CN103934008A - Preparation method of halloysite loading phosphoric acid Silverlight catalyst - Google Patents

Preparation method of halloysite loading phosphoric acid Silverlight catalyst Download PDF

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CN103934008A
CN103934008A CN 201410156228 CN201410156228A CN103934008A CN 103934008 A CN103934008 A CN 103934008A CN 201410156228 CN201410156228 CN 201410156228 CN 201410156228 A CN201410156228 A CN 201410156228A CN 103934008 A CN103934008 A CN 103934008A
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halloysite
acid
silver
method
preparation
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CN 201410156228
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CN103934008B (en )
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马建锋
邹静
李良银
姚超
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常州大学
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Abstract

The invention discloses a preparation method of a halloysite loading phosphoric acid Silverlight catalyst. The preparation method comprises the following specific steps of adding halloysite in a salpeter solution so as to obtain the halloysite after acid treatment, placing the 4-8g halloysite after acid treatment into a vacuum filtration bottle, mixing the halloysite and a silver nitrate ethanol solution under a vacuum state, enabling the silver nitrate to fully enter a halloysite pipe, sequentially stirring 2-5h, carrying out solid-liquid separation, and vacuum drying at 70-80 DEG C; adding the obtained product after drying in a 50 mL of sodium dihydrogen phosphate solution the concentration of which is 0.5-1.5mol/L, stirring for 4-5h, carrying out solid-liquid separation, washing, drying at 100-105 DEG C so as to obtain the halloysite loading phosphoric acid Silverlight catalyst. The preparation method provided by the invention has the advantages that the air and moisture in a halloysite pipeline are discharged, the silver nitrate enters a pipeline, an aluminum oxide of the inner wall of the halloysite is removed, the effects of increasing light penetrating degree and aperture property action can be achieved, the obtained silver phosphate particles are arranged in a halloysite pipe and are prevented from birdnesting and falling.

Description

一种埃洛石负载磷酸银光催化剂的制备 Preparation of a phosphoric acid catalyst is silver supported halloysite

技术领域 FIELD

[0001] 本发明涉及环境污染控制新材料领域,尤其涉及一种埃洛石负载磷酸银光催化剂的制备。 [0001] The present invention relates to new materials, environmental pollution control, especially in the preparation of silver phosphoric acid catalyst is directed to a load halloysite.

背景技术 Background technique

[0002] 随着科技的发展,来自工农业生产中产生的毒害有机污染物严重威胁着环境和人类的健康,寻求一种新型高效的环境治理技术具有重要的意义。 [0002] With the development of science and technology, toxic organic pollutants from industrial and agricultural production generated a serious threat to the environment and human health, to seek a new and efficient environmental control technology is of great significance. 光催化技术因其节能、高效、污染物降解彻底、无二次污染优点,目前已成为一种具有重要应用前景的新兴环境治理技术。 Photocatalytic technology because of its energy-saving, efficient and complete degradation of pollutants, no secondary pollution advantages, has become a new environmental management technique has important application prospects. 近年来,新型高效的可见光光催化剂的研制成为光催化技术中的一个重要研究内容,其中具有表面等离子共振效应的光催化材料,因其独特的表面物理化学性质和高效的可见光光催化性能,成为研究的热点之一。 In recent years, development of new efficient catalysts under visible light becomes an important research photocatalytic art, wherein the photocatalytic material having ionic surface-resonance effects, etc., because of their unique physical and chemical properties of the surface and efficient photocatalytic properties of visible light, becomes one of the hotspots. 但纳米颗粒物容易团聚,团聚后表面积大大减小,效果减弱。 But easily agglomerated nanoparticles, the surface area of ​​the aggregates is greatly reduced, less effective.

[0003] 埃洛石又被称多水高岭石。 [0003] halloysite has been called halloysite. 化学组成与高岭石相同,具有相同的1:1的SiO2/Al2O3比,片层结构卷曲成了SiO2在外层,Al2O3在内层,因此埃络石纳米管具有与Si02非常相似的表面性质,和Al2O3相似的内层性质。 Kaolinite same chemical composition, with the same 1: 1 SiO2 / Al2O3 ratio, the lamellar structure in the outer curling became SiO2, Al2O3 in the inner layer, so ERIOCHROME stone Si02 nanotubes have very similar surface properties, Al2O3 similar properties and the inner layer. 一般来说埃洛石纳米管由多个高岭土片层卷曲而成,是天然的多壁型纳米管,管外径为20-100nm,内径为5_30nm,长度为150nm_2 μ m。 Generally halloysite nanotube by a plurality of crimped sheets from kaolin, natural multi-wall nano-tube, the tube outer diameter of 20 to 100 nm, an inner diameter of 5_30nm, length 150nm_2 μ m. 埃洛石与高岭土在晶体结构上的主要区别,一是管状构造,一是片状构造。 Halloysite kaolin main difference in the crystal structure, one of the tubular structure, first, a sheet-like configuration. 埃洛石纳米管,由高岭石的片层在天然条件下卷曲而成,呈微管状结构。 Halloysite nanotube, the sheet curl from kaolinite under native conditions, was slightly the tubular structure. 将纳米银颗粒负载到埃洛石的管内,可以有效的控制纳米银颗粒尺寸。 The silver nanoparticles loading into the tube halloysite, can effectively control the size of the silver nanoparticles. 但现有的技术仅仅是将纳米银颗粒负载到埃洛石的外表面,而内表面面积巨大,同时有很好的吸附效果,如果将内层充分利用,则可以有效的解决磷酸银颗粒团聚的问题。 However, the prior art silver nanoparticles are only loaded onto an outer surface of the halloysite, and great internal surface area, while good adsorption effect, if the full use of the inner layer, can effectively solve the silver phosphate of particle agglomeration The problem.

发明内容 SUMMARY

[0004] 本发明的目的是为克服现有技术的不足,提供一种埃洛石负载磷酸银光催化剂的制备。 [0004] The object of the present invention is to overcome the disadvantages of the prior art, to provide halloysite preparing a supported silver catalyst is phosphoric acid.

[0005] 本发明采用的技术方案是依次包括如下步骤: [0005] aspect of the present invention uses a sequence comprising the steps of:

[0006] I)将纯度不低于80wt%的埃洛石加入到I〜5wt%的硝酸溶液中,反应体系固液比按质量百分比为5〜10%,常温下搅拌4〜8h,离心脱水并干燥,得到酸处理的埃洛石,处理后埃洛石内层的铝氧化合物被溶解掉,管道内径变大,留下二氧化硅层,具有透明效果,催化剂可以有效接收光照; [0006] I) having a purity of not less than 80wt% of halloysite was added to I~5wt% nitric acid solution, the reaction system liquid ratio of 5 to 10% by mass percentage, was stirred at room temperature 4~8h, a centrifugal dehydrator and dried to obtain acid-treated halloysite, an aluminum oxy-compound treated stone Houai Luo inner layer is dissolved away, pipe diameter becomes larger, leaving a silicon dioxide layer having a transparency, the catalyst can be effectively received light;

[0007] 2)将2g硝酸银溶解于80〜IOOmL乙醇中,配制成硝酸银乙醇溶液; [0007] 2) 2g of silver nitrate was dissolved in ethanol 80~IOOmL prepare a silver nitrate solution in ethanol;

[0008] 3)将4〜8g酸处理的埃洛石置于真空抽滤瓶中,真空抽滤瓶中放入磁力搅拌转子,真空抽滤瓶侧面细颈接真空泵,真空抽滤瓶瓶口通过橡皮塞连接分液漏斗,橡皮塞起封闭作用,使分液漏斗和真空抽滤瓶之间紧密连接,分液漏斗旋塞处于关闭状态; [0008] 3) The 4~8g acid treated halloysite placed in a vacuum suction flask, vacuum suction flask containing a magnetic stirring rotor, the vacuum flask connected to a vacuum pump side neck, vacuum flask bottle connected by a separatory funnel rubber plug, a rubber stopper closing action from the tight connection, the separatory funnel stopcock is in a closed state between the separatory funnel and a vacuum flask;

[0009] 4)将硝酸银乙醇溶液装入分液漏斗中,将连着分液漏斗的真空抽滤瓶置于磁力搅拌器上,打开真空泵,抽真空,打开磁力搅拌器,打开分液漏斗旋塞,让分液漏斗中的硝酸银乙醇溶液滴下,在真空状态下混合,在硝酸银快要滴加完成时,迅速完全打开分液漏斗旋塞,让空气完全进入,在空气的压力下,让硝酸银充分进入埃洛石管内,继续搅拌2〜3h,固液分离,真空70〜80°C烘干; [0009] 4) The silver nitrate solution was charged into a separatory funnel and the ethanol in the separatory funnel attached to a vacuum suction bottle was placed on a magnetic stirrer, the vacuum pump, a vacuum pump, opens a magnetic stirrer, separatory funnel opening cock, so dropping the ethanol solution of silver nitrate in a separatory funnel, mixed, at the time of completion of the dropwise addition of silver nitrate is about to rapidly separatory funnel stopcock is fully opened in a vacuum state, so that all air entering the air under pressure, so that nitrate halloysite fully into the silver tube, stirring was continued 2~3h, solid-liquid separation, and drying in vacuo 70~80 ° C;

[0010] 5)将烘干得到的产品加入到50mL,浓度为0.5〜1.5mol/L的磷酸二氢钠溶液中,搅拌4〜5h,固液分离,洗涤,100〜105°C烘干即得一种埃洛石负载磷酸银光催化剂。 [0010] 5) The resulting dried product was added to 50mL, concentration 0.5~1.5mol / L sodium dihydrogen phosphate solution was stirred 4~5h, solid-liquid separation, washing, 100~105 ° C Drying i.e. to give one kind of silver phosphate supported catalyst is halloysite.

[0011] 本发明的优点是:1.排空埃洛石管道中的空气和水汽,使埃洛石和硝酸银能够充分接触,特别是让硝酸银能进入到管道中。 [0011] The advantage of the present invention are: 1 halloysite emptying duct air and moisture, so halloysite and thoroughly contacting the silver nitrate, especially silver nitrate allow to enter into the pipe. 2.去除埃洛石内壁的铝氧化物,可以达到增加光透度和增加孔径的作用。 2. Remove the aluminum oxide halloysite inner wall can be achieved and the effect of increasing the permeability of light of increased pore size. 3.得到的磷酸银颗粒存在于埃洛石管内部,避免团聚和脱落。 3. The resulting silver phosphate particles are present in the interior tubes halloysite, and avoid agglomeration falling off.

具体实施方式 detailed description

[0012] 以下进一步提供本发明的3个实施例: [0012] The present invention further provides the following three embodiments:

[0013] 实施例1 [0013] Example 1

[0014] 将纯度不低于80wt%的埃洛石加入到5wt%的硝酸溶液中,反应体系固液比按质量百分比为10%,常温下搅拌8h,离心脱水并干燥,得到酸处理的埃洛石df2g硝酸银溶解于IOOmL乙醇中,配制成硝酸银乙醇溶液JfSg酸处理的埃洛石置于真空抽滤瓶中,真空抽滤瓶中放入磁力搅拌转子,真空抽滤瓶侧面细颈接真空泵,真空抽滤瓶瓶口通过橡皮塞连接分液漏斗,橡皮塞起封闭作用,使分液漏斗和真空抽滤瓶之间紧密连接,分液漏斗旋塞处于关闭状态;将硝酸银乙醇溶液装入分液漏斗中,将连着分液漏斗的真空抽滤瓶置于磁力搅拌器上,打开真空泵,抽真空,打开磁力搅拌器,打开分液漏斗旋塞,让分液漏斗中的硝酸银乙醇溶液滴下,在真空状态下混合,在硝酸银快要滴加完成时,迅速完全打开分液漏斗旋塞,让空气完全进入,在空气的压力下,让硝酸银充分进入 [0014] The purity of not less than 80wt% of halloysite was added to 5wt% nitric acid solution, the reaction system liquid ratio by mass percentage of 10%, stirred at room temperature 8h, centrifugal dehydrated and dried to obtain acid-treated Å Los stone df2g IOOmL dissolving silver nitrate in ethanol to prepare a solution of silver nitrate in ethanol JfSg acid treated halloysite placed in a vacuum suction flask, vacuum suction flask containing a magnetic stirring rotor, side vacuum flask neck then a vacuum pump, the vacuum flask connected to a separatory funnel and bottle through a rubber stopper, the rubber stopper from blocking action, so that between the separatory funnel and vacuum flask tightly connected to a separatory funnel stopcock is in a closed state; the ethanol solution of silver nitrate was charged to a separatory funnel, attached to a separatory funnel vacuum filtration flasks were placed on a magnetic stirrer, the vacuum pump, a vacuum pump, opens a magnetic stirrer, separatory funnel stopcock is opened, so that the silver nitrate in the separatory funnel ethanol solution dropwise, mixed, at the completion of the dropwise addition of silver nitrate is about to rapidly separatory funnel stopcock is fully opened in a vacuum state, so that all air entering the air under pressure, so that full access to the silver nitrate 埃洛石管内,继续搅拌3h,固液分离,真空80°C烘干;将烘干得到的产品加入到50mL,浓度为1.5mol/L的磷酸二氢钠溶液中,搅拌5h,固液分离,洗涤,105°C烘干即得一种埃洛石负载磷酸银光催化剂。 Halloysite inner tube, stirring was continued for 3h, solid-liquid separation, and drying in vacuo 80 ° C; the resulting dried product was added to 50mL, a concentration of 1.5mol / L sodium dihydrogen phosphate solution, stirred for 5h, the solid-liquid separation , washing, 105 ° C and drying to obtain one kind of silver phosphate supported catalyst is halloysite.

[0015] 将制得的埃洛石负载磷酸银光催化剂用于处理含亚甲基蓝废水:0.5g埃洛石负载磷酸银光催化剂加入到300mL浓度为40mg/L的亚甲基蓝废水中,在300w金卤灯照射下,反应30min,脱色率为96.4%,催化剂分离重复利用7次后,同样条件下,反应30min,脱色率为92.5%。 [0015] The resulting silver phosphate supported catalyst is halloysite for processing waste water containing methylene blue: 0.5g halloysite supported silver catalyst was added to 300mL phosphate concentration of 40mg / L methylene blue wastewater, the metal halide lamp 300w under irradiation, the reaction 30min, bleaching was 96.4%, after separation of the catalyst reused seven times under the same conditions, the reaction 30min, bleaching was 92.5%. 同样质量的磷酸银颗粒在相同的条件下,30min时脱色率为92.6%,相比剥离型膨润土负载磷酸银催化剂,磷酸银颗粒所含的银量相对要大得多,因此本申请所得到的产品更经济,效果更好。 The same mass of silver particles in phosphoric acid under the same conditions, and 30min decolorization rate 92.6%, compared to phosphoric acid exfoliated bentonite supported silver catalyst, the amount of silver contained in the silver phosphate comparatively larger particles, herein thus obtained products more economical, better.

[0016] 实施例2 [0016] Example 2

[0017] 将纯度不低于80wt%的埃洛石加入到lwt%的硝酸溶液中,反应体系固液比按质量百分比为5%,常温下搅拌4h,离心脱水并干燥,得到酸处理的埃洛石;将2g硝酸银溶解于SOmL乙醇中,配制成硝酸银乙醇溶液;将4g酸处理的埃洛石置于真空抽滤瓶中,真空抽滤瓶中放入磁力搅拌转子,真空抽滤瓶侧面细颈接真空泵,真空抽滤瓶瓶口通过橡皮塞连接分液漏斗,橡皮塞起封闭作用,使分液漏斗和真空抽滤瓶之间紧密连接,分液漏斗旋塞处于关闭状态;将硝酸银乙醇溶液装入分液漏斗中,将连着分液漏斗的真空抽滤瓶置于磁力搅拌器上,打开真空泵,抽真空,打开磁力搅拌器,打开分液漏斗旋塞,让分液漏斗中的硝酸银乙醇溶液滴下,在真空状态下混合,在硝酸银快要滴加完成时,迅速完全打开分液漏斗旋塞,让空气完全进入,在空气的压力下,让硝酸银充分 [0017] The purity of not less than 80wt% of halloysite was added to lwt% nitric acid solution, the reaction system liquid ratio from 5% by mass, stirred at room temperature 4h, centrifugal dehydrated and dried to obtain acid-treated Å Los stone; 2g of silver nitrate was dissolved in SOmL ethanol to prepare a solution of silver nitrate in ethanol; 4g of acid treated halloysite placed in a vacuum suction flask, vacuum suction flask containing a magnetic stirring rotor, vacuum filtration side pump connection neck bottle, bottle vacuum flask is connected via a separatory funnel and the rubber stopper, the rubber stopper from blocking action, so that between the separatory funnel and vacuum flask tightly connected to a separatory funnel stopcock is in a closed state; and silver nitrate ethanol solution was charged to a separatory funnel, attached to a separatory funnel vacuum filtration flasks were placed on a magnetic stirrer, the vacuum pump, a vacuum pump, opens a magnetic stirrer, separatory funnel stopcock is opened, so that a separatory funnel the silver nitrate solution was added dropwise ethanol, mixed and, during the completion of the dropwise addition of silver nitrate is about to rapidly separatory funnel stopcock is fully opened in a vacuum state, so that all air entering the air under pressure, so that sufficient silver nitrate 进入埃洛石管内,继续搅拌2h,固液分离,真空70°C烘干;将烘干得到的产品加入到50mL,浓度为0.5mol/L的磷酸二氢钠溶液中,搅拌4h,固液分离,洗涤,100°C烘干即得一种埃洛石负载磷酸银光催化剂。 Halloysite tube into the stirring was continued for 2h, the solid-liquid separation, and drying in vacuo 70 ° C; the resulting dried product was added to 50mL, a concentration of 0.5mol / L sodium dihydrogen phosphate solution, stirred for 4h, solid-liquid separated, washed, 100 ° C and drying to obtain one kind of silver phosphate supported catalyst is halloysite.

[0018] 将制得的埃洛石负载磷酸银光催化剂用于处理含酸性大红废水:0.5g埃洛石负载磷酸银光催化剂加入到300mL浓度为40mg/L的酸性大红废水中,在300w金卤灯照射下,反应30min,脱色率为96.3%,催化剂分离重复利用7次后,同样条件下,反应30min,脱色率为93.0%。 [0018] The resulting silver phosphate supported catalyst is halloysite for processing wastewater containing Acid Red: 0.5g halloysite supported silver catalyst was added to 300mL phosphate concentration of 40mg / L of Acid Red wastewater, the gold 300w the halogen light irradiation, the reaction 30min, bleaching was 96.3%, after separation of the catalyst reused seven times under the same conditions, the reaction 30min, bleaching was 93.0%. 同样质量的磷酸银颗粒在相同的条件下,30min时脱色率为91.1%。 The same mass of silver particles in phosphoric acid under the same conditions, 30min when bleaching was 91.1%.

[0019] 实施例3 [0019] Example 3

[0020] 将纯度不低于80wt%的埃洛石加入到3wt%的硝酸溶液中,反应体系固液比按质量百分比为10%,常温下搅拌8h,离心脱水并干燥,得到酸处理的埃洛石;将2g硝酸银溶解于IOOmL乙醇中,配制成硝酸银乙醇溶液酸处理的埃洛石置于真空抽滤瓶中,真空抽滤瓶中放入磁力搅拌转子,真空抽滤瓶侧面细颈接真空泵,真空抽滤瓶瓶口通过橡皮塞连接分液漏斗,橡皮塞起封闭作用,使分液漏斗和真空抽滤瓶之间紧密连接,分液漏斗旋塞处于关闭状态;将硝酸银乙醇溶液装入分液漏斗中,将连着分液漏斗的真空抽滤瓶置于磁力搅拌器上,打开真空泵,抽真空,打开磁力搅拌器,打开分液漏斗旋塞,让分液漏斗中的硝酸银乙醇溶液滴下,在真空状态下混合,在硝酸银快要滴加完成时,迅速完全打开分液漏斗旋塞,让空气完全进入,在空气的压力下,让硝酸银充分进入 [0020] The purity of not less than 80wt% of halloysite was added to 3wt% nitric acid solution, the reaction system liquid ratio by mass percentage of 10%, stirred at room temperature 8h, centrifugal dehydrated and dried to obtain acid-treated Å Los stone; 2g of silver nitrate was dissolved in ethanol IOOmL, formulated as an ethanol solution of silver nitrate halloysite acid-treated in a vacuum suction flask, vacuum suction flask containing a magnetic stirring rotor, the vacuum flask of the capillary necking a vacuum pump, the vacuum flask bottle is connected via a separatory funnel and the rubber stopper, the rubber stopper from blocking action, so that between the separatory funnel and vacuum flask tightly connected to a separatory funnel stopcock is in a closed state; the silver nitrate in ethanol solution was charged into a separatory funnel, attached to a separatory funnel vacuum filtration flasks were placed on a magnetic stirrer, the vacuum pump, a vacuum pump, opens a magnetic stirrer, separatory funnel stopcock is opened, so that a separatory funnel nitrate silver ethanol solution dropwise, mixed, at the completion of the dropwise addition of silver nitrate is about to rapidly separatory funnel stopcock is fully opened in a vacuum state, so that all air entering the air under pressure, so that full access to the silver nitrate 埃洛石管内,继续搅拌3h,固液分离,真空75°C烘干;将烘干得到的产品加入到50mL,浓度为lmol/L的磷酸二氢钠溶液中,搅拌4h,固液分离,洗涤,100°C烘干即得一种埃洛石负载磷酸银光催化剂。 Halloysite inner tube, stirring was continued for 3h, solid-liquid separation, and drying in vacuo 75 ° C; the resulting dried product was added to 50mL, a concentration of lmol / L sodium dihydrogen phosphate solution, stirred for 4h, solid-liquid separation, washing, 100 ° C and drying to obtain one kind of silver phosphate supported catalyst is halloysite.

[0021] 将制得的埃洛石负载磷酸银光催化剂用于处理含酸性大红废水:0.5g埃洛石负载磷酸银光催化剂加入到300mL浓度为40mg/L的酸性大红废水中,在300w金卤灯照射下,反应30min,脱色率为96.8%,催化剂分离重复利用7次后,同样条件下,反应30min,脱色率为92.4%。 [0021] The resulting silver phosphate supported catalyst is halloysite for processing wastewater containing Acid Red: 0.5g halloysite supported silver catalyst was added to 300mL phosphate concentration of 40mg / L of Acid Red wastewater, the gold 300w the halogen light irradiation, the reaction 30min, bleaching was 96.8%, after separation of the catalyst reused seven times under the same conditions, the reaction 30min, bleaching was 92.4%. 同样质量的磷酸银颗粒在相同的条件下,30min时脱色率为93.3%。 The same mass of silver particles in phosphoric acid under the same conditions, 30min when bleaching was 93.3%.

Claims (1)

  1. 1.一种埃洛石负载磷酸银光催化剂的制备,其特征是依次包括如下步骤: 1)将纯度不低于80wt%的埃洛石加入到I〜5wt%的硝酸溶液中,反应体系固液比按质量百分比为5〜10%,常温下搅拌4〜8h,离心脱水并干燥,得到酸处理的埃洛石,处理后埃洛石内层的铝氧化合物被溶解掉,管道内径变大,留下二氧化硅层,具有透明效果,催化剂可以有效接收光照; 2)将2g硝酸银溶解于80〜IOOmL乙醇中,配制成硝酸银乙醇溶液; 3)将4〜8g酸处理的埃洛石置于真空抽滤瓶中,真空抽滤瓶中放入磁力搅拌转子,真空抽滤瓶侧面细颈接真空泵,真空抽滤瓶瓶口通过橡皮塞连接分液漏斗,橡皮塞起封闭作用,使分液漏斗和真空抽滤瓶之间紧密连接,分液漏斗旋塞处于关闭状态; 4)将硝酸银乙醇溶液装入分液漏斗中,将连着分液漏斗的真空抽滤瓶置于磁力搅拌器上,打开真空泵, Catalyst Preparation A silver phosphate halloysite load, characterized by sequentially comprising the following steps: 1) The purity of not less than 80wt% of halloysite was added to I~5wt% nitric acid solution, the solid reaction system liquid ratio of the aluminum compound is 5 to 10% by mass percentage, was stirred at room temperature 4~8h, centrifugal dehydrated and dried to obtain acid-treated halloysite, stone processing Houai Luo inner layer is dissolved away, the pipe diameter increases , leaving a silicon dioxide layer having a transparency, the catalyst can be effectively received light; 2) 2g of silver nitrate was dissolved in ethanol 80~IOOmL prepare a silver nitrate solution in ethanol; 3) the acid treated halloysite 4~8g stone a vacuum suction flask, vacuum suction flask containing a magnetic stirring rotor, the vacuum flask connected to a vacuum pump side neck, bottle vacuum flask connected to a separatory funnel through the rubber stopper, the rubber stopper from blocking effect, so that between the separatory funnel and vacuum flask tightly connected to a separatory funnel stopcock is in a closed state; 4) silver nitrate ethanol solution was charged to a separatory funnel, separatory funnel attached to the vacuum flask placed on a magnetic agitator, the vacuum pump, 真空,打开磁力搅拌器,打开分液漏斗旋塞,让分液漏斗中的硝酸银乙醇溶液滴下,在真空状态下混合,在硝酸银快要滴加完成时,迅速完全打开分液漏斗旋塞,让空气完全进入,在空气的压力下,让硝酸银充分进入埃洛石管内,继续搅拌2〜3h,固液分离,真空70〜80°C烘干; 5)将烘干得到的产品加入到50mL,浓度为0.5〜1.5mol/L的磷酸二氢钠溶液中,搅拌4〜5h,固液分离,洗涤,100〜105°C烘干即得一种埃洛石负载磷酸银光催化剂。 Vacuo open magnetic stirrer, separatory funnel stopcock is opened, so that an ethanol solution of silver nitrate was dropped in a separatory funnel, mixed, at the time of completion of the dropwise addition of silver nitrate is about to rapidly separatory funnel stopcock is fully opened in a vacuum state, so that the air full access, under air pressure, so that sufficient silver nitrate into the tube halloysite, stirring was continued 2~3h, solid-liquid separation, and drying in vacuo 70~80 ° C; 5) the dry product obtained was added to a 50mL, concentration 0.5~1.5mol / L sodium dihydrogen phosphate solution was stirred 4~5h, solid-liquid separation, washing, 100~105 ° C and drying to obtain one kind of silver phosphate supported catalyst is halloysite.
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