CN114100506A - Continuous flow synthesis method of coated nano magnetic particles - Google Patents
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Abstract
A continuous flow synthesis method of coated nano magnetic particles is characterized by comprising the following steps: step one, building a continuous reaction device, wherein the continuous reaction device comprises: the device comprises: an iron salt storage tank V1101, an alkali liquor storage tank V1102, a reaction kettle R1101 for preparing naked magnetic particles, an acid storage tank V1103, a sodium silicate storage tank V1104, a modification reaction kettle R1102 and a magnetic particle suspension storage tank V1105; the invention prepares the coated nano magnetic particles under the condition of normal temperature, and greatly reduces the preparation cost of the nano magnetic particles. And the stable, repeatable and macro preparation of the nano magnetic particles can be realized by utilizing the flow synthesis method, and the prepared nano magnetic particles have good size uniformity and crystallinity.
Description
Technical Field
The invention discloses a continuous flow synthesis method of coated nano magnetic particles, belongs to the field of preparation of functional magnetic particles, and particularly relates to a continuous flow synthesis method of coated nano magnetic particles.
Background
Nano magnetic particles are increasingly widely applied in many fields of modern science, such as biomedicine, magnetofluid, catalysis, nuclear magnetic resonance imaging, data storage, environmental protection and the like. The nano magnetic particles generally comprise a magnetic core made of metal oxides such as iron, cobalt, nickel and the like, and shells made of high molecular polymers, silicon, hydroxyapatite and the like and wrapped outside the magnetic core. The most common core layer is made of Fe with superparamagnetic or ferromagnetic properties3O4Or gamma-Fe2O3The magnetic guide film is made, has magnetic guidance (targeting), can realize directional movement under the action of an external magnetic field, is convenient to position and is convenient to combine with a mediumAnd (5) separating. The surface coating and modification of the inner core of the nano magnetic particle can not only enhance the stability of the nano magnetic particle, but also improve the stability, the dispersibility and the biocompatibility of the nano magnetic particle in aqueous solution, and further compound other nano particles, compounds or biological ligands to realize the functionalization of the nano magnetic particle. The technology of coating silicon oxide on the surfaces of the nano magnetic particles is one of modification methods in the preparation process of the magnetic particles, is favorable for the dispersion of the particles, and improves the weather resistance, acid resistance and wear resistance of the magnetic material.
The common method for coating the surface of the inner core of the nano-magnetic particle with silicon oxide is a sol-gel method. The sol-gel method needs organic solvent and organosilane, and the preparation cost is high. Although a method for coating silicon oxide on the surface of a nano magnetic particle inner core by using sodium silicate as a silicon source is reported (proceedings of Process engineering, 2002, 2(4) 319-324; patent 201410608653.8; patent 202011456805.9), the reported method firstly adopts a high-temperature (60-90 ℃) coprecipitation method to prepare the ferroferric oxide nano magnetic particle inner core, the ferroferric oxide nano magnetic particle inner core is washed and recovered by utilizing magnet separation, a product is ultrasonically dispersed in a sodium silicate solution, and then acid is added into the solution under the condition of stirring at high temperature (40-100 ℃) to adjust the pH value of a reaction system from alkalinity to neutrality. The product was separated by a magnet to obtain magnetic particles coated with silica on the surface. However, this method has the disadvantage of requiring high temperature conditions, resulting in high preparation cost, and is not suitable for large-scale preparation of magnetic particles.
Unlike the conventional batch synthesis, the continuous flow synthesis is a method in which a small amount of raw material is continuously supplied into a reactor to induce a synthesis reaction. The continuous flow synthesis process can mix various materials in the pipeline, the use of the pipeline mixer enables the mixing efficiency of the materials to be higher, the chemical reaction to be faster, and the reaction time to be obviously shortened. The continuous flow synthesis method has excellent mixing efficiency, greatly reduces the reaction time compared with the basic batch synthesis method, and can synthesize materials with high efficiency and high quality. The patent (202010462822.7) discloses a fluid method for the continuous preparation of iron oxide nanoparticle cores, but does not provide a coating method for the magnetic particles.
Disclosure of Invention
The invention aims to provide a continuous flow synthesis method of coated nano magnetic particles, which overcomes the defects of the prior art.
A continuous flow synthesis method of coated nano magnetic particles is characterized by comprising the following steps:
step one, building a continuous reaction device, wherein the continuous reaction device comprises: an iron salt storage tank V1101, an alkali liquor storage tank V1102, a reaction kettle R1101 for preparing naked magnetic particles, an acid storage tank V1103, a sodium silicate storage tank V1104, a modification reaction kettle R1102 and a magnetic particle suspension storage tank V1105;
a sampling pump P1101 and a feeding control valve FV-101 are arranged on an iron salt sample introduction channel connected with an iron salt storage tank V1101; a sampling pump P1102 and a feeding control valve FV-102 are arranged on an alkali liquor sample introduction channel connected with the alkali liquor storage tank V1102; feeding control valve FV-101 and feeding control valve FV-102 are both communicated into reactor R1101 through a channel;
a sampling pump P1105 and a feeding control valve FV-105 are arranged on an acid sample feeding channel connected with the acid storage tank V1103; a sampling pump P1104 and a feeding control valve FV-104 are arranged on a sodium silicate sample inlet channel connected with a sodium silicate storage tank V1104; the feeding control valve FV-105 and the feeding control valve FV-105 are both led into the reaction kettle R1102 through a channel;
a reaction kettle R1101 is connected with a reaction kettle R1102 through a control valve FV-103 and a sampling pump P1103; the reaction kettle R1102 is connected with a magnetic particle suspension storage tank V1105 through a channel by a control valve FV-106 and a sampling pump P1106;
step two, utilizing a continuous reaction device to carry out continuous reaction: firstly, iron salt solution is filled into an iron salt storage tank V1101, alkali solution is filled into an alkali solution storage tank V1102, the mixture is pumped into a reaction kettle R1101 after being mixed by a pipeline mixer to prepare Fe3O4The pH value of the mixed iron salt solution and alkali solution in a reaction kettle R1101 is controlled to be 7.5-13.5, preferably 9.5-12, and the average residence time is 5min-2 h;
step three, Fe obtained in the step two3O4Mixing the nano particles with a sodium silicate solution and an acid solution in sequence through a pipeline mixer, pumping the mixture into a reaction kettle R1102, and preparing Fe3O4@SiO2A nanoparticle; fe3O4The pH value of the mixed nano magnetic particles, sodium silicate solution and acid solution in the reaction kettle R1102 is controlled to be 0.5-4, preferably 1.5-3.5, and the average residence time is 10min-4 h.
And pH meters are arranged in the reaction kettle R1101 and the modification reaction kettle R1102 and used for monitoring the pH of the reaction, the pH meters are connected with an automatic control system, and the automatic control system automatically regulates and controls the sampling flow rate of the acid and the alkali liquor according to the set pH value. The whole reaction process is finished at normal temperature and normal pressure without the protection of inert gas.
The acid in the second step and the third step is selected from one of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid or acetic acid.
The alkali solution is one of sodium hydroxide solution and ammonia water.
The molysite solution is prepared from the following components in a molar ratio of 2: 1, a mixed solution of a ferric salt and a ferrous salt;
prepared Fe3O4The nano particles directly enter into Fe without magnetic separation and washing process3O4@SiO2And (3) preparation process of the nano particles.
Technical advantages of the invention
The method for synthesizing the nano magnetic particles in the prior art generally needs high temperature conditions, so that the preparation cost is high, and the method is not suitable for large-scale preparation of the magnetic particles. The invention prepares the coated nano magnetic particles under the condition of normal temperature, and greatly reduces the preparation cost of the nano magnetic particles. And the stable, repeatable and macro preparation of the nano magnetic particles can be realized by utilizing the flow synthesis method, and the prepared nano magnetic particles have good size uniformity and crystallinity.
The scheme is different from the traditional technical scheme depending on high-temperature conditions, and is beneficial to reducing the preparation cost of the nano magnetic particles. The stable, repeatable and macro preparation of the magnetic nanoparticles can be realized by utilizing the flow synthesis method, and the prepared magnetic nanoparticles have good size uniformity.
Drawings
FIG. 1 is a schematic view of a reaction apparatus according to the present invention;
FIG. 2 Fe prepared in example 2 of the present invention3O4And Fe3O4@SiO2An infrared test result graph of the nanoparticles;
FIG. 3 Fe obtained in example 3 of the present invention3O4@SiO2Transmission electron microscopy of nanoparticles.
Detailed Description
A continuous flow synthesis method of coated nano magnetic particles is characterized by comprising the following steps:
the method comprises the following steps: a continuous reaction apparatus was constructed according to FIG. 1, the apparatus comprising: molysite storage tank, alkali lye storage tank, No. 1 reation kettle, sodium silicate storage tank, sour storage tank, No. 2 reation kettle, magnetic particle turbid liquid storage tank. The sampling channels are provided with sampling pumps and feeding control valves, and the outlets of the sampling channels are communicated with the reactors to form a pipeline mixer so as to mix reagents flowing out of various channels. The reaction kettle is internally provided with a pH meter for monitoring the pH value of the reaction, the pH meter is connected with an automatic control system, and the sample injection flow rate of the acid and alkali liquor can be automatically regulated according to the set pH value.
Step two: firstly, mixing ferric salt and alkali through a pipeline mixer and pumping the mixture into a No. 1 reaction kettle to prepare Fe by utilizing a continuous reaction device3O4The number of the nano-particles is,
step three: then mixing the nano magnetic particles with sodium silicate and acid in sequence through a pipeline mixer, and pumping the mixture into a No. 2 reaction kettle to prepare Fe3O4@SiO2And (3) nanoparticles.
Wherein, in the second step, the pH value of the mixture of the ferric salt and the alkali in the No. 1 reaction kettle is controlled to be 7.5-13.5, and the average residence time is 5min-2 h. Fe3O4The pH value of the mixed nano particles, sodium silicate and acid in the No. 2 reaction kettle is controlled to be 0.5-4, and the average residence time is 10min-4 h.
Prepared Fe3O4The nano particles directly enter into Fe without magnetic separation and washing process3O4@SiO2And (3) preparation process of the nano particles.
The whole reaction process is finished at normal temperature and normal pressure without the protection of inert gas.
In a word, a sampling pump and a feeding control valve are arranged on the sample feeding channel, and a pipeline mixer is communicated between the outlets of the sample feeding channels and the reactor so as to mix reagents flowing out of various channels. The reaction kettle is internally provided with a pH meter for monitoring the pH value of the reaction, the pH meter is connected with an automatic control system, and the sample injection flow rate of the acid and alkali liquor can be automatically regulated according to the set pH value.
Example 1 flow Synthesis apparatus
Referring to fig. 1, the flow synthesis apparatus of this embodiment includes a ferric salt storage tank, an alkali liquor storage tank, No. 1 reaction kettle, a sodium silicate storage tank, an acid storage tank, No. 2 reaction kettle, and a magnetic particle suspension storage tank. The sampling channels are provided with sampling pumps and feeding control valves, and the outlets of the sampling channels are communicated with the reactors to form a pipeline mixer so as to mix reagents flowing out of various channels. The reaction kettle is internally provided with a pH meter for monitoring the pH value of the reaction, the pH meter is connected with an automatic control system, and the sample injection flow rate of the acid and alkali liquor can be automatically regulated according to the set pH value.
The automatic control system can be realized by adopting the existing computer, industrial personal computer or microcontroller; the sampling valve and the sampling pump can adopt the existing metering valve and metering pump, and the control of the metering valve and the metering pump is the prior art; the material of the reaction kettle comprises one or more of hastelloy, 316L stainless steel, glass, Polydimethylsiloxane (PDMS) and ceramic. The pipeline mixer can adopt the prior T-shaped, Y-shaped or static mixer and is used for mixing a plurality of raw materials to form mixed reaction solution, and then the mixed reaction solution is introduced into the reactor for reaction.
Example 2 flow Synthesis method
Firstly, 70kg of ferric chloride hexahydrate and 25.8kg of ferrous chloride tetrahydrate are dissolved in 400L of water, ferric salt and sodium hydroxide solution are mixed by a pipeline mixer by using a continuous reaction device and then pumped into a No. 1 reaction kettle, the pH value of the mixed ferric salt and sodium hydroxide solution in the No. 1 reaction kettle is controlled to be 7.5, the average residence time is 2 hours, and Fe is prepared3O4And (3) nanoparticles.
Mixing Fe3O4Mixing the nano particles with sodium silicate and hydrochloric acid in sequence through a pipeline mixer, pumping into a No. 2 reaction kettle, controlling the pH of a mixing system in the reaction kettle to be 0.5, and controlling the average residence time to be 10min to prepare Fe3O4@SiO2And (3) nanoparticles.
Example 3 flow Synthesis method
Firstly, 70kg of ferric chloride hexahydrate and 25.8kg of ferrous chloride tetrahydrate are dissolved in 400L of water, ferric salt and ammonia water are mixed by a pipeline mixer by using a continuous reaction device and then pumped into a No. 1 reaction kettle, the pH value of the mixture of the ferric salt and the ammonia water in the No. 1 reaction kettle is controlled to be 13.5, the average residence time is 5min, and Fe is prepared3O4And (3) nanoparticles.
Mixing Fe3O4Mixing the nano particles with sodium silicate and nitric acid in sequence through a pipeline mixer, pumping into a No. 2 reaction kettle, controlling the pH value of a mixing system in the reaction kettle to be 4, and controlling the average residence time to be 4h to prepare Fe3O4@SiO2And (3) nanoparticles.
Example 4 flow Synthesis method
Firstly, 70kg of ferric chloride hexahydrate and 25.8kg of ferrous chloride tetrahydrate are dissolved in 400L of water, ferric salt and ammonia water are mixed by a pipeline mixer by using a continuous reaction device and then pumped into a No. 1 reaction kettle, the pH value of the mixture of the ferric salt and the ammonia water in the No. 1 reaction kettle is controlled to be 10, the average residence time is 1h, and Fe is prepared3O4And (3) nanoparticles.
Mixing Fe3O4Mixing the nano particles with sodium silicate and sulfuric acid in sequence through a pipeline mixer, pumping into a No. 2 reaction kettle, controlling the pH of a mixing system in the reaction kettle to be 2.5, and controlling the average residence time to be 2h to prepare Fe3O4@SiO2And (3) nanoparticles.
Example 5
A continuous flow synthesis method of coated nano magnetic particles comprises the following steps:
step one, a flow synthesis device is built according to the attached figure 1, and the device comprises: the device comprises a V1101 iron salt storage tank, a V1102 alkali liquor storage tank, a R1101 bare magnetic particle preparation reaction kettle, a V1103 acid storage tank, a V1104 sodium silicate storage tank, a R1102 modification reaction kettle and a V1105 magnetic particle suspension storage tank.
A sampling pump P1101 and a feeding control valve FV-101 are arranged on the ferric salt sample injection channel, a sampling pump P1102 and a feeding control valve FV-102 are arranged on the alkali liquor sample injection channel, a sampling pump P1105 and a feeding control valve FV-105 are arranged on the acid sample injection channel, a sampling pump P1104 and a feeding control valve FV-104 are arranged on the sodium silicate sample injection channel, and the naked magnetic particles enter the reaction kettle R1102 from the reaction kettle R1101 through the control valve FV-103 and the sampling pump P1103. The modified nano magnetic particles enter a magnetic particle suspension storage tank V1105 through a control valve FV-106 and a sampling pump P1106. In a word, a sampling pump and a feeding control valve are arranged on the sample feeding channel, and a pipeline mixer is communicated between the outlets of the sample feeding channels and the reactor so as to mix reagents flowing out of various channels. The reaction kettle is internally provided with a pH meter for monitoring the pH value of the reaction, the pH meter is connected with an automatic control system, and the sample injection flow rate of the acid and alkali liquor can be automatically regulated according to the set pH value.
Step two, utilizing a continuous reaction device, firstly mixing ferric salt and alkali through a pipeline mixer, and pumping into a No. 1 reaction kettle to prepare Fe3O4The pH value of the nano particles, the iron salt and the alkali after being mixed in the No. 1 reaction kettle is controlled to be 7.5-13.5, and the average residence time is 5min-2 h. Preferably, the molar ratio of the ferric salt solution is 2: 1 of a mixed solution of a ferric salt and a ferrous salt. The alkali is one of sodium hydroxide solution and ammonia water. Prepared Fe3O4The nano particles can directly enter into Fe without magnetic separation and washing processes3O4@SiO2And (3) preparation process of the nano particles.
Step three, adding Fe3O4Mixing the nano particles with sodium silicate and acid in sequence through a pipeline mixer, and pumping the mixture into a No. 2 reaction kettle to prepare Fe3O4@SiO2The pH value of the mixed nano particles, the nano magnetic particles, the sodium silicate and the acid in the No. 2 reaction kettle is controlled to be 0.5-4, and the average residence time is 10min-4 h. Preferably, the acid is selected from one of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid or acetic acid. The whole reaction process is finished at normal temperature and normal pressure without the protection of inert gas.
Claims (10)
1. A continuous flow synthesis method of coated nano magnetic particles is characterized by comprising the following steps:
step one, building a continuous reaction device, wherein the continuous reaction device comprises: an iron salt storage tank V1101, an alkali liquor storage tank V1102, a reaction kettle R1101 for preparing naked magnetic particles, an acid storage tank V1103, a sodium silicate storage tank V1104, a modification reaction kettle R1102 and a magnetic particle suspension storage tank V1105;
a sampling pump P1101 and a feeding control valve FV-101 are arranged on an iron salt sample introduction channel connected with an iron salt storage tank V1101; a sampling pump P1102 and a feeding control valve FV-102 are arranged on an alkali liquor sample introduction channel connected with the alkali liquor storage tank V1102; feeding control valve FV-101 and feeding control valve FV-102 are both communicated into reactor R1101 through a channel;
a sampling pump P1105 and a feeding control valve FV-105 are arranged on an acid sample feeding channel connected with the acid storage tank V1103; a sampling pump P1104 and a feeding control valve FV-104 are arranged on a sodium silicate sample inlet channel connected with a sodium silicate storage tank V1104; the feeding control valve FV-105 and the feeding control valve FV-105 are both led into the reaction kettle R1102 through a channel;
a reaction kettle R1101 is connected with a reaction kettle R1102 through a control valve FV-103 and a sampling pump P1103; the reaction kettle R1102 is connected with a magnetic particle suspension storage tank V1105 through a channel by a control valve FV-106 and a sampling pump P1106;
step two, utilizing a continuous reaction device to carry out continuous reaction: firstly, iron salt solution is filled into an iron salt storage tank V1101, alkali solution is filled into an alkali solution storage tank V1102, the mixture is pumped into a reaction kettle R1101 after being mixed by a pipeline mixer to prepare Fe3O4The pH value of the mixed iron salt solution and alkali solution in a reaction kettle R1101 is controlled to be 7.5-13.5, preferably 9.5-12, and the average residence time is 5min-2 h;
step three, Fe obtained in the step two3O4Mixing the nano particles with a sodium silicate solution and an acid solution in sequence through a pipeline mixer, pumping the mixture into a reaction kettle R1102, and preparing Fe3O4@SiO2A nanoparticle; fe3O4Reaction of nano magnetic particle, sodium silicate solution and acid solutionThe pH value of the mixture in the reactor R1102 is controlled to be 0.5-4, preferably 1.5-3.5, and the average residence time is 10min-4 h.
2. The continuous flow synthesis method of coated nano-magnetic particles as claimed in claim 1, wherein pH meters are disposed in the reaction vessel R1101 and the modification reaction vessel R1102 for monitoring pH of the reaction, the pH meters are connected to an automatic control system, the automatic control system automatically controls the flow rates of the acid and alkali solutions according to the set pH values, and the whole reaction process is completed at normal temperature and pressure without inert gas protection.
3. The method for continuous flow synthesis of coated nano-magnetic particles as claimed in claim 1 or 2, wherein the acid in step two and step three is selected from one of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid or acetic acid.
4. The continuous flow synthesis method of coated nano-magnetic particles as claimed in claim 1 or 2, wherein the alkali solution is one of sodium hydroxide solution and ammonia water.
5. The continuous-flow synthesis method of coated nano-magnetic particles as claimed in claim 3, wherein the alkali solution is one of sodium hydroxide solution and ammonia water.
6. The continuous-flow synthesis method of coated nano-magnetic particles as claimed in claim 1 or 2, wherein the molar ratio of the ferric salt solution is 2: 1 of a mixed solution of a ferric salt and a ferrous salt.
7. The continuous-flow synthesis method of coated nano-magnetic particles as claimed in claim 5, wherein the molar ratio of the ferric salt solution is 2: 1 of a mixed solution of a ferric salt and a ferrous salt.
8.The continuous-flow synthesis method of coated nano-magnetic particles as claimed in claim 1 or 2, wherein the prepared Fe3O4The nano particles directly enter into Fe without magnetic separation and washing process3O4@SiO2And (3) preparation process of the nano particles.
9. The continuous flow synthesis method of the coated nano magnetic particles as claimed in claim 1 or 2, wherein the pH of the iron salt solution and the alkali solution mixed in the reaction kettle R1101 in the step two is controlled to be 9.5-12.
10. The continuous-flow synthesis method of coated nano-magnetic particles as claimed in claim 1 or 2, wherein the Fe in step three3O4And the pH value of the mixed nano magnetic particles, sodium silicate solution and acid solution in the reaction kettle R1102 is controlled to be 1.5-3.5.
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