Double-needle type electric spraying device for constructing flying-up reactor
By a double-needle electrospray device that sprays two components of the two-component reaction mixture solution simultaneously under the action of an electric field, the problem that existing electrohydraulic atomization device is difficult to prepare micro nanoparticle materials is solved, and the preparation effect of smaller particle size and narrower distribution range is achieved.
Patent Information
- Application Number
- CN202420878616.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-04-25
- Publication Date
- 2025-03-11
- Estimated Expiration
- 2034-04-25
AI Technical Summary
It is difficult for existing electrohydraulic atomization devices to prepare tiny nanoparticle materials, and there are uncontrollable factors such as local uneven mixing, excessive reaction, and heat transfer limits.
A double-needle electrospray device for constructing a ascending reactor is designed. By atomizing and spraying two components of the two-component reaction mixed solution under the action of an electric field, it can mix and react at the same site, enhancing the micro-mixing efficiency of the reaction mixed solution.
The particle nucleation is achieved in a relatively uniform solution environment, and the prepared particle size is smaller and the distribution range is narrower, solving the problem of difficult particle size and morphology, and achieving better preparation effect at a smaller voltage, greatly increasing safety.
Smart Images
Figure CN222586597U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of nano material synthesis devices, in particular to a double-needle type electrospray device for constructing a femtosecond reactor. Background Art
[0002] Micro-nanoscale materials have attracted extensive attention in the fields of scientific research and industrial production due to their numerous advantages. The research on micro-nano materials has become a research hotspot in various fields and industries. The rapid development of today's era has put forward higher requirements on the quality and rapid production of nanoparticle materials. Nanoparticle materials are prepared by precipitation, hydrothermal and sol-gel methods, but these traditional nanoparticle preparation methods have problems such as low yield, large particle size, wide distribution range, complex operation, and potential safety hazards, which cannot meet the needs of high-quality and rapid preparation of nanoparticles.
[0003] Since the 1990s, external field technology has become a new research hotspot. The introduction of external field technology into the chemical production process has demonstrated its great potential and broad application prospects in the synthesis, improvement and large-scale production of materials. As a type of external field enhancement technology, electrohydrodynamic atomization technology is considered to be a fast and efficient method for preparing nanomaterials due to its advantages such as simple operation and controllable process. However, the existing electrohydrodynamic atomization device usually prepares nanoparticles based on the volatilization of the solvent that forms the droplets or the atomization of a single component to react with another component. The reaction process has uncontrollable factors such as local uneven mixing, too fast reaction, and heat transfer limits, making it difficult to use for the preparation of tiny nanoparticle materials. Utility Model Content
[0004] In view of the fact that the existing electrohydrodynamic atomization device is difficult to use for preparing tiny nanoparticle materials, the utility model provides a double-needle electrospray device for constructing a femtoliter reactor. The utility model can simultaneously atomize the two components of a two-component reaction mixed solution into a plurality of femtoliter-scale (10 -15 L) and sprayed to the same site for mixing reaction, which enhances the micro-mixing efficiency of the reaction mixture. The nucleation of the particles is carried out in a relatively uniform solution environment (low dielectric constant organic solvent). The prepared particles are smaller in size and have a narrower distribution range, thereby solving the difficult-to-control problems of particle size and morphology.
[0005] The technical solution adopted by the utility model is:
[0006] A double-needle electrospray device for constructing a femtosecond reactor comprises a first injection pump, a second injection pump, a first raw material container, a second raw material container, a positive high-voltage power supply, a negative high-voltage power supply, a first metal nozzle, a second metal nozzle and a product collection container; the first metal nozzle is connected to the positive high-voltage power supply through a wire, the second metal nozzle is connected to the negative high-voltage power supply through a wire, the first metal nozzle and the second metal nozzle are arranged at two ends above the product collection container, and the outlet ends both extend into the product collection container, the outlet ends of the first metal nozzle and the second metal nozzle are arranged oppositely, so that the injection direction is toward a point between the two; the product collection container is used to contain a low dielectric constant organic solvent, and the outlet ends of the first metal nozzle and the second metal nozzle are located below the liquid level of the low dielectric constant organic solvent; the first raw material container and the second raw material container are detachably mounted on the first injection pump and the second injection pump respectively, and the first raw material container and the second raw material container are connected to the first metal nozzle and the second metal nozzle respectively through pipelines.
[0007] Furthermore, the positive high-voltage power supply voltage is 0 to 30 kV, and the negative high-voltage power supply voltage is 0 to -30 kV.
[0008] Furthermore, the dielectric constant of the low dielectric constant organic solvent is less than 10.
[0009] Furthermore, a collection layer is disposed below the low dielectric constant organic solvent, the collection layer has a density greater than that of the low dielectric constant organic solvent, and is poorly soluble or insoluble in the low dielectric constant organic solvent.
[0010] Furthermore, the collection layer is a deionized water layer.
[0011] Furthermore, the low dielectric constant organic solvent is n-hexane or cyclohexane.
[0012] Furthermore, the distance between the outlet ends of the first metal nozzle and the second metal nozzle is 3 to 5 cm.
[0013] Furthermore, a liquid outlet is provided at the bottom of the product collection container.
[0014] The beneficial effects of the utility model are:
[0015] The two-component solutions in the first raw material container and the second raw material container of the utility model are respectively transported to the first metal nozzle and the second metal nozzle under the driving of the first injection pump and the second injection pump, and then the two-component solutions are respectively atomized into a plurality of femtoliter-scale (10 - 15L) small particles. The utility model can simultaneously atomize and spray the two components of a two-component reaction mixed solution under the action of an electric field, and the outlet ends of the first metal nozzle and the second metal nozzle are relatively arranged so that the spraying direction is toward a point between the two, so that the small particles of the two-component solution after atomization are sprayed and mixed and reacted at the point, thereby enhancing the microscopic mixing efficiency of the reaction mixed solution, and the nucleation of the particles is carried out in a relatively uniform solution environment (low dielectric constant organic solvent), and the prepared particles are smaller in size and have a narrower distribution range, thereby solving the problem of difficult control of particle size, morphology, etc. The outlet ends of the first metal nozzle and the second metal nozzle of the utility model are located below the liquid level of the low dielectric constant organic solvent, so that the outlet ends of the first metal nozzle and the second metal nozzle are isolated from the air. Compared with being in the air, the influence of other ions in the air is reduced, and a better preparation effect can be achieved at a smaller voltage, and the safety is greatly increased.
[0016] A collection layer is provided below the low dielectric constant organic solvent in the utility model, and the product can be suspended in the collection layer, reducing the product from adhering to the inner wall of the product collection container, so as to facilitate the collection of the product. In the utility model, the spacing between the outlet ends of the first metal nozzle and the second metal nozzle is 3 to 5 cm. If the spacing between the first metal nozzle and the second metal nozzle is too large, the two components are not easy to contact, which affects the reaction rate. If the spacing is too small, the products formed are easy to agglomerate, and the agglomeration of the products easily leads to the final product particles being too large in size. BRIEF DESCRIPTION OF THE DRAWINGS
[0017] Figure 1 The utility model is a schematic diagram of a double-needle electrospray device for constructing a femtosecond reactor.
[0018] Figure 2 These are morphology images of Co3O4 nanoparticles and Mg(OH)2 nanoparticles prepared using the device of the utility model, wherein (a) and (b) are transmission electron microscope (TEM) images of Co3O4 nanoparticles, and (c) and (d) are transmission electron microscope (TEM) images of Mg(OH)2 nanoparticles.
[0019] In the figure, 1. first injection pump, 2. second injection pump, 3. first raw material container, 4. second raw material container, 5. positive high voltage power supply, 6. negative high voltage power supply, 7. first metal nozzle, 8. second metal nozzle, 9. product collection container. DETAILED DESCRIPTION
[0020] The present invention will be further described in detail below with reference to the specific implementation modes of the accompanying drawings, but the protection scope of the present invention is not limited thereto.
[0021] Embodiment 1
[0022] Figure 1The double-needle electrospray device for constructing a flying reactor according to the utility model is a specific embodiment. The double-needle electrospray device includes a first injection pump 1, a second injection pump 2, a first raw material container 3, a second raw material container 4, a positive high-voltage power supply 5, a negative high-voltage power supply 6, a first metal nozzle 7, a second metal nozzle 8, and a product collection container 9. The first metal nozzle 7 is connected to the positive high-voltage power supply 5 through a wire, and the voltage of the positive high-voltage power supply 5 is 0-30kV. The second metal nozzle 8 is connected to the negative high-voltage power supply 6 through a wire, and the voltage of the negative high-voltage power supply 6 is 0--30kV, so that there is a voltage difference between the first metal nozzle 7 and the second metal nozzle 8, and the two components of the two-component reaction mixed solution can be atomized and sprayed at the same time under the action of the electric field. The first metal nozzle 7 and the second metal nozzle 8 are arranged at both ends above the product collection container 9, and the outlet ends are both extended into the product collection container 9. The outlet ends of the first metal nozzle 7 and the second metal nozzle 8 are arranged relative to each other, so that the spray direction is toward a point between the two, so that the small particles of the two-component solution after atomization are sprayed and mixed and reacted at this point, thereby enhancing the microscopic mixing efficiency of the reaction mixed solution.
[0023] The product collection container 9 is used to contain a low dielectric constant organic solvent, so that the nucleation of the particles is carried out in a relatively uniform solution environment, and the prepared particles are smaller in size and have a narrower distribution range. The dielectric constant of the low dielectric constant organic solvent is less than 10, which reduces the weakening of the electric field by the low dielectric constant organic solvent, thereby reducing the influence of the weakening of the electric field on the atomization effect. The outlet ends of the first metal nozzle 7 and the second metal nozzle 8 are located below the liquid level of the low dielectric constant organic solvent, so that the outlet ends of the first metal nozzle and the second metal nozzle are isolated from the air. Compared with being in the air, the influence of other ions in the air is reduced, and a better preparation effect can be achieved at a lower voltage, and the safety is greatly increased. The distance between the outlet end of the first metal nozzle 7 and the outlet end of the second metal nozzle 8 is 3 to 5 cm. If the distance between the first metal nozzle 7 and the second metal nozzle 8 is too large, the two components are not easy to contact, which affects the reaction rate. If the distance is too small, the product formed is easy to agglomerate, and the product agglomeration is easy to cause the final product particle size to be too large. A collection layer is provided below the low dielectric constant organic solvent, the density of the collection layer is greater than that of the low dielectric constant organic solvent, and the collection layer is poorly soluble or incompatible with the low dielectric constant organic solvent, so that when the low dielectric constant organic solvent and the collection layer are added to the product collection container 9, the low dielectric constant organic solvent and the collection layer can be divided into two layers and the collection layer is located below the low dielectric constant organic solvent. The low dielectric constant organic solvent is n-hexane or cyclohexane, and the collection layer is a deionized water layer. The product can be suspended in the deionized water to reduce the adhesion of the product to the inner wall of the product collection container 9, so as to facilitate the collection of the product. A liquid outlet is provided at the bottom of the product collection container 9 for collecting the product; in addition, when the product collection container 9 needs to be cleaned, the liquid and impurities after cleaning the product collection container 9 can also be discharged from the liquid outlet for cleaning.
[0024] The first raw material container 3 and the second raw material container 4 are detachably mounted on the first injection pump 1 and the second injection pump 2, respectively, so as to facilitate adding two-component solutions into the first raw material container 3 and the second raw material container 4. The first raw material container 3 and the second raw material container 4 are respectively connected to the first metal nozzle 7 and the second metal nozzle 8 through pipelines, so that the two-component solutions in the first raw material container 3 and the second raw material container 4 can be transported to the first metal nozzle 7 and the second metal nozzle 8 under the drive of the first injection pump 1 and the second injection pump 2, respectively.
[0025] The two-component solutions in the first raw material container 3 and the second raw material container 4 are respectively transported to the first metal nozzle 7 and the second metal nozzle 8 under the driving of the first injection pump 1 and the second injection pump 2, and then the two-component solutions are respectively atomized into a plurality of femtoliter-scale (10 -15L) small particles. The utility model can simultaneously atomize and spray the two components of the two-component reaction mixed solution under the action of an electric field, and the outlet ends of the first metal nozzle 7 and the second metal nozzle 8 are relatively arranged so that the spraying directions are all toward a point between the two, so that the small particles of the two-component solution after atomization are sprayed and mixed and reacted at the point, thereby enhancing the microscopic mixing efficiency of the reaction mixed solution, and the nucleation of the particles is carried out in a relatively uniform solution environment (low dielectric constant organic solvent), and the prepared particles are smaller in size and narrower in distribution range, thereby solving the problem of difficult control of particle size, morphology, etc.
[0026] Embodiment 2
[0027] This embodiment provides a method for using the double-needle electrospray device for constructing a femtosecond reactor. Taking the process of preparing Co3O4 nanoparticles as an example, the specific steps are as follows:
[0028] Weigh 5.8206g Co(NO3) 2. 6H2O and 0.8g NaOH are dissolved in 100ml deionized water, respectively, and are recorded as reaction solution A and reaction solution B, respectively. Reaction solution A is loaded into the first raw material container 3, and the first raw material container 3 is installed on the first injection pump 1, so that the first injection pump 1 can squeeze the reaction solution A out of the first raw material container 3 by compressing the space inside the first raw material container 3. The output end of the first raw material container 3 is connected to the first metal nozzle 7 through a pipeline, so that the reaction solution A can be transported into the first metal nozzle 7 after being squeezed out of the first raw material container 3. The first metal nozzle 7 is connected to the positive high-voltage power supply 5 through a wire. Similarly, reaction solution B is loaded into the second raw material container 4, and the second raw material container 4 is installed on the second injection pump 2, so that the second injection pump 2 can squeeze the reaction solution A out of the second raw material container 4 by compressing the space inside the second raw material container 4. The output end of the second raw material container 4 is connected to the second metal nozzle 8 through a pipeline, so that the reaction solution A can be transported into the second metal nozzle 8 after being squeezed out of the second raw material container 4. The first metal nozzle 7 is connected to the positive high-voltage power supply 5 through a wire.
[0029] 10 ml of deionized water and 200 ml of n-hexane are added to the product collection container 9 in sequence. Since deionized water and n-hexane are incompatible and the density of deionized water is greater than that of n-hexane, the deionized water is located below the n-hexane. In order to isolate the outlet ends of the first metal nozzle 7 and the second metal nozzle 8 from the air, the first metal nozzle 7 and the second metal nozzle 8 are extended into the n-hexane and the outlet ends of the first metal nozzle 7 and the second metal nozzle 8 are located in the low dielectric constant organic solvent, and the outlet ends of the first metal nozzle 7 and the second metal nozzle 8 are arranged relative to each other, and the outlet ends of the first metal nozzle 7 and the second metal nozzle 8 are set to 4 cm. Then adjust the parameters of the first injection pump 1 and the second injection pump 2 respectively, so that the total injection amount of the reaction solution A and the reaction solution B are both 5 ml, and the flow rate is 0.5-2 ml / h. After starting the first injection pump 1 and the second injection pump 2, start the positive high-voltage power supply 5 and the negative high-voltage power supply 6 to work.
[0030] After the experiment, the product was transferred to a three-necked flask, hydrogen peroxide was added, and condensation reflux was performed at 90° C. The obtained product was then dried in an oven at 60° C. to obtain the final target product.
[0031] Figure 2 (a) and Figure 2 (b) is a transmission electron microscope (TEM) image of Co3O4 nanoparticles prepared by the present invention. Figure 2 (a) and Figure 2 It can be seen in (b) that the Co3O4 particles are granular with an average size of 8.2 nm, a smaller average particle size and a narrower particle size distribution.
[0032] Embodiment 3
[0033] This embodiment provides a method for using the double-needle electrospray device for constructing a femtosecond reactor. Taking the process of preparing Mg(OH)2 nanoparticles as an example, the specific steps are as follows:
[0034] NaOH and MgCl2 aqueous solutions with concentrations of 0.3286 mol / L and 0.1786 mol / L are respectively prepared, and the two are respectively recorded as reaction solution A and reaction solution B. Reaction solution A is loaded into the first raw material container 3, and the first raw material container 3 is installed on the first injection pump 1, so that the first injection pump 1 can squeeze the reaction solution A out of the first raw material container 3 by compressing the space inside the first raw material container 3. The output end of the first raw material container 3 is connected to the first metal nozzle 7 through a pipeline, so that the reaction solution A can be transported into the first metal nozzle 7 after being squeezed out of the first raw material container 3. The first metal nozzle 7 is connected to the positive high-voltage power supply 5 through a wire. Similarly, reaction solution B is loaded into the second raw material container 4, and the second raw material container 4 is installed on the second injection pump 2, so that the second injection pump 2 can squeeze the reaction solution A out of the second raw material container 4 by compressing the space inside the second raw material container 4. The output end of the second raw material container 4 is connected to the second metal nozzle 8 through a pipeline, so that the reaction solution A can be transported into the second metal nozzle 8 after being squeezed out of the second raw material container 4. The first metal nozzle 7 is connected to the positive high-voltage power supply 5 through a wire.
[0035] 10 ml of deionized water and 200 ml of n-hexane are added to the product collection container 9 in sequence. Since deionized water and n-hexane are incompatible and the density of deionized water is greater than that of n-hexane, the deionized water is located below the n-hexane. In order to isolate the outlet ends of the first metal nozzle 7 and the second metal nozzle 8 from the air, the first metal nozzle 7 and the second metal nozzle 8 are extended into the n-hexane and the outlet ends of the first metal nozzle 7 and the second metal nozzle 8 are located in the low dielectric constant organic solvent, and the outlet ends of the first metal nozzle 7 and the second metal nozzle 8 are arranged relative to each other, and the outlet ends of the first metal nozzle 7 and the second metal nozzle 8 are set to 4 cm. Then adjust the parameters of the first injection pump 1 and the second injection pump 2 respectively, so that the total injection amount of the reaction solution A and the reaction solution B are both 5 ml, and the flow rate is 0.5-2 ml / h. After starting the first injection pump 1 and the second injection pump 2, start the positive high-voltage power supply 5 and the negative high-voltage power supply 6 to work.
[0036] After the experiment is completed, the collected products are placed in a drying oven at 60°C and dried to obtain the target product.
[0037] Figure 2 (c) and Figure 2 (d) is a transmission electron microscope (TEM) image of Mg(OH)2 nanoparticles prepared by the present invention. Figure 2 (c) and Figure 2 It can be seen from (d) that the Mg(OH)2 particles are flake-shaped with an average size of 37 nm. The particle size is relatively small and the particle size distribution is narrow.
[0038] The examples are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments. Any obvious improvements, substitutions or modifications that can be made by those skilled in the art without departing from the essential content of the present invention belong to the protection scope of the present invention.
Claims
1. A double-needle electrospray device for constructing a femtosecond reactor, characterized in that: It comprises a first injection pump (1), a second injection pump (2), a first raw material container (3), a second raw material container (4), a positive high-voltage power supply (5), a negative high-voltage power supply (6), a first metal nozzle (7), a second metal nozzle (8), and a product collection container (9); The first metal nozzle (7) is connected to the positive high-voltage power supply (5) through a wire, and the second metal nozzle (8) is connected to the negative high-voltage power supply (6) through a wire. The first metal nozzle (7) and the second metal nozzle (8) are arranged at two ends above the product collection container (9), and the outlet ends both extend into the product collection container (9). The outlet ends of the first metal nozzle (7) and the second metal nozzle (8) are arranged relative to each other so that the spraying direction is toward a point between the two. The product collection container (9) is used to contain a low dielectric constant organic solvent, and the outlet ends of the first metal nozzle (7) and the second metal nozzle (8) are located below the liquid surface of the low dielectric constant organic solvent. The first raw material container (3) and the second raw material container (4) are detachably mounted on the first injection pump (1) and the second injection pump (2), respectively, and the first raw material container (3) and the second raw material container (4) are connected to the first metal nozzle (7) and the second metal nozzle (8) respectively through pipelines.
2. The double-needle electrospray device for constructing a femtosecond reactor according to claim 1, characterized in that: The voltage of the positive high-voltage power supply (5) is 0 to 30 kV, and the voltage of the negative high-voltage power supply (6) is 0 to -30 kV.
3. The double-needle electrospray device for constructing a femtosecond reactor according to claim 1, characterized in that: The low dielectric constant organic solvent has a dielectric constant of less than 10.
4. The double-needle electrospray device for constructing a femtosecond reactor according to claim 3, characterized in that: A collection layer is arranged below the low dielectric constant organic solvent. The collection layer has a density greater than that of the low dielectric constant organic solvent and is poorly soluble or insoluble in the low dielectric constant organic solvent.
5. The double-needle electrospray device for constructing a femtosecond reactor according to claim 4, characterized in that: The collection layer is a deionized water layer.
6. The double-needle electrospray device for constructing a femtosecond reactor according to claim 3, characterized in that: The low dielectric constant organic solvent is n-hexane or cyclohexane.
7. The double-needle electrospray device for constructing a femtosecond reactor according to claim 1, characterized in that: The distance between the outlet ends of the first metal nozzle (7) and the second metal nozzle (8) is 3 to 5 cm.
8. The double-needle electrospray device for constructing a femtosecond reactor according to claim 3, characterized in that: A liquid outlet is arranged at the bottom of the product collecting container (9).