阅读说明：本技术 一种利用薤白提取物合成四氧化三铁纳米颗粒的方法 (Method for synthesizing ferroferric oxide nano-particles by using allium macrostemon extract ) 是由 刘红宇 廖家蔚 谢凯欣 沈慧玲 刘佳乐 郑兴农 王敏阳 于 2021-10-31 设计创作，主要内容包括：本发明公开了一种利用薤白提取物合成四氧化三铁纳米颗粒的方法。具体步骤为：在室温下往三口烧瓶内加入一定体积比的去离子水与薤白提取物,混合一段时间,待其混合均匀后升温；升高至一定温度后,投入铁源与碱源反应一段时间,等待反应完全；倒出产物进行磁性分离,将磁性分离所得产物清洗后抽滤,抽滤所得产物在马弗炉中于一定温度下煅烧一段时间；煅烧完成后,取出产物进行研磨,得到四氧化三铁纳米颗粒。(The invention discloses a method for synthesizing ferroferric oxide nano-particles by using allium macrostemon extract. The method comprises the following specific steps: adding deionized water and the allium macrostemon extract in a certain volume ratio into a three-neck flask at room temperature, mixing for a period of time, and heating after the mixture is uniformly mixed; after the temperature is raised to a certain temperature, adding an iron source and an alkali source to react for a period of time, and waiting for the reaction to be complete; pouring out the product, performing magnetic separation, cleaning the product obtained by the magnetic separation, performing suction filtration, and calcining the product obtained by the suction filtration in a muffle furnace at a certain temperature for a period of time; and after the calcination is finished, taking out the product and grinding to obtain the ferroferric oxide nano particles.)

1. A method for synthesizing ferroferric oxide nano particles by using allium macrostemon extract is characterized by comprising the following steps: adding deionized water and the allium macrostemon extract in a certain volume ratio into a three-neck flask at room temperature, mixing for a period of time, and heating after the mixture is uniformly mixed; after the temperature is raised to a certain temperature, adding an iron source and an alkali source to react for a period of time, and waiting for the reaction to be complete; pouring out the product, performing magnetic separation, cleaning the product obtained by the magnetic separation, performing suction filtration, and calcining the product obtained by the suction filtration in a muffle furnace at a certain temperature for a period of time; and after the calcination is finished, taking out the product and grinding to obtain the ferroferric oxide nano particles.

2. The method for synthesizing ferroferric oxide nanoparticles by using allium macrostemon extract as claimed in claim 1, wherein the volume ratio of the deionized water to the allium macrostemon extract is 1: 20-1: 40.

3. The method for synthesizing the ferroferric oxide nano-particles by using the allium macrostemon extract as claimed in claim 1, wherein the mixing is carried out for a period of time of 20-40 min.

4. The method for synthesizing ferroferric oxide nano-particles by using allium macrostemon extract as claimed in claim 1, wherein the temperature range of the temperature rising to a certain temperature is 60-80 ℃.

5. The method for synthesizing ferroferric oxide nano particles by using allium macrostemon extract as claimed in claim 1, wherein the input iron source and the alkali source react for a period of 30-120 min.

6. The method for synthesizing ferroferric oxide nano-particles by using allium macrostemon extract as claimed in claim 1, wherein the muffle furnace calcining temperature range is 300-400 ℃.

7. The method for synthesizing the ferroferric oxide nano-particles by using the allium macrostemon extract as claimed in claim 1, wherein the muffle furnace calcination time is 30-90 min.

Technical Field

The invention belongs to the field of preparation of inorganic metal powder, and particularly relates to a method for synthesizing ferroferric oxide nano-particles by using allium macrostemon extract.

Background

Currently, ferroferric oxide nano particles get higher attention in the aspects of magnetic targeting drug carriers, biological magnetic resonance imaging contrast agents, tumor magnetic thermal therapy agents and the like. The ferroferric oxide nano particles have high biocompatibility and tissue trafficability, and cannot cause local inflammation or adverse reaction. In the preparation method of the ferroferric oxide nano particles, the chemical coprecipitation method has obvious advantages, and compared with the other four preparation methods (a microemulsion method, a hydrothermal method, a sol-gel method and a thermal decomposition method), the chemical coprecipitation method has the advantages of simple process, high operability and low cost. The chemical precipitation method can be further divided into an oxidation coprecipitation method, a reduction coprecipitation method and a coprecipitation method. The core of the oxidation coprecipitation method is that ferrous iron ions in raw materials are slowly oxidized to generate ferric iron ions, the core of the reduction coprecipitation method is that the ferric iron ions in the raw materials are reduced to the ferrous iron ions under the action of a reducing agent, and the two methods can both cause the purity of the generated ferroferric oxide nano particles to be reduced. The coprecipitation method has the advantages of simple process and high purity of the produced ferroferric oxide nano particles, but the problem of redundant oxygen in the system needs to be solved by the coprecipitation method. The reason is that the ferrous ions in the system are easily oxidized due to long-term aging, and the prepared ferroferric oxide nano particles are impure due to insufficient ionic strength. At present, two ideas are provided for solving the problem, namely reducing the content of dissolved oxygen in the system and continuously introducing inert gas into the system. The preparation of the ferroferric oxide nano particles by the reaction requires the nitrogen to be introduced for a long time in the whole process so as to ensure the purity of the product. The use of inert gas poses problems such as increased production costs and safety gas use. And secondly, an antioxidant is used and dissolved in deionized water in advance to play a role in resisting oxidation. However, no matter the antioxidant is put in or the inert gas is introduced, the problem of agglomeration cannot be solved when the ferroferric oxide nano particles are produced and prepared.

The invention provides a method for synthesizing ferroferric oxide nano particles by using allium macrostemon extract. Cheap ferric chloride hexahydrate, ferrous sulfate heptahydrate and ammonia water are used as raw materials, so that the cost is reduced, and the mass production is facilitated; the antioxidant and dispersion-assisting effective components are extracted from the allium macrostemon, inert gas is not required to be introduced in the reaction, and the equipment requirement and the operation risk are reduced; the allium macrostemon extract plays roles in resisting oxidation and assisting in dispersion, so that the purity of the prepared ferroferric oxide is improved, and the agglomeration degree is reduced as much as possible; the extraction process of the allium macrostemon extract is simple, and the prepared product is almost not remained in the product after deionized water washing, alcohol washing and spray drying; the wastewater of the cleaning product can be directly discharged after the pH value is adjusted, and the discharged wastewater can not cause pollution to the environment because a natural product is used as a raw material; the solvent used in the extraction of the allium macrostemon is water, can be used as mother liquor for recycling, can also be directly discharged, and does not cause damage to the environment.

Disclosure of Invention

The invention aims to provide a method for synthesizing ferroferric oxide nano-particles by using allium macrostemon extract. The method comprises the following steps: adding deionized water and allium macrostemon extract in a volume ratio of 1: 20-1: 40 into a three-neck flask at room temperature, stirring for 20-40 min, and after the two are uniformly mixed, adding ferric chloride hexahydrate and ferrous sulfate heptahydrate according to a feeding molar ratio n (Fe)²⁺)/n(Fe³⁺) Putting the obtained product in a three-neck flask with the dosage of 1.1-1.8; raising the temperature to 60-80 ℃, and dissolving the input iron source; after the catalyst is fully dissolved, dropwise adding ammonia water, stopping dropwise adding the ammonia water after the pH value of the reaction system is increased to 8-11, and reacting for 30-120 min; after the reaction is completed, pouring out the product for magnetic separation, and repeatedly cleaning deionized water and absolute ethyl alcohol until the pH is = 7; and (3) after carrying out vacuum filtration on the product, taking out the filtered product, and calcining the filtered product in a muffle furnace at 300-400 ℃ for 30-90 min.

The ferroferric oxide nano-particles prepared by the method have the following advantages: (1) the low-cost ferric chloride hexahydrate, ferrous sulfate heptahydrate and ammonia water are used as raw materials, the allium macrostemon extract is used as an additive, and the generated by-product is few and is easy to remove; (2) organic solvent and atmosphere are not used in the preparation process, and the product only needs simple water washing and alcohol washing, so that the production safety is improved; (3) the preparation method is simple, has small technical difficulty and is suitable for mass preparation.

The invention is further described in the following examples without limiting its scope.

Drawings

FIG. 1 shows that the ferroferric oxide sample is 500-4000 cm^-1FTIR spectra in the wavelength range. Infrared spectrum, 3114 cm ^-1The band appeared nearby is generated by stretching vibration of OH-, and the band corresponding to bending vibration is 1388 cm^-1Nearby 561 cm^-1Corresponding to the stretching vibration of Fe-O-Fe, a small amount of impurity peaks are a small amount of residual longstamen onion bulb extract after the product is washed by deionized water, washed by alcohol and calcined by a muffle furnace.

Best mode for carrying out the invention

Weighing 4ml of allium macrostemon extract and 100ml of deionized water respectively, adding the allium macrostemon extract and the deionized water into a three-neck flask, mixing the allium macrostemon extract and the deionized water for 30min at room temperature, weighing 2.6209g of ferric chloride hexahydrate and 1.7992g of ferrous sulfate heptahydrate, adding the materials into the three-neck flask, heating to 70 ℃, dropwise adding ammonia water to adjust the pH value of a reaction system to be 9 after complete dissolution, continuously stirring until black precipitates appear, reacting for 90 min at 70 ℃, washing the product with deionized water after the reaction is finished, carrying out vacuum filtration after the alcohol washing, calcining the product obtained by the filtration in a muffle furnace for 60 min at 350 ℃, and taking out the product for grinding after the calcination is finished to obtain the ferroferric oxide nano-particles.