阅读说明：本技术 一种利用柳树叶提取物合成四氧化三铁纳米颗粒的方法 (Method for synthesizing ferroferric oxide nanoparticles by using willow leaf 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 2021-10-10 设计创作，主要内容包括：本发明公开了一种利用柳树叶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和柳树叶提取物,在一定温度下搅拌一段时间,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,反应完全后倒出产物进行磁性分离,抽滤清洗产物,配置成悬浊液进行喷雾干燥,得到四氧化三铁纳米颗粒。(The invention discloses a method for synthesizing ferroferric oxide nanoparticles by using willow leaf extract. The method comprises the following specific steps: adding deionized water and willow leaf extract in a certain volume ratio into a three-neck flask at room temperature, stirring for a period of time at a certain temperature, heating after uniformly mixing, raising the temperature to a certain temperature, adding an iron source and an alkali source, reacting for a period of time, pouring out a product after complete reaction, performing magnetic separation, performing suction filtration and cleaning on the product, preparing a suspension, and performing spray drying to obtain ferroferric oxide nanoparticles.)

1. A method for synthesizing ferroferric oxide nanoparticles by using willow leaf extract is characterized by comprising the following steps: adding deionized water and willow leaf extract in a certain volume ratio into a three-neck flask at room temperature, stirring for a period of time at a certain temperature, heating after uniformly mixing, raising the temperature to a certain temperature, adding an iron source and an alkali source, reacting for a period of time, pouring out a product after complete reaction, performing magnetic separation, performing suction filtration and cleaning on the product, preparing a suspension, and performing spray drying to obtain ferroferric oxide nanoparticles.

2. The method for synthesizing ferroferric oxide nanoparticles by using willow leaf extract as claimed in claim 1, wherein the volume ratio of the deionized water to the willow leaf extract is 1: 10-1: 16.

3. The method for synthesizing ferroferric oxide nanoparticles by using willow leaf extract as claimed in claim 1, wherein the temperature range at a certain temperature is 40-60 ℃.

4. The method for synthesizing ferroferric oxide nanoparticles by using willow leaf extract as claimed in claim 1, wherein the deionized water and the willow leaf extract are stirred for a period of time of 30-80 min.

5. The method for synthesizing ferroferric oxide nanoparticles by using willow leaf extract as claimed in claim 1, wherein the temperature range after the temperature is raised to a certain temperature is 70-90 ℃.

6. The method for synthesizing ferroferric oxide nanoparticles by using willow leaf extract as claimed in claim 1, wherein the reaction time is 90-240 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 nanoparticles by using willow leaf extract.

Background

The ferroferric oxide nano-particles have the dual advantages of magnetic particles and nano-particles, so that the ferroferric oxide nano-particles are concerned more in the biological fields of magnetic targeting drug carriers, biological magnetic resonance imaging contrast agents, tumor magnetic thermal therapy agents, nucleic acid hybridization and the like at present. The ferroferric oxide nanoparticles are almost non-toxic, and the particle size of the ferroferric oxide nanoparticles serving as a drug carrier is more distributed in the range of 60-120 nm, so that the ferroferric oxide nanoparticles do not cause rejection reaction of organisms, and have high biocompatibility. Currently, the preparation of ferroferric oxide nano particles mainly comprises the following methods, namely a chemical coprecipitation method, a sol-gel method, a solvothermal method, a thermal decomposition method and a microemulsion method. Compared with the other four preparation methods, the chemical coprecipitation method has the advantages of simple process, high operability and low cost. However, the core of the chemical coprecipitation method lies in the condition that ferroferric oxide crystal nuclei grow, and the particle size distribution of the prepared ferroferric oxide nano particles is wider under the condition of low concentration and long-time aging. The reason is that the ferrous ions in the system are easily oxidized due to long-term aging, the ionic strength is not enough, the impurity content of the generated product is high, and the prepared ferroferric oxide nano particles are impure. In order to solve the problem, two ideas exist at present, one is to use inert gas to remove oxygen in the reaction system as much as possible, for example, deionized water for reaction needs to be introduced with nitrogen for secondary treatment to reduce the content of dissolved oxygen in water. 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 brings about problems such as an increase in production cost and a decrease in production efficiency. Secondly, a reducing agent, such as sodium sulfite and the like, is used and dissolved in the deionized water in advance to play a role in resisting oxidation. However, no matter the reducing agent is added or nitrogen is introduced, the problem of agglomeration needs to be solved when the ferroferric oxide nano particles are produced and prepared. According to the method for synthesizing ferroferric oxide nanoparticles by using the willow leaf extract, cheap ferric nitrate nonahydrate, ferrous sulfate heptahydrate and ammonia water are used as raw materials, so that the cost is reduced, and the method is favorable for mass production; the antioxidant and dispersion-assisting active ingredients are extracted from the willow leaves, and the atmosphere such as nitrogen and the like is not required to be introduced in the reaction, so that the equipment requirement and the production cost are reduced; the willow leaf extract has the functions of oxidation resistance and dispersion assistance, 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 willow leaf extract is simple, and the 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 willow leaves can be recycled, and the physical and chemical properties of the extract cannot be influenced.

Disclosure of Invention

The invention aims to provide a method for synthesizing ferroferric oxide nanoparticles by using willow leaf extract, which comprises the following steps: adding deionized water and willow leaf extract in a volume ratio of 1: 10-1: 16 into a three-neck flask at room temperature, heating to 40-60 ℃, stirring for 30-80 min, and mixing the two uniformly, then adding ferric nitrate nonahydrate and ferrous sulfate heptahydrate according to a feeding molar ratio n (Fe)²⁺)/n(Fe³⁺) Putting the obtained product in a three-neck flask in an amount of =1 (1.2-2); raising the temperature to 70-90 ℃, 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 a reaction system is increased to 8-11, and reacting for 90-240 min; and after the reaction is completed, pouring out the product, performing magnetic separation, repeatedly cleaning the product with deionized water and absolute ethyl alcohol until the pH is =7, performing vacuum filtration on the product, preparing a suspension with a certain amount of deionized water, and performing spray drying.

The ferroferric oxide nano-particles prepared by the method have the following advantages: (1) the low-cost ferric nitrate nonahydrate, ferrous sulfate heptahydrate and ammonia water are used as raw materials, the willow leaf extract is used as an additive, the used reagent is low in price, and the generated by-product is few and is easy to remove; (2) organic solvents with strong irritation and any atmosphere are not used in the preparation process, and products only need to be simply washed by water and alcohol, 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^-1An infrared spectrum in the wavelength range. 3080 cm ^-1The band appeared nearby is generated by stretching vibration of OH-, and the band corresponding to bending vibration is 1300 cm^-1Near, 580 cm^-1Corresponding to the stretching vibration of Fe-O-Fe.

Best mode for carrying out the invention

Respectively weighing 10ml of willow leaf extract, 100ml of deionized water, adding the willow leaf extract and the deionized water into a three-neck flask, mixing for 50min at 50 ℃, uniformly mixing, weighing 3.7046g of ferric nitrate nonahydrate and 2.4805g of ferrous sulfate heptahydrate, adding the ferric nitrate nonahydrate and the ferrous sulfate heptahydrate into the three-neck flask, heating to 75 ℃, after complete dissolution, dropwise adding ammonia water to adjust the pH value of a reaction system to 9, continuously stirring until black precipitates appear, reacting for 120 min at 75 ℃, washing a product deionized water after the reaction is finished, carrying out vacuum filtration after alcohol washing, preparing 100ml of deionized water and the product after filtration into turbid liquid, carrying out spray drying at the inlet air temperature of 200 ℃, carrying out air outlet at 45 ℃, and carrying out spray drying to obtain the ferroferric oxide nanoparticles.