CN111014720A - Method and device for synthesizing nano silver on line - Google Patents

Method and device for synthesizing nano silver on line Download PDF

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Publication number
CN111014720A
CN111014720A CN201911371313.7A CN201911371313A CN111014720A CN 111014720 A CN111014720 A CN 111014720A CN 201911371313 A CN201911371313 A CN 201911371313A CN 111014720 A CN111014720 A CN 111014720A
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nano silver
silver
injector
extract
platycladus orientalis
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苑春刚
刘晨晨
王厚宇
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North China Electric Power University
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North China Electric Power University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

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Abstract

A method for synthesizing nano silver on line selects arborvitae extract to react with silver nitrate solution to prepare nano silver, comprising the following steps: cleaning Platycladus orientalis, placing on tin foil paper, oven drying, grinding, weighing Platycladus orientalis powder, placing in a container, adding purified water, boiling under magnetic stirring, cooling, centrifuging, collecting supernatant, and filtering to obtain Platycladus orientalis extractive solution; respectively filling the platycladus orientalis extract and the silver nitrate solution into two injectors, pushing the injectors by a push-pull injection pump, and continuously injecting the platycladus orientalis extract and the silver nitrate solution into a polytetrafluoroethylene tube through a three-way valve for mixing; the polytetrafluoroethylene tube is arranged in the heating device in an extending way, and the mixed solution of the arborvitae extract and the silver nitrate solution is subjected to reduction reaction in the heating device to generate the nano silver. The invention realizes the on-line rapid synthesis of nano silver synthesized by the arborvitae by using an injection pump continuous sample injection method and taking on-line water bath or microwave as a heating control unit, shortens the synthesis time to be within 4min, and has convenient installation and simple disassembly.

Description

Method and device for synthesizing nano silver on line
Technical Field
The invention relates to a method for synthesizing nano silver, in particular to a method and a device for synthesizing nano silver on line.
Background
The nano gold/silver has good application prospect in the fields of medicine, optics and biology due to the unique physical and chemical properties of the nano gold/silver. The widespread use of nanomaterials has at least two negative impacts on our environment. The first is that toxic chemical reagents are inevitably used in the synthesis process, and the second is that the nano particles are released into the environment after being used, and directly affect the biological groups. Therefore, it is important to find green and benign nanoparticle synthesis methods. At present, the synthesis method of nano silver mainly comprises a physicochemical method and a biological synthesis method. The instrument and equipment for synthesizing the nano silver by the physical and chemical method are complex, the synthesis cost is high, toxic and harmful chemical reagents are required to be used, and the environment and the applied materials are influenced to a certain extent; the biosynthesis technology is a new type of nanometer material preparation technology which appears recently, and comprises a microbial synthesis method and a plant reduction method, wherein the microbial synthesis method has high operation requirement, complex equipment, long microbial growth period and easy breeding of microbial hazards; in contrast, the advantages of the plant body reduction method are shown, the plant extracting solution is used for preparing the nano silver, the extracting solution simultaneously plays the dual functions of the reducing agent and the stabilizing agent, strong acid, strong alkali and toxic and harmful chemical reagent solvents are not needed in the process, the preparation conditions are mild, the raw materials are low in price and easy to obtain, the synthesis efficiency is high, the environment is friendly and safe, the prepared nano material is good in dispersity and strong in stability, and the method is suitable for preparing the nano silver on a large scale in a short time. However, each step of the existing plant synthesis method needs independent operation, the nano silver can not be synthesized in a linkage manner, the synthesis efficiency is low, and other impurities are easily doped in the synthesis process to influence the purity of the nano silver.
Disclosure of Invention
The invention provides a method and a device for synthesizing nano silver on line, which overcome the defects of the prior art, realize the on-line rapid synthesis of the nano silver synthesized by plants by using an on-line water bath or microwave as a heating control unit by using a method of continuous sample injection by using a syringe pump, shorten the synthesis time to be within 4min, have convenient installation and simple disassembly, and are suitable for industrial production.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for synthesizing nano silver on line adopts a plant reduction method to synthesize nano silver, selects a biota orientalis extract to react with a silver nitrate solution to prepare the nano silver, and comprises the following steps:
a. preparation of arborvitae powder: cleaning branches and leaves of Chinese arborvitae, placing on tin foil paper, oven drying in oven at 55 deg.C for 12 hr, grinding, and placing Chinese arborvitae powder in a sealed bag;
b. preparing a arborvitae extract: weighing Platycladus orientalis powder, placing in a container, adding purified water, boiling under magnetic stirring, cooling, centrifuging, collecting supernatant, and filtering to obtain Platycladus orientalis extractive solution;
c. respectively filling the platycladus orientalis extract and a silver nitrate solution into a first injector and a second injector, pushing the injectors by a push-pull injection pump, and continuously injecting the platycladus orientalis extract and the silver nitrate solution into a polytetrafluoroethylene tube through a three-way valve for mixing to form a platycladus orientalis extract and silver nitrate solution mixed solution;
d. heating and reacting: the polytetrafluoroethylene tube is arranged in the heating device in an extending way, and the mixed solution of the platycladus orientalis extract and the silver nitrate solution is subjected to reduction reaction in the heating device to generate nano silver;
e. and the synthesized nano silver continuously flows out from the liquid outlet end of the polytetrafluoroethylene tube, is collected and is cooled to obtain the product nano silver.
According to the method for synthesizing the nano silver on line, the concentration of the platycladus orientalis extracting solution is 1.0-1.8g/100mL, and the concentration of the silver nitrate solution is 10-16 mmol.
In the method for synthesizing nano silver on line, the injection speed in the step c is 2.33-3.11mL/min, and the total length of the polytetrafluoroethylene tube is 15-25 m.
In the method for synthesizing the nano silver on line, the heating mode in the step d is water bath heating or microwave heating, and the heating temperature is 60-90 ℃.
The device comprises a push-pull injection pump, a first injector, a second injector, a three-way valve, a polytetrafluoroethylene tube, a heating device and a collecting container, wherein the first injector and the second injector are fixedly mounted on the push-pull injection pump through pressing sheets, piston core rods of the first injector and the second injector are both connected with a sliding sheet on the push-pull injection pump, the sliding sheet simultaneously pushes two piston core rods, the front ends of the two needle cylinders are connected with the polytetrafluoroethylene tube through the three-way valve, the polytetrafluoroethylene tube is wound in the heating device, and the liquid outlet end of the polytetrafluoroethylene tube is connected with the collecting container.
In the device for synthesizing nano silver on line, the heating device is a water bath or a microwave oven.
In the device for synthesizing nano silver on line, the collecting container is a test tube and is placed in a beaker, and ice blocks are also filled in the beaker.
In the device for synthesizing nano silver on line, the microwave oven is also internally provided with a rotating disk, and the polytetrafluoroethylene tube is wound on the rotating disk.
According to the device for synthesizing the nano silver on line, the volume models of the first injector and the second injector are the same.
The invention has the beneficial effects that: according to the invention, the platycladus orientalis extract and the silver nitrate solution in the injector are continuously injected into the polytetrafluoroethylene tube by adopting a push-pull injection pump, the mixed solution in the polytetrafluoroethylene tube is heated in a water bath heating or microwave heating mode, so that the platycladus orientalis extract and the silver nitrate solution are subjected to reduction reaction to generate nano silver, the nano silver continuously flows out from the liquid outlet, the injection speed and the heating temperature are controlled, the nano silver is continuously synthesized, the whole synthesis process is continuously carried out, the synthesis time is controlled within 4min, the synthesis time is greatly shortened, and the synthesis efficiency is improved; air is isolated in the synthesis process, and no interference of other substances exists, so that the nano silver is purer.
Drawings
The invention will be further explained with reference to the drawings.
FIG. 1 is a schematic view of the overall structure of the water bath heating system of the present invention;
FIG. 2 is a schematic view of the structure inside the water bath;
FIG. 3 is a schematic view of the overall structure of microwave heating;
FIG. 4 is a schematic view of the structure inside the microwave oven;
FIG. 5 is a UV-VIS spectrum of a nanosilver-containing solution prepared with silver nitrate of different concentrations;
FIG. 6 is a UV-VIS spectrum of a nano-silver-containing solution prepared from Platycladus orientalis extractive solutions of different concentrations;
FIG. 7 is a graph of the UV-Vis spectra of the nanosilver-containing solutions prepared at different water bath heating temperatures;
FIG. 8 is a UV-VIS spectrum of nano-silver containing solutions prepared at different injection speeds;
FIG. 9 is a UV-VIS spectrum of nano-silver containing solutions prepared at different tube lengths;
FIG. 10 is a diagram of catalytic degradation performance of nano-silver degradation pollutants synthesized under optimal conditions;
FIG. 11 is a chromatogram of an ultraviolet spectrophotometer for preparing a nano-silver solution by reducing silver nitrate with different plant extracts.
In the figure: 1. push-pull injection pump; 1-1, tabletting; 1-2, sliding sheets; 2. a first syringe; 3. a second syringe; 4. a three-way valve; 5. a polytetrafluoroethylene tube; 6. a heating device; 6-1, rotating the disc; 7. and (4) collecting the container.
Detailed Description
The invention will be further explained with reference to the drawings.
The invention discloses a method for preparing extracting solutions of biota orientalis with different concentrations, which comprises the following steps: picking branches and leaves of biota orientalis, cleaning, placing on tin foil paper, placing in an oven, drying at 55 ℃ for 12h, after the branches and leaves of the biota orientalis are dried and become crisp, placing in a pulverizer for grinding, weighing 1.0-1.8g of the ground biota orientalis powder respectively, placing in different beakers, adding 150mL of purified water into the beakers respectively, boiling to 100mL on a magnetic stirrer, cooling, centrifuging the liquid, taking supernatant, and filtering to obtain biota orientalis extracting solution with the concentration of 1.0-1.8g/100mL respectively.
Example 1
Adopting a water bath heating mode to synthesize nano silver on line, as shown in figures 1 to 2, selecting a biota orientalis extracting solution with the concentration of 1.2g/100mL to be placed in a first injector 2, taking a silver nitrate solution with the same volume as 10mmol to be placed in a second injector 3, fixing the first injector 2 and the second injector 3 on a push-pull injection pump 1 through a tabletting 1-1, setting the water bath heating temperature of a water bath kettle to be 80 ℃, setting the injection speed of the push-pull injection pump 1 to be 2.33mL/min, selecting the pipe length of a polytetrafluoroethylene pipe 5 to be 20m, synthesizing the nano silver, enabling the synthesized nano silver-containing solution to flow into a collecting container 7 (test tube), and cooling through ice blocks to enable the synthesized nano silver to be stabilized in the optimal synthesis state. In the same step, the concentrations of the silver nitrate solution are changed to 12mmol, 14mmol and 16mmol respectively to synthesize nano silver, and the prepared nano silver solution is subjected to chromatographic determination through ultraviolet-visible (UV-vis) absorption spectrum.
Under the condition that the concentration, the injection speed, the heating temperature and the tube length of the platycladus orientalis extract are fixed, the characteristic SPR absorption wavelength of the silver nanoparticles is about 415nm along with the reaction, and the absorbance is continuously increased; using the same volume and concentration of the extract of biota orientalis to prepare AgNO3The concentration of (2) was increased to 12mmol, and the generation of silver nanoparticles was detected by UV-vis absorption spectroscopy, and it can be seen from FIG. 5 that the SPR absorption wavelength of silver nanoparticles was about 415nm and the absorbance was increased with the increase of silver nitrate concentration, compared to 10mmol of AgNO3SPR peak absorbance of the silver nano-particles after stabilization, 12mmolAgNO3The final SPR peak absorbance of the obtained silver nano-particles is improved, which shows that the concentration of the silver nano-particles is greatly improved, and also proves that the extracting solution also contains enough reducing substances to reduce AgNO3Then AgNO is added3The concentration of the silver nanoparticles is increased to 14mmol, the SPR absorption wavelength of the silver nanoparticles is still about 415nm, the absorbance is continuously increased, the peak shape is obvious compared with the peak shape of the nano silver synthesized by silver nitrate with the concentration of 10mmol and 12mmol, and AgNO is added3The concentration of the silver nanoparticles is increased to 16mmol, the SPR absorption wavelength of the silver nanoparticles is still about 415nm, the absorbance is continuously increased, and the peak value fluctuates due to overhigh concentration of silver nitrate, so that the silver nitrate is excessively concentrated, the reducing agent for reaction is far from enough, the nano silver particles obtained by reaction are few, and the shape is irregular. As described above, the optimum silver nitrate concentration was 14 mmol.
Example 2
Selecting silver nitrate solution with concentration of 14mmol, water bath heating temperature of 80 deg.C, injection speed of 2.33mL/min, polytetrafluoroethylene tube 5 with length of 20m, changing the concentration of the extract of Platycladus orientalis to 1.0g/100mL, 1.2g/100mL, 1.4g/100mL, 1.6g/100mL and 1.8g/100mL respectively, and performing ultraviolet-visible spectrophotometer to perform chromatographic determination on the prepared nano silver solution.
Under the conditions that the concentration of a silver nitrate solution, the injection speed, the heating temperature and the tube length are fixed, the concentration of the platycladus orientalis extracting solution is changed, the characteristic SPR absorption wavelength of the silver nanoparticles is about 415nm along with the reaction, and the absorbance is continuously increased; as can be seen from FIG. 6, with the increase of the concentration of the arborvitae extract, the SPR absorption wavelength of the silver nanoparticles is about 415nm, the absorbance is increased, and compared with the stable SPR peak absorbance of the silver nanoparticles obtained from the arborvitae extract with the concentration of 1g/100mL, the final SPR peak absorbance of the silver nanoparticles obtained from the arborvitae with the concentration of 1.2g/100mL is increased, which shows that the concentration of the silver nanoparticles is greatly increased, and also shows that the extract also contains enough reducing substances to reduce AgNO3Then, the concentration of the extracting solution is increased, the SPR absorption wavelength of the nano-particles is still about 415nm, the absorbance is continuously increased, the peak shape is obvious compared with the peak shape of nano-silver synthesized by using the biota orientalis with the concentration of 1.0g/100mL and 1.2g/100mL, the concentration of the extracting solution is increased, the SPR absorption wavelength of the silver nano-particles is still about 415nm, the absorbance is continuously increased, and the peak value fluctuates due to overhigh concentration of the biota orientalis extracting solution, because the concentration of the extracting solution is overhigh, the concentration of the contained reducing agent is overhigh, and the shape is irregular. As described above, the extract was obtained at an optimum concentration of 1.4g/100mL of biota orientalis.
Example 3
Selecting silver nitrate solution with concentration of 14mmol, Chinese arborvitae extract with concentration of 1.4g/100mL, injection speed of 2.33mL/min, selecting polytetrafluoroethylene tube 5 with length of 20m, reacting at 60 deg.C, 70 deg.C, 80 deg.C and 90 deg.C while changing water bath heating temperature, and performing ultraviolet-visible spectrophotometer for chromatographic determination. As can be seen from fig. 7, when the temperature is 60 ℃, the absorbance of the nano silver synthesized by the reaction is not high and the peak shape is not obvious, the characteristic SPR absorption wavelength of the silver nano particle is about 420nm with the increase of the temperature, the absorbance is continuously increased, the reaction speed is very stable, but the absorption peak is wide, the characteristic SPR absorption wavelength of the silver nano particle is about 420nm under the condition of the temperature of 90 ℃, the absorption peak of the nano silver is always stable at 420nm without shift and has a narrow peak width, the particle size distribution of the obtained nano particle is narrow, and if the temperature is higher than 90 ℃, the reaction is too fast and the change of the absorption spectrum cannot be detected. In summary, the optimal reaction temperature for the synthesis process is 90 ℃.
Example 4
Selecting silver nitrate solution with concentration of 14mmol, Chinese arborvitae extract with concentration of 1.4g/100mL, heating in water bath at 90 deg.C, selecting polytetrafluoroethylene tube 5 with length of 20m, changing injection speed to 2.33mL/min, 2.66mL/min, and 3.1mL/min, and performing ultraviolet-visible spectrophotometer for chromatographic determination. As can be seen from fig. 8, at three speeds, the characteristic SPR absorption wavelength of the synthesized nanoparticles is about 420nm as detected by an ultraviolet spectrophotometer, the synthesized nanoparticles are stable at a push-pull injection pump speed of 2.66ml/min, the absorption peak of the nano-silver is always stable at 420nm, no shift occurs, the peak width is narrow, and the obtained nanoparticles have narrow particle size distribution. In summary, the optimal push-pull syringe pump speed for the synthetic procedure was 2.66 ml/min.
Example 5
Selecting silver nitrate solution with concentration of 14mmol, arborvitae extract with concentration of 1.4g/100mL, heating in water bath at 90 deg.C, injecting at 2.66mL/min, changing the tube length of polytetrafluoroethylene tube to 15m, 20m and 25m, and performing ultraviolet-visible spectrophotometer for chromatographic determination. As can be seen from fig. 8, when the length of the teflon tube is 15m, the synthesized nanoparticles are detected by an ultraviolet spectrophotometer, and the characteristic SPR absorption wavelength of the silver nanoparticles is about 420nm, the absorbance is not high, the peak shape is wide, and it may be that the length of the teflon tube is too short, the synthesis space is not sufficient, the synthesized nanoparticles are few, and the shape is irregular. When the length of the polytetrafluoroethylene tube is 25m, the synthesized nanoparticles are detected by an ultraviolet spectrophotometer, the characteristic SPR absorption wavelength of the silver nanoparticles is about 420nm, the length of the synthesized tube is too long, the synthesis time is longer than the former two types, and the peak of the synthesized nanoparticles is wider and shifts when the length of the synthesized nanoparticle is 20m longer than that of the polytetrafluoroethylene tube. When the length of the polytetrafluoroethylene tube is 20m, the absorption peak is narrow, the absorbance is highest, no deviation exists, and the particle size distribution of the obtained nanoparticles is narrow. In summary, the preferred polytetrafluoroethylene tube length is 20 m.
(I) testing the catalytic performance of the nano-silver prepared by the synthetic method of the invention
The catalytic degradation test is carried out on the nano silver synthesized under the conditions that the concentration of a silver nitrate solution is 14mmol, the concentration of a platycladus orientalis extracting solution is 1.4g/100mL, the water bath heating temperature is 90 ℃, the injection speed is 2.66mL/min and the tube length is 20 m. Generally, sodium borohydride is used as a reducing agent to degrade nitroaromatic compounds. The catalytic performance of the silver nanoparticles in a pseudo-homogeneous system is investigated by taking the catalytic degradation of tetranitrophenol (4-NP) to tetraaminophenol (4-AP) as a reaction model. Preparation of 20mM 4-NP solution, 5M NaBH4Simultaneously, 2mM of fresh nano-silver sol was prepared. A typical experiment is: 2.76 mL of deionized water was put into a quartz cuvette of 1cm × 1cm, 20uL of 4-NP solution (20 mM) and 200 uL of NaBH solution (5M) were added, and 20uL of nano-silver sol prepared from biota orientalis was added to the mixture, the total volume of the reaction system was 3mL each time, and UV-vis absorption spectra were measured at 0, 3, 6, 9, 12, 15, 18 and 21 minutes after the reaction with gentle stirring. As can be seen from FIG. 10, when NaBH was added to the 4-NP solution44-NP and Na when reducing with an extract of biota orientalis to obtain a silver sol+The absorption peak generated at 400nm in combination slowly decreased until it disappeared, while the absorption peak of 4-AP appeared at about 313 nm. The result shows that the catalytic degradation of the nano-silver can be completed within 21min generally under the room temperature condition, which shows that the nano-silver has good catalytic effect. While the silver sol was replaced by the biota powder, there was still a characteristic peak at about 400 nm. Therefore, silver nanoparticles prepared by the reduction of the arborvitae powder can catalyze the conversion of 4-NP to 4-AP, the catalytic conversion of 4-NP to 4-AP cannot be realized by only adding the arborvitae powder extracting solution, and the catalytic degradation of 4-NP to 4-AP can be selected as a nano silver catalyst for evaluating biosynthesisModel reaction of activity.
(II) the invention selects the arborvitae extract as the experimental verification of reducing silver nitrate
Respectively picking branches and leaves of different plants, drying and crushing, and the steps are the same as the preparation method of the arborvitae powder.
Weighing 1g of powder of ilex chinensis, cedar, willow, poplar, ginkgo biloba, white bark pine, platycladus orientalis, sabina chinensis, spruce, persimmon, jujube, shaddock peel, chenopodium, kochia scoparia stem and Lala seedling in a beaker by using an electronic balance respectively. In the weighing process, each plant is provided with a unique weighing scoop and cannot be mixed, so that the interference of reducing components in other plants on the experimental result is avoided. 150mL of Wahaha purified water is added into each beaker, and the mixture is boiled to 100mL on a magnetic stirring instrument. And pouring the cooled liquid into a 50mL centrifuge tube, and centrifuging in a high-speed centrifuge at the set time of 20min and the rotating speed of 6000 r. Filtering the supernatant with qualitative filter paper, and filtering the obtained filtrate with 0.1 μm microfiltration filter paper to obtain various plant extractive solutions. 10mL of the plant extract was placed in a 15mL centrifuge tube, and 400. mu.L of 100mmol of silver nitrate standard solution was added to the centrifuge tube.
The centrifuge tube was placed on a vortex mixer and shaken, then placed in a digital display thermostatted water bath and heated, set at 70 ℃. And (3) diluting the solution containing the nano silver by a certain factor at intervals, and performing spectral scanning on an ultraviolet spectrophotometer. The data from the experiment are plotted in FIG. 11. As can be seen from FIG. 11, the effect of cedar is the best, and the cedar reducing effect is affected by seasonal factors, so that the cedar is selected as the extracting solution to reduce the silver nitrate in the experiment.
The water bath heating of the invention can also be replaced by microwave heating, referring to fig. 3 to 4, the polytetrafluoroethylene tube enters the microwave oven from the left hole of the microwave oven and exits the microwave oven from the right hole, the left hole and the right hole are both sealing rotary tables, the polytetrafluoroethylene tube in the microwave oven is coiled on the rotary table 6-1 in the microwave oven, and the rotary table is rotated in the heating process, so that the mixed liquid is heated more uniformly in the microwave oven. The heating temperature and time are set by using a firepower adjusting knob and a time adjusting knob on the microwave oven. Experiments prove that the synthesis time of synthesizing the nano-silver by microwave heating can be shortened to be within 2min, and the synthesis efficiency is greatly improved.

Claims (9)

1. The method for synthesizing the nano silver on line adopts a plant reduction method to synthesize the nano silver, and is characterized in that: selecting a platycladus orientalis extracting solution to react with a silver nitrate solution to prepare the nano silver, wherein the synthesis method comprises the following steps:
a. preparation of arborvitae powder: cleaning branches and leaves of Chinese arborvitae, placing on tin foil paper, oven drying in oven at 55 deg.C for 12 hr, grinding, and placing Chinese arborvitae powder in a sealed bag;
b. preparing a arborvitae extract: weighing Platycladus orientalis powder, placing in a container, adding purified water, boiling under magnetic stirring, cooling, centrifuging, collecting supernatant, and filtering to obtain Platycladus orientalis extractive solution;
c. respectively filling the platycladus orientalis extract and a silver nitrate solution into a first injector and a second injector, pushing the injectors by a push-pull injection pump, and continuously injecting the platycladus orientalis extract and the silver nitrate solution into a polytetrafluoroethylene tube through a three-way valve for mixing to form a platycladus orientalis extract and silver nitrate solution mixed solution;
d. heating and reacting: the polytetrafluoroethylene tube is arranged in the heating device in an extending way, and the mixed solution of the platycladus orientalis extract and the silver nitrate solution is subjected to reduction reaction in the heating device to generate nano silver;
e. and the synthesized nano silver continuously flows out from the liquid outlet end of the polytetrafluoroethylene tube, is collected and is cooled to obtain the product nano silver.
2. The method for synthesizing nano silver on line according to claim 1, wherein: the concentration of the arborvitae extract is 1.0-1.8g/100mL, and the concentration of the silver nitrate solution is 10-16 mmol.
3. The method for synthesizing nano silver on line according to claim 2, wherein: the injection speed in the step c is 2.33-3.11mL/min, and the total length of the polytetrafluoroethylene tube is 15-25 m.
4. The method for synthesizing nano silver on line according to claim 3, wherein: the heating mode in the step d is water bath heating or microwave heating, and the heating temperature is 60-90 ℃.
5. An apparatus for on-line synthesizing nano silver according to any one of claims 1 to 4, wherein: the device comprises a push-pull injection pump (1), a first injector (2), a second injector (3), a three-way valve (4), a polytetrafluoroethylene tube (5), a heating device (6) and a collecting container (7), the first injector (2) and the second injector (3) are fixedly arranged on the push-pull injection pump (1) through a pressing sheet (1-1), the piston core rods of the first injector (2) and the second injector (3) are connected with a slide sheet (1-2) on the push-pull injection pump, the slide sheet (1-2) pushes the two piston core rods simultaneously, the front ends of the two syringes are connected with the polytetrafluoroethylene tube (5) through the three-way valve (4), the polytetrafluoroethylene tube (5) is coiled in the heating device (6), the liquid outlet end of the polytetrafluoroethylene tube (5) is connected with the collecting container (7).
6. The apparatus for synthesizing nano silver on line according to claim 5, wherein: the heating device (6) is a water bath kettle or a microwave oven.
7. The device for synthesizing nano silver on line according to claim 6, wherein: the collecting container (7) is a test tube and is placed in a beaker, and ice blocks are also filled in the beaker.
8. The apparatus for synthesizing nano silver on line according to claim 7, wherein: the microwave oven is also internally provided with a rotating disk (6-1), and the polytetrafluoroethylene tube (5) is wound on the rotating disk (6-1).
9. The apparatus for synthesizing nano silver on line according to claim 8, wherein: the first injector (2) and the second injector (3) have the same volume.
CN201911371313.7A 2019-12-27 2019-12-27 Method and device for synthesizing nano silver on line Pending CN111014720A (en)

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CN112126416A (en) * 2020-10-14 2020-12-25 北京工业大学 Microfluidic synthesis method and device for silver nanofluid
CN114029500A (en) * 2021-11-09 2022-02-11 南京大学 Nano silver wire apparatus for producing suitable for hundred kilograms are grades

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Application publication date: 20200417