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CN104118892A - Method for preparing nano magnesium hydroxide from microplasma seawater - Google Patents

Method for preparing nano magnesium hydroxide from microplasma seawater Download PDF

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CN104118892A
CN104118892A CN201410314174.5A CN201410314174A CN104118892A CN 104118892 A CN104118892 A CN 104118892A CN 201410314174 A CN201410314174 A CN 201410314174A CN 104118892 A CN104118892 A CN 104118892A
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micro
plasma
magnesium hydroxide
seawater
voltage
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杜长明
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Sun Yat Sen University
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Abstract

本发明公开一种微等离子体海水制备纳米氢氧化镁的方法和装置,具体步骤将将海水倒入微等离子体反应器,加入NaOH调节溶液初始pH值到一定值;打开氩气瓶,调节流量计控制气体流量,待气流稳定后开启直流高压电源,当电压达到2500V左右时,气体被击穿,形成微等离子体;随后立即调节电压使微等离子体稳定在一定电压和电流水平,反应正式开始;放电处理5~20min,完成纳米氢氧化镁的制备。本发明可以根据实际要求完成纳米氢氧化镁的制备过程,简单、低成本、高效的制备出纳米氢氧化镁,具有潜在的发展前景。

The invention discloses a method and device for preparing nano-magnesium hydroxide from micro-plasma seawater. The specific steps include pouring seawater into a micro-plasma reactor, adding NaOH to adjust the initial pH value of the solution to a certain value; opening the argon gas bottle, and adjusting the flow rate. The gas flow is controlled by the meter, and the DC high-voltage power supply is turned on after the gas flow is stable. When the voltage reaches about 2500V, the gas is broken down to form a micro-plasma; then the voltage is adjusted immediately to stabilize the micro-plasma at a certain voltage and current level, and the reaction officially begins ; Discharge treatment for 5-20 minutes to complete the preparation of nano-magnesium hydroxide. The invention can complete the preparation process of nano-magnesium hydroxide according to actual requirements, and prepares nano-magnesium hydroxide simply, at low cost and with high efficiency, and has potential development prospects.

Description

一种微等离子体海水制备纳米氢氧化镁的方法A method for preparing nano-magnesium hydroxide from micro-plasma seawater

技术领域 technical field

本发明涉及纳米材料制备技术领域,特别是涉及一种微等离子体海水制备纳米氢氧化镁的方法和装置。  The invention relates to the technical field of nanomaterial preparation, in particular to a method and a device for preparing nano magnesium hydroxide from micro-plasma seawater. the

背景技术 Background technique

海水综合利用技术迅速发展,将海水淡化与综合利用相结合是未来海水利用的方向。氢氧化镁是一种重要的无机化合物,可广泛应用于塑料、树脂等有机体的阻燃剂、含铅废水处理、烟气脱硫及医药等领域。纳米级的氢氧化镁由于具备了纳米材料的特性,是近年来阻燃剂的发展方向,具有阻燃、消烟、防滴、填充等多重功能,是一种环保型绿色阻燃剂,市场前景更广阔。目前,从海水制备纳米氢氧化镁的最基本方法就是直接沉淀法,往浓海水里加碱,使氢氧化镁沉淀,但此方法产品粒度大且分布宽、纯度低、团聚严重。因此,经济、高效、高纯度地从海水制备纳米氢氧化镁,除改进现有的技术外,尚须发展新的技术。  Seawater comprehensive utilization technology is developing rapidly, and the combination of seawater desalination and comprehensive utilization is the direction of future seawater utilization. Magnesium hydroxide is an important inorganic compound, which can be widely used in the fields of flame retardant for plastics, resins and other organisms, lead-containing wastewater treatment, flue gas desulfurization and medicine. Nano-scale magnesium hydroxide is the development direction of flame retardants in recent years due to the characteristics of nano-materials. It has multiple functions such as flame retardant, smoke elimination, anti-drip, filling, etc. It is an environmentally friendly green flame retardant. The market The prospects are broader. At present, the most basic method for preparing nano-magnesium hydroxide from seawater is the direct precipitation method, adding alkali to concentrated seawater to precipitate magnesium hydroxide, but the product of this method has large particle size, wide distribution, low purity, and serious agglomeration. Therefore, to economically, efficiently, and highly purely prepare nano-magnesium hydroxide from seawater, in addition to improving existing technologies, new technologies still need to be developed. the

发明内容 Contents of the invention

为解决上述问题,本发明提出一种微等离子体海水制备纳米氢氧化镁的方法和装置。该方法和装置的优势在于简单、高效、消耗低的制备纳米氢氧化镁,具有潜在的发展前景。  In order to solve the above problems, the present invention proposes a method and device for preparing nano-magnesium hydroxide from micro-plasma seawater. The method and device have the advantages of simple, high-efficiency, and low-consumption preparation of nano-magnesium hydroxide, and have potential development prospects. the

本发明为达到以上目的,是通过以下的技术方案来实现的:  The present invention is to achieve above object, realizes by following technical scheme:

提供一种微等离子体海水制备纳米氢氧化镁的方法,1)将海水倒入微等离子体反应器,加入NaOH调节溶液初始pH值到一定值;2)打开氩气瓶,调节流量计控制气体流量,待气流稳定后开启直流高压电源,当电压达到2500V左右时,气体被击穿,形成微等离子体;随后立即调节电压使微等离子体稳定在一定电压和电流水平,反应正式开始;放电处理5~20min,完成纳米氢氧化镁的制备。  A method for preparing nano-magnesium hydroxide from micro-plasma seawater is provided. 1) Pour seawater into a micro-plasma reactor, add NaOH to adjust the initial pH value of the solution to a certain value; 2) open the argon gas bottle, and adjust the flow meter to control the gas Flow rate, after the air flow is stable, turn on the DC high-voltage power supply. When the voltage reaches about 2500V, the gas is broken down to form a micro-plasma; then immediately adjust the voltage to stabilize the micro-plasma at a certain voltage and current level, and the reaction officially begins; discharge treatment 5-20 minutes to complete the preparation of nano-magnesium hydroxide. the

提供一种微等离子体海水制备纳米氢氧化镁的装置,包括微等离子体反应器、给微等离子体反应器供电的直流高压电源(1)和给微等离子体反应器供气的氩气瓶(9);微等离子体反应器采用玻璃反应器(5),溶液搅拌采用磁力搅拌器(8),阳极主体为毛细不锈钢管(3),氩气从氩气瓶经过玻璃转子流量计 注入不锈钢电极体内直至反应器中;不锈钢电极垂直置于反应溶液上方,电极出气端距离溶液表面2mm;阴极为细钨棒(4);钨棒通过串联镇流电阻(2)与直流高压电源的接地端连接;启动直流高压电源后,不锈钢电极与液面之间产生微等离子体(6),体系形成通路。  A device for preparing nano-magnesium hydroxide from micro-plasma seawater is provided, comprising a micro-plasma reactor, a DC high-voltage power supply (1) for powering the micro-plasma reactor and an argon bottle (1) for supplying gas to the micro-plasma reactor 9); the micro-plasma reactor adopts a glass reactor (5), the solution is stirred by a magnetic stirrer (8), the anode body is a capillary stainless steel tube (3), and the argon gas is injected into the stainless steel electrode from the argon gas bottle through the glass rotameter Inside the body to the reactor; the stainless steel electrode is placed vertically above the reaction solution, and the gas outlet of the electrode is 2mm away from the surface of the solution; the cathode is a thin tungsten rod (4); the tungsten rod is connected to the ground terminal of the DC high voltage power supply through a series ballast resistor (2) ; After starting the DC high-voltage power supply, micro plasma (6) is generated between the stainless steel electrode and the liquid surface, and the system forms a path. the

本发明制备纳米氢氧化镁的原理:本发明以微等离子体做阴极,其与阳极通过电解介质连接构成微等离子体电化学体系,气体击穿产生微等离子体之后,微等离子体携带的大量高能电子进入反应介质,并发生如下反应:  The principle of preparing nano-magnesium hydroxide in the present invention: the present invention uses micro-plasma as the cathode, which is connected with the anode through an electrolytic medium to form a micro-plasma electrochemical system. After gas breakdown produces micro-plasma, a large amount of high-energy Electrons enter the reaction medium, and the following reactions occur:

Mg2++2OH→Mg(OH)2↓  Mg 2+ +2OH→Mg(OH) 2

本发明可以根据实际要求完成纳米氢氧化镁的制备过程,简单、低成本、高效的制备出纳米氢氧化镁。  The invention can complete the preparation process of nano-magnesium hydroxide according to actual requirements, and can prepare nano-magnesium hydroxide simply, at low cost and with high efficiency. the

附图说明 Description of drawings

图1为本发明方法的装置示意图。  Fig. 1 is the device schematic diagram of the method of the present invention. the

图中:1直流高压电源、2镇流电阻、3不锈钢管、4钨棒、5玻璃反应器、6微等离子体、7磁力搅拌器、8玻璃转子流量计、9氩气瓶。  In the figure: 1. DC high voltage power supply, 2. Ballast resistor, 3. Stainless steel tube, 4. Tungsten rod, 5. Glass reactor, 6. Micro plasma, 7. Magnetic stirrer, 8. Glass rotameter, 9. Argon cylinder. the

具体实施方式 Detailed ways

实施例  Example

如附图1所示,微等离子体反应器采用玻璃反应器,高8.5cm,内径5.5cm。阳极主体为不锈钢管,长8cm,内径0.7mm。氩气从氩气瓶经过玻璃转子流量计注入不锈钢电极体内直至反应器中。不锈钢电极垂直置于反应溶液上方,电极出气端距离溶液表面2mm。阴极为钨棒,长15cm,直径2mm。钨棒通过串联10kΩ镇流电阻与直流高压电源的接地端连接。两个电极保持3cm的距离。启动直流高压电源后,不锈钢电极与液面之间产生微等离子体,体系形成通路。溶液搅拌采用数显恒温磁力搅拌器。  As shown in Figure 1, the micro-plasma reactor is a glass reactor with a height of 8.5 cm and an inner diameter of 5.5 cm. The main body of the anode is a stainless steel tube with a length of 8 cm and an inner diameter of 0.7 mm. Argon gas is injected from the argon cylinder through the glass rotameter into the stainless steel electrode body until it reaches the reactor. The stainless steel electrode is placed vertically above the reaction solution, and the gas outlet of the electrode is 2mm away from the solution surface. The cathode is a tungsten rod with a length of 15cm and a diameter of 2mm. The tungsten rod is connected to the ground terminal of the DC high-voltage power supply through a 10kΩ ballast resistor in series. The two electrodes were kept at a distance of 3 cm. After starting the DC high-voltage power supply, micro-plasma is generated between the stainless steel electrode and the liquid surface, and the system forms a path. The solution was stirred using a digital constant temperature magnetic stirrer. the

取一定量海水和0.5mol/LNaOH混合充分,取40mL溶液倒入反应器,并加入乙二醇。将氩气通入不锈钢针管内,其流量通过玻璃转子流量计控制在60mL/min。装置连接完毕之后,开启直流高压电源,电压到达2500V左右时,溶液与不锈钢管之间的气体被击穿,产生明亮的微等离子体,随后立即调节电压使放电稳定运行,纳米氢氧化镁制备开始,反应20min。放电结束后,将沉淀产物离心分离过滤,并依此用乙醇和去离子水洗涤数次,最后置于60℃真空干 燥箱干燥6h。对所得产物作纯度、XRD及TEM分析。产物XRD图,经与Mg(OH)2标准图比较,各峰强度与位置与标准衍射图吻合,证明产物是Mg(OH)2。TEM分析表明产物具有规则的六方片状结构,粒度大小约60~200nm,分散性好,分布均匀。  Take a certain amount of seawater and mix well with 0.5mol/L NaOH, take 40mL of the solution and pour it into the reactor, and add ethylene glycol. Pass argon gas into the stainless steel needle tube, and its flow rate is controlled at 60 mL/min by a glass rotameter. After the device is connected, turn on the DC high-voltage power supply. When the voltage reaches about 2500V, the gas between the solution and the stainless steel tube is broken down to generate bright micro-plasma. Then adjust the voltage immediately to make the discharge run stably, and the preparation of nano-magnesium hydroxide begins. , react for 20min. After the discharge, the precipitated product was centrifuged and filtered, washed several times with ethanol and deionized water, and finally dried in a vacuum oven at 60°C for 6 hours. The obtained product was analyzed for purity, XRD and TEM. The XRD pattern of the product is compared with the standard pattern of Mg(OH) 2 , and the intensity and position of each peak are consistent with the standard diffraction pattern, which proves that the product is Mg(OH) 2 . TEM analysis shows that the product has a regular hexagonal sheet structure with a particle size of about 60-200nm, good dispersion and uniform distribution.

Claims (2)

1.一种微等离子体海水制备纳米氢氧化镁的方法,其特征在于该方法的步骤如下:将海水倒入微等离子体反应器,加入NaOH调节溶液初始pH值到一定值;打开氩气瓶,调节流量计控制气体流量,待气流稳定后开启直流高压电源,当电压达到2500V左右时,气体被击穿,形成微等离子体;随后立即调节电压使微等离子体稳定在一定电压和电流水平,反应正式开始;放电处理5~20min,完成纳米氢氧化镁的制备。1. A method for preparing nano-magnesium hydroxide from micro-plasma seawater is characterized in that the steps of the method are as follows: seawater is poured into a micro-plasma reactor, and NaOH is added to adjust the initial pH value of the solution to a certain value; the argon cylinder is opened , adjust the flowmeter to control the gas flow, and turn on the DC high-voltage power supply after the air flow is stable. When the voltage reaches about 2500V, the gas is broken down to form a micro plasma; then immediately adjust the voltage to stabilize the micro plasma at a certain voltage and current level, The reaction officially starts; the discharge treatment is 5-20 minutes, and the preparation of nano-magnesium hydroxide is completed. 2.根据权利要求1所述方法的一种微等离子体海水制备纳米氢氧化镁的装置,其特征在于包括微等离子体反应器、给微等离子体反应器供电的直流高压电源(1)和给微等离子体反应器供气的氩气瓶(9);微等离子体反应器采用玻璃反应器(5),溶液搅拌采用磁力搅拌器(8),阳极主体为毛细不锈钢管(3),氩气从氩气瓶经过玻璃转子流量计注入不锈钢电极体内直至反应器中;不锈钢电极垂直置于反应溶液上方,电极出气端距离溶液表面2mm;阴极为细钨棒(4);钨棒通过串联镇流电阻(2)与直流高压电源的接地端连接;启动直流高压电源后,不锈钢电极与液面之间产生微等离子体(6),体系形成通路。2. according to the device that a kind of micro-plasma seawater of method according to claim 1 prepares nano-magnesium hydroxide, it is characterized in that comprising micro-plasma reactor, the DC high-voltage power supply (1) that supplies power to micro-plasma reactor and power supply The argon bottle (9) for gas supply to the micro-plasma reactor; the micro-plasma reactor adopts a glass reactor (5), the solution is stirred using a magnetic stirrer (8), the anode body is a capillary stainless steel tube (3), and the argon gas The argon gas bottle is injected into the stainless steel electrode body through the glass rotameter to the reactor; the stainless steel electrode is placed vertically above the reaction solution, and the gas outlet of the electrode is 2mm away from the surface of the solution; the cathode is a thin tungsten rod (4); the tungsten rod is ballasted in series The resistor (2) is connected to the ground terminal of the DC high-voltage power supply; after the DC high-voltage power supply is started, micro-plasma (6) is generated between the stainless steel electrode and the liquid surface, and the system forms a path.
CN201410314174.5A 2014-07-01 2014-07-01 Method for preparing nano magnesium hydroxide from microplasma seawater Pending CN104118892A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104892974A (en) * 2015-06-26 2015-09-09 浙江海洋学院 Environment-friendly inorganic flame retardant
CN105926002A (en) * 2016-05-20 2016-09-07 西北师范大学 Method for preparing sheet-like nanometer Mg(OH)2 by using electrolytic diaphragm discharge plasma

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060060464A1 (en) * 2002-05-08 2006-03-23 Chang Chak M T Plasma formed in a fluid
CN101125669A (en) * 2007-07-13 2008-02-20 马敬环 Method for producing high-pure ultra-thin micro-powder magnesium hydroxide by extracting sea water
CN101973609A (en) * 2010-10-14 2011-02-16 中国科学院等离子体物理研究所 Method for removing soluble Cr (VI) in wastewater by utilizing electric arc discharge
CN103880048A (en) * 2012-12-23 2014-06-25 吕子玉 Method for extracting magnesium hydroxide from seawater

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060060464A1 (en) * 2002-05-08 2006-03-23 Chang Chak M T Plasma formed in a fluid
CN101125669A (en) * 2007-07-13 2008-02-20 马敬环 Method for producing high-pure ultra-thin micro-powder magnesium hydroxide by extracting sea water
CN101973609A (en) * 2010-10-14 2011-02-16 中国科学院等离子体物理研究所 Method for removing soluble Cr (VI) in wastewater by utilizing electric arc discharge
CN103880048A (en) * 2012-12-23 2014-06-25 吕子玉 Method for extracting magnesium hydroxide from seawater

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104892974A (en) * 2015-06-26 2015-09-09 浙江海洋学院 Environment-friendly inorganic flame retardant
CN105926002A (en) * 2016-05-20 2016-09-07 西北师范大学 Method for preparing sheet-like nanometer Mg(OH)2 by using electrolytic diaphragm discharge plasma

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Application publication date: 20141029