin films of the two kinds of reaction liquid are in a uniform concentration environment;
(3) due to the action of the centrifugal force of the disc, the mixed film flows along the radial direction of the disc, and meanwhile, redundant reaction precursors can continue to grow on the original crystal nucleus;
(4) injecting the surface modification reaction liquid onto the inner side wall of the inner cylinder through a second liquid inlet pipe, and spreading the surface modification reaction liquid into a longitudinal film on the inner side wall of the inner cylinder; when the films of the two reaction liquids are thrown away from the disc, the films and the surface modification reaction liquid film on the inner side wall of the inner cylinder body are subjected to surface modification reaction and curing to obtain the surface-modified nano crystal particles with uniform particle size.
10. The method according to claim 9, further comprising a step (5) of allowing the nanocrystal particles to flow into the outer cylinder through the diversion hole at the bottom of the inner cylinder, and to flow out of the outer cylinder through the liquid outlet pipe orifice of the outer cylinder.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112705319A (en) * | 2020-12-28 | 2021-04-27 | 荣成富邦金属科技有限公司 | Clay sand molding sand crusher |
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| US6858189B1 (en) * | 1999-02-17 | 2005-02-22 | Protensive Limited (A Company Incorporated In England) | Rotating surface of revolution reactor with feed and collection mechanisms |
| US20040241430A1 (en) * | 2001-07-20 | 2004-12-02 | Jachuck Roshan Jeet Jee | Methods of manufacturing particles |
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