阅读说明：本技术 无定型羟基氧化铁的制备方法及吸附有机物后的回收方法 (Preparation method of amorphous iron oxyhydroxide and recovery method after organic matter adsorption ) 是由 李楠 易中周 单科 翟凤瑞 何云龙 于 2019-08-09 设计创作，主要内容包括：本发明公开了一种无定型羟基氧化铁的制备方法及吸附有机物后的回收方法,本发明提高无定型羟基氧化铁的制备效率,由于所采用的制备原料为氯化铁,其中的铁为三价铁,而非传统的氯化亚铁或硫酸亚铁,避免了制备过程中的氧化流程,使无定型羟基氧化铁的制备效率大幅提高。吸附有机物后的羟基氧化铁得到有效回收利用,经过煅烧后获得具有光催化效果的纳米α氧化铁,由于有机物的存在,使得所制得的纳米氧化铁,其晶粒比直接由无定型羟基氧化铁制备的纳米氧化铁更细,表面具有更多的活性点,催化效果更好。(The invention discloses a preparation method of amorphous FeOOH and a recovery method after organic matter adsorption, which improves the preparation efficiency of amorphous FeOOH. The hydroxyl ferric oxide after adsorbing the organic matters is effectively recycled, the nanometer alpha ferric oxide with the photocatalysis effect is obtained after calcination, and due to the existence of the organic matters, the crystal grains of the prepared nanometer ferric oxide are thinner than those of the nanometer ferric oxide directly prepared from amorphous hydroxyl ferric oxide, the surface of the nanometer ferric oxide has more active points, and the catalysis effect is better.)

1. A preparation method of amorphous iron oxyhydroxide and a recovery method after organic matter adsorption are characterized in that: the coal oil, span 80, tween 80 and distilled water are mixed according to the mass ratio: preparing a micro-emulsion phase according to the ratio of 20:10:10:1, and stirring until the micro-emulsion phase is transparent for later use; adding ferric chloride powder, wherein the mass ratio of the ferric chloride powder to distilled water is 1-4:1, fully stirring until the powder is completely dissolved, adding sodium hydroxide particles, wherein the molar ratio of the sodium hydroxide to the ferric chloride is 1:1, heating to 80-90 ℃, reacting for 30 minutes, stopping heating, centrifuging to obtain a precipitate, washing for 2 times by using absolute ethyl alcohol, washing for 2 times by using distilled water, and drying to obtain the amorphous ferric oxyhydroxide.

2. A recovery method of amorphous iron oxyhydroxide after preparing adsorbed organic matter is characterized in that: adding a proper amount of prepared amorphous iron oxyhydroxide into the printing and dyeing wastewater, fully stirring, and effectively removing organic matters in the printing and dyeing wastewater through the adsorption effect of the amorphous iron oxyhydroxide; the amorphous iron oxyhydroxide after absorbing the organic matter is calcined for 1-3 hours at 600-800 ℃ to obtain the nano iron oxide with the photocatalytic effect, and the nano iron oxide can be used for photocatalysis of printing and dyeing wastewater.

3. The method for preparing amorphous iron oxyhydroxide according to claim 1 and the method for recovering adsorbed organic substances, wherein: the residual microemulsion phase after centrifugal extraction and precipitation can be continuously recycled.

4. The method for recovering the adsorbed organic matter from the amorphous iron oxyhydroxide according to claim 2, wherein: removing organic matters in the printing and dyeing wastewater by using an amorphous iron oxyhydroxide physical adsorption method.

5. The method for recovering the adsorbed organic matter from the amorphous iron oxyhydroxide according to claim 2, wherein: the nano iron oxide obtained by calcining amorphous iron oxyhydroxide at 600-800 ℃ is alpha iron oxide.

6. The method for recovering the adsorbed organic matter from the amorphous iron oxyhydroxide according to claim 2, wherein: after calcination at 600-800 ℃, the organic matter adsorbed by the iron oxyhydroxide is decomposed, part of the organic matter is carbonized in the decomposition process, and the function of refining nano iron oxide grains is achieved in the further oxidation process, so that the surface active points are more, and the photocatalysis effect is better.

Technical Field

The invention relates to the field of degradation of organic matters in printing and dyeing wastewater, in particular to a preparation method of amorphous iron oxyhydroxide and a recovery method after organic matters are adsorbed.

Background

at present, the domestic production of iron oxyhydroxide mainly adopts ferrous sulfate and sodium carbonate or ammonium bicarbonate as raw materials, and the raw materials are mixed according to a certain proportion, and then air is introduced to oxidize under a heating state, and the product is prepared by washing and filtering. The process adopts an air oxidation method, and has slow reaction speed and low production efficiency.

The amorphous FeOOH is widely used as a desulfurizer, a heavy metal remover and a sewage treatment agent. The organic wastewater is mainly removed by physical adsorption, organic matters are not decomposed, iron oxyhydroxide of the organic matters is adsorbed, and the adsorption efficiency is sharply reduced when the iron oxyhydroxide is reused.

Disclosure of Invention

the invention provides a preparation method of amorphous FeOOH and a recovery method after adsorbing organic matters, aiming at the problems that the preparation efficiency of FeOOH is low and the amorphous FeOOH is difficult to recycle after adsorbing organic matters, the method takes ferric chloride as a raw material to prepare amorphous FeOOH, does not need an oxidation process and has high efficiency; the hydroxyl ferric oxide after adsorbing the organic matters is calcined to obtain the nano ferric oxide with photocatalytic performance, and the nano ferric oxide can be used for photocatalytic explanation of the organic matters.

the invention realizes the purpose through the following technical scheme:

The invention relates to a preparation method of amorphous iron oxyhydroxide and a recovery method after organic matter adsorption, which is characterized in that: the coal oil, span 80, tween 80 and distilled water are mixed according to the mass ratio: preparing a micro-emulsion phase according to the ratio of 20:10:10:1, and stirring until the micro-emulsion phase is transparent for later use; adding ferric chloride powder, wherein the mass ratio of the ferric chloride powder to distilled water is 1-4:1, fully stirring until the powder is completely dissolved, adding sodium hydroxide particles, wherein the molar ratio of the sodium hydroxide to the ferric chloride is 1:1, heating to 80-90 ℃, reacting for 30 minutes, stopping heating, centrifuging to obtain a precipitate, washing for 2 times by using absolute ethyl alcohol, washing for 2 times by using distilled water, and drying to obtain the amorphous ferric oxyhydroxide.

The invention relates to a recovery method of amorphous iron oxyhydroxide after preparing adsorbed organic matter, which is characterized by comprising the following steps: adding a proper amount of prepared amorphous iron oxyhydroxide into the printing and dyeing wastewater, fully stirring, and effectively removing organic matters in the printing and dyeing wastewater through the adsorption effect of the amorphous iron oxyhydroxide; the amorphous iron oxyhydroxide after absorbing the organic matter is calcined for 1-3 hours at 600-800 ℃ to obtain the nano iron oxide with the photocatalytic effect, and the nano iron oxide can be used for photocatalysis of printing and dyeing wastewater.

Specifically, the residual microemulsion phase after centrifugal extraction and precipitation can be continuously recycled.

specifically, the amorphous iron oxyhydroxide removes organic matters in the printing and dyeing wastewater by a physical adsorption method.

Specifically, the nano iron oxide obtained by calcining amorphous iron oxyhydroxide at 600-800 ℃ is alpha iron oxide.

Specifically, after calcination at 600-800 ℃, the organic matter adsorbed by the iron oxyhydroxide is decomposed, part of the organic matter is carbonized in the decomposition process, and the effect of refining nano iron oxide grains is achieved in the further oxidation process, so that the surface active points are more, and the photocatalysis effect is better.

The invention has the beneficial effects that:

The invention relates to a preparation method of amorphous FeOOH and a recovery method after organic matter adsorption, compared with the prior art, the preparation method improves the preparation efficiency of the amorphous FeOOH. The hydroxyl ferric oxide after adsorbing the organic matters is effectively recycled, the nanometer alpha ferric oxide with the photocatalysis effect is obtained after calcination, and due to the existence of the organic matters, the crystal grains of the prepared nanometer ferric oxide are thinner than those of the nanometer ferric oxide directly prepared from amorphous hydroxyl ferric oxide, the surface of the nanometer ferric oxide has more active points, and the catalysis effect is better.

Drawings

FIG. 1 is an XRD pattern of amorphous iron oxyhydroxide prepared;

FIG. 2 is a graph showing the effect of cycle number on the 10-minute adsorption decoloration rate of amorphous iron oxyhydroxide;

FIG. 3 is an XRD (X-ray diffraction) diagram of nano-iron oxide obtained after the iron oxyhydroxide adsorbed with organic matters is calcined at 700 ℃ for 2 hours;

FIG. 4 is a graph of the rate of degradation of methyl orange by ultraviolet photocatalytic degradation of nano-iron oxide;

FIG. 5 is a graph showing the degradation rate of methyl orange catalyzed by nano-iron oxide under simulated sunlight.

Detailed Description

The invention is further illustrated below: