CN101221155A - Photocatalytic separation membrane performance testing device and testing method - Google Patents

Photocatalytic separation membrane performance testing device and testing method Download PDF

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CN101221155A
CN101221155A CNA2007100195620A CN200710019562A CN101221155A CN 101221155 A CN101221155 A CN 101221155A CN A2007100195620 A CNA2007100195620 A CN A2007100195620A CN 200710019562 A CN200710019562 A CN 200710019562A CN 101221155 A CN101221155 A CN 101221155A
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separation film
separation membrane
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CN100538356C (en
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胡科研
崔平
李勇
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Hefei Institutes of Physical Science of CAS
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Abstract

本发明公开了一种光催化分离膜性能测试装置及其测试方法。装置为光催化分离膜(3)置于进口处依次连接有流量传感器(10)、电磁调节阀(11)、增减压器(12)和待测物容器(13)的待降解物容器(2)与出口处连接有检测器(4)的反应物容器(6)之间,光源(1)与光催化分离膜(3)平行设置,流量传感器(10)、电磁调节阀(11)、增减压器(12)和检测器(4)均与计算机(8)电连接;方法包括配制流体、选择检测器、确定光源,由计算机控制光降解过程,并根据流体的浓度和检测器测得的数据,按公式ρ=r/φ和吸附曲线计算出光催化分离膜的光催化量子效率和吸附量,从而获得光催化分离膜的性能。它能自动、全面地测试出光催化分离膜的性能。

Figure 200710019562

The invention discloses a photocatalytic separation membrane performance testing device and a testing method thereof. The device comprises a photocatalytic separation membrane (3) placed between a to-be-degraded material container (2) whose inlet is sequentially connected with a flow sensor (10), an electromagnetic regulating valve (11), a pressure regulator (12) and a to-be-tested material container (13) and a reactant container (6) whose outlet is connected with a detector (4); a light source (1) and the photocatalytic separation membrane (3) are arranged in parallel; the flow sensor (10), the electromagnetic regulating valve (11), the pressure regulator (12) and the detector (4) are all electrically connected with a computer (8); the method comprises preparing a fluid, selecting a detector, determining a light source, controlling the photodegradation process by a computer, and calculating the photocatalytic quantum efficiency and adsorption amount of the photocatalytic separation membrane according to the formula ρ=r/φ and an adsorption curve based on the concentration of the fluid and the data measured by the detector, thereby obtaining the performance of the photocatalytic separation membrane. The device can automatically and comprehensively test the performance of the photocatalytic separation membrane.

Figure 200710019562

Description

光催化分离膜性能测试装置及其测试方法 Photocatalytic separation membrane performance testing device and testing method

技术领域  technical field

本发明涉及一种测试装置及测试方法,尤其是光催化分离膜性能测试装置及其测试方法。The invention relates to a test device and a test method, in particular to a photocatalytic separation membrane performance test device and a test method.

背景技术 Background technique

光催化技术可以充分利用取之不尽、用之不竭的太阳能,在常温常压、不消耗其他能源和材料的条件下将水分解产生氢气、降解一系列的有机化合物和一些如细菌、病菌、病毒等微生物,从而有效地解决社会可持续发展所面临的可再生能源和环境污染这两个问题。作为实现光催化技术的物质基础,光催化剂的性能起着决定性的作用,在将其实际应用前,如能定量地知悉光催化剂的性能指标,则极利于其效能的充分发挥。为此,人们作了一些尝试和努力,试图建立起相应的测试装置和测试方法,以对光催化剂产品的性能进行定量的测试,如在2003年4月9日公开的中国发明专利申请公开说明书CN 1409109A中披露的一种“纳米粉体材料光催化性能评估方法”。它包括建立光催化装置,配制光催化降解溶液,添加待评估的纳米粉体材料,光催化降解反应,离心、取溶液,测定末吸光度和评估纳米粉体材料光催化性能七个操作步骤,其中的光催化装置由夹层式恒温反应器中置有紫外灯和搅拌子构成。但是,无论是这种评估方法,还是实现方法的装置均存在着不足之处,首先,仅能对纳米粉体材料的光催化性能进行测试,而不能对光催化分离膜的性能进行测试;其次,操作步骤繁杂,极易出错;最后,自动化程度低,不能实时地在线评估。Photocatalytic technology can make full use of the inexhaustible and inexhaustible solar energy, decompose water to generate hydrogen, degrade a series of organic compounds and some such as bacteria and germs at normal temperature and pressure without consuming other energy and materials. , viruses and other microorganisms, thus effectively solving the two problems of renewable energy and environmental pollution faced by the sustainable development of society. As the material basis for realizing photocatalytic technology, the performance of photocatalyst plays a decisive role. Before its practical application, if the performance index of photocatalyst can be known quantitatively, it will be very beneficial to give full play to its effectiveness. For this reason, people have made some attempts and efforts to try to set up corresponding test devices and test methods to quantitatively test the performance of photocatalyst products, as disclosed in the Chinese invention patent application published on April 9, 2003 A "method for evaluating the photocatalytic performance of nanopowder materials" disclosed in CN 1409109A. It includes seven steps of establishing a photocatalytic device, preparing a photocatalytic degradation solution, adding the nanopowder material to be evaluated, photocatalytic degradation reaction, centrifugation, taking the solution, measuring the final absorbance and evaluating the photocatalytic performance of the nanopowder material, among which The photocatalytic device consists of a sandwich-type constant temperature reactor with an ultraviolet lamp and a stirrer. However, both the evaluation method and the device for realizing the method have shortcomings. First, only the photocatalytic performance of the nanopowder material can be tested, but the performance of the photocatalytic separation membrane cannot be tested; secondly, , the operation steps are complicated and error-prone; finally, the degree of automation is low, and real-time online evaluation cannot be performed.

发明内容 Contents of the invention

本发明要解决的技术问题为克服现有技术中的不足之处,提供一种结构简单、自动化程度高,使用方便的光催化分离膜性能测试装置及其测试方法。The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, and provide a photocatalytic separation membrane performance test device and its test method with simple structure, high degree of automation and convenient use.

光催化分离膜性能测试装置包括光源、反应容器和其内置的光催化物,特别是(a)所说反应容器包含相连通的待降解物容器和反应物容器,所说光催化物为光催化分离膜,所说光催化分离膜置于所说待降解物容器与反应物容器之间,且将待降解物容器与反应物容器相隔离;(b)所说光源置于待降解物容器一侧,且与光催化分离膜平行设置;(c)所说待降解物容器的进口处依次连接有流量传感器、电磁调节阀、增减压器和待测物容器,所说反应物容器的出口处连接有检测器,所说流量传感器、电磁调节阀、增减压器和检测器均与计算机电连接。The photocatalytic separation membrane performance testing device includes a light source, a reaction vessel and a built-in photocatalyst, especially (a) the reaction vessel includes a connected container of the degraded substance and a reactant container, and the photocatalyst is a photocatalyst Separation membrane, the photocatalytic separation membrane is placed between the container of the object to be degraded and the container of the reactant, and the container of the object to be degraded is isolated from the container of the reactant; (b) the light source is placed between the container of the object to be degraded and side, and set in parallel with the photocatalytic separation membrane; (c) the inlet of said container to be degraded is connected with a flow sensor, an electromagnetic regulating valve, a pressure regulator and an object container in sequence, and the outlet of said reactant container A detector is connected at the place, and the flow sensor, the electromagnetic regulating valve, the pressure regulator and the detector are all electrically connected with the computer.

作为光催化分离膜性能测试装置的进一步改进,所述的光源为可见光或紫外光;所述的可见光为波长为500nm的可见光,紫外光为波长为365nm的紫外光或波长为254nm的紫外光;所述的待降解物容器中置有压力传感器,所说压力传感器与计算机电连接;所述的反应物容器中置有温度传感器,所说温度传感器与计算机电连接;所述的检测器为紫外-可见光分光光度计或气相色谱仪或相应气体的专用气体检测仪;所述的检测器与容器相连接。As a further improvement of the photocatalytic separation membrane performance testing device, the light source is visible light or ultraviolet light; the visible light is visible light with a wavelength of 500nm, and the ultraviolet light is ultraviolet light with a wavelength of 365nm or ultraviolet light with a wavelength of 254nm; A pressure sensor is placed in the container to be degraded, and the pressure sensor is electrically connected to the computer; a temperature sensor is placed in the reactant container, and the temperature sensor is electrically connected to the computer; the detector is an ultraviolet - a visible light spectrophotometer or a gas chromatograph or a dedicated gas detector for corresponding gases; the detector is connected to the container.

光催化分离膜性能测试装置的测试方法包括待降解物的配制和光的催化,特别是方法包含以下步骤:(a)根据测试目的,配制相应的流体,对于液相的光催化降解反应,配制溶液,对于气相的光催化降解反应,配制气体;(b)根据测试需要,选择相应的检测器,对于液相流体的光催化降解反应,选择紫外-可见光分光光度计,对于气相流体的光催化降解反应,选择气相色谱仪或相应气体的专用气体检测仪;(c)根据待测的光催化分离膜的类型,确定光源为可见光或紫外光;(d)由计算机按设定的流量控制光降解的过程,并由检测器测得降解数据;(e)由计算机根据配制流体的浓度和测得的数据,按公式计算出光催化分离膜的光催化量子效率,式中:ρ为催化剂的量子产率、r为反应速率(每秒反应的分子摩尔数)、

Figure A20071001956200052
为光子流量(每秒有效光子数);(f)由计算机按吸附曲线计算出光催化分离膜的吸附量,从而获得所测试的光催化分离膜的性能。The test method of the photocatalytic separation membrane performance test device includes the preparation of the degraded substance and the photocatalysis, especially the method includes the following steps: (a) according to the purpose of the test, prepare the corresponding fluid, and prepare the solution for the photocatalytic degradation reaction in the liquid phase , for the photocatalytic degradation reaction of the gas phase, prepare the gas; (b) according to the test needs, select the corresponding detector, for the photocatalytic degradation reaction of the liquid phase fluid, select the ultraviolet-visible spectrophotometer, for the photocatalytic degradation of the gas phase fluid reaction, select a gas chromatograph or a special gas detector for the corresponding gas; (c) determine the light source as visible light or ultraviolet light according to the type of photocatalytic separation membrane to be tested; (d) control the photodegradation by the computer according to the set flow rate process, and the degradation data is measured by the detector; (e) by the computer according to the concentration of the prepared fluid and the measured data, according to the formula Calculate the photocatalytic quantum efficiency of the photocatalytic separation membrane, where: ρ is the quantum yield of the catalyst, r is the reaction rate (molecule number of reactions per second),
Figure A20071001956200052
is the photon flux (the number of effective photons per second); (f) Calculate the adsorption amount of the photocatalytic separation membrane by the computer according to the adsorption curve, so as to obtain the performance of the tested photocatalytic separation membrane.

作为光催化分离膜性能测试装置的测试方法的进一步改进,所述的溶液为20μmol/L的亚甲基蓝流体或20mg/L的苯酚流体;所述的气体为5μmol/L的甲醛流体或5μmol/L的三氯乙烯流体。As a further improvement of the test method of the photocatalytic separation membrane performance testing device, the solution is 20 μmol/L methylene blue fluid or 20 mg/L phenol fluid; the gas is 5 μmol/L formaldehyde fluid or 5 μmol/L Trichlorethylene fluid.

相对于现有技术的有益效果是,其一,采用将光催化分离膜置于待降解物容器与反应物容器之间,并将两者相隔离,光源置于待降解物容器一侧,且与光催化分离膜平行设置的结构,为使用液相流体或气相流体待降解物测试光催化分离膜奠定了物质基础。选用于待降解物容器的进口处依次连接流量传感器、电磁调节阀、增减压器和待测物容器,反应物容器的出口处连接检测器,且流量传感器、电磁调节阀、增减压器和检测器均与计算机电连接的构造,增加了测试装置的自动化程度,使测试的过程具有了智能化;其二,测试装置的整体结构简单、造价低,运行可靠,测试和分析的种类齐全,既能测试光催化分离膜对液相流体的降解性能、又能测试其对气相流体的降解性能,且测试的速度快,数据重现性好;其三,测试方法科学可行,且贴近和涵盖了被测试的光催化分离膜可能的使用范围,测试的步骤简洁,测定的数据真实可靠,可作为被测光催化分离膜实际使用时的直接依据。Compared with the beneficial effects of the prior art, first, the photocatalytic separation membrane is placed between the container of the degraded product and the reactant container, and the two are isolated, the light source is placed on one side of the container of the degraded product, and The structure arranged in parallel with the photocatalytic separation membrane lays a material foundation for testing the photocatalytic separation membrane with liquid phase fluid or gas phase fluid to be degraded. It is selected to connect the flow sensor, electromagnetic regulating valve, pressure increaser and pressure reducer, and the object to be tested at the inlet of the container to be degraded, and the detector is connected to the outlet of the reactant container, and the flow sensor, electromagnetic regulating valve, pressure increaser and pressure reducer The structure in which the tester and the detector are electrically connected to the computer increases the degree of automation of the testing device and makes the testing process intelligent; secondly, the overall structure of the testing device is simple, low in cost, reliable in operation, and has a complete range of testing and analysis. , it can not only test the degradation performance of the photocatalytic separation membrane on the liquid phase fluid, but also test its degradation performance on the gas phase fluid, and the test speed is fast and the data reproducibility is good; thirdly, the test method is scientific and feasible, and it is close to and Covering the possible use range of the tested photocatalytic separation membrane, the test steps are simple, the measured data is true and reliable, and can be used as a direct basis for the actual use of the tested photocatalytic separation membrane.

作为有益效果的进一步体现,一是光源为可见光或紫外光,可见光的波长优选为500nm的可见光,紫外光的波长优选为365nm的紫外光或254nm的紫外光,既使被测试的光催化分离膜的受光范围得到了较大的扩展,又对常用的被测试的光催化分离膜的光敏性具有了针对性;二是待降解物容器和反应物容器中还分别置有与计算机电连接的压力传感器和温度传感器,它们均提升了测试装置的智能化程度,使测得的结果更具有了可比性;三是检测器采用紫外-可见光分光光度计或气相色谱仪或相应气体的专用气体检测仪,使其不仅能适用于液相光催化降解反应的测试,也能适用于气相光催化降解反应的测试;四是溶液选用20μmol/L的亚甲基蓝流体或20mg/L的苯酚流体,完全有代表性地测试出了光催化分离膜于液相流体条件下的性能;五是气体选为5μmol/L的甲醛流体或5μmol/L的三氯乙烯流体,即可有代表性地测试出光催化分离膜于气相流体条件下的性能。As a further embodiment of the beneficial effect, one is that the light source is visible light or ultraviolet light, the wavelength of visible light is preferably 500nm visible light, and the wavelength of ultraviolet light is preferably 365nm ultraviolet light or 254nm ultraviolet light, even if the tested photocatalytic separation membrane The light-receiving range has been greatly expanded, and it is also targeted at the photosensitivity of the commonly used photocatalytic separation membranes; the second is that the container of the degraded product and the container of the reactant are respectively equipped with a pressure sensor that is electrically connected to the computer. Sensors and temperature sensors, both of which have improved the intelligence of the test device, making the measured results more comparable; the third is that the detector uses a UV-visible spectrophotometer or a gas chromatograph or a special gas detector for the corresponding gas , so that it can be applied not only to the test of liquid-phase photocatalytic degradation reaction, but also to the test of gas-phase photocatalytic degradation reaction; the fourth is that the solution is 20μmol/L methylene blue fluid or 20mg/L phenol fluid, which is completely representative The performance of the photocatalytic separation membrane under the condition of liquid phase fluid has been thoroughly tested; the fifth is that the gas is selected as 5 μmol/L formaldehyde fluid or 5 μmol/L trichlorethylene fluid, which can representatively test the performance of the photocatalytic separation membrane in the liquid phase. Performance under gas-phase fluid conditions.

附图说明 Description of drawings

下面结合附图对本发明的优选方式作进一步详细的描述。The preferred modes of the present invention will be further described in detail below in conjunction with the accompanying drawings.

图1是本发明光催化分离膜性能测试装置的一种基本结构示意图;Fig. 1 is a kind of basic structure schematic diagram of photocatalytic separation membrane performance testing device of the present invention;

图2是亚甲基蓝于图1所示测试装置上被待测光催化分离膜降解前后的浓度变化图,其中,横坐标为时间,纵坐标为浓度,图中的A点为光照的起始点;Fig. 2 is the concentration change diagram of methylene blue on the test device shown in Fig. 1 before and after being degraded by the photocatalytic separation membrane to be tested, wherein, the abscissa is time, the ordinate is concentration, and point A in the figure is the starting point of illumination;

图3是亚甲基蓝于图1所示测试装置上被待测光催化分离膜降解前后的压力变化图,其中,横坐标为时间,纵坐标为压力,图中的A点为光照的起始点。Fig. 3 is a diagram of the pressure change of methylene blue before and after being degraded by the photocatalytic separation membrane to be tested on the test device shown in Fig. 1, wherein the abscissa is time, the ordinate is pressure, and point A in the figure is the starting point of illumination.

具体实施方式 Detailed ways

参见图1,光催化分离膜性能测试装置的构造为:光催化分离膜3置于相连通的待降解物容器2和反应物容器6之间,并将其相隔离。光源1置于待降解物容器2一侧,且与光催化分离膜3平行设置;其中,光源1根据被测试的光催化分离膜来选用可见光或紫外光,若选可见光,则选波长为500nm的可见光,若选紫外光,则选波长为365nm的紫外光或波长为254nm的紫外光。待降解物容器2中置有压力传感器9,待降解物容器2的进口处依次连接有流量传感器10、电磁调节阀11、增减压器12和待测物容器13。反应物容器6中置有温度传感器7,反应物容器6的出口处依次连接有检测器4和容器5;其中,检测器4为紫外-可见光分光光度计(当用液相流体降解测试时;若用气相流体降解测试时,则使用气相色谱仪或相应气体的专用气体检测仪)。上述压力传感器9、流量传感器10、电磁调节阀11、增减压器12、检测器4和温度传感器7均与计算机8电连接。Referring to FIG. 1 , the structure of the photocatalytic separation membrane performance test device is as follows: the photocatalytic separation membrane 3 is placed between the connected container 2 of the degraded substance and the container 6 of the reactant, and isolates them. The light source 1 is placed on the side of the container 2 of the to-be-degraded substance, and is arranged parallel to the photocatalytic separation membrane 3; wherein, the light source 1 selects visible light or ultraviolet light according to the photocatalytic separation membrane to be tested, and if visible light is selected, the wavelength is 500nm Visible light, if you choose ultraviolet light, then choose the ultraviolet light with a wavelength of 365nm or the ultraviolet light with a wavelength of 254nm. A pressure sensor 9 is placed in the container 2 of the degradation product, and a flow sensor 10 , an electromagnetic regulating valve 11 , a pressure increaser and pressure reducer 12 , and a container 13 for the sample to be detected are sequentially connected to the inlet of the degradation product container 2 . A temperature sensor 7 is placed in the reactant container 6, and the outlet of the reactant container 6 is connected with a detector 4 and a container 5 in sequence; wherein, the detector 4 is an ultraviolet-visible spectrophotometer (when using a liquid phase fluid for degradation testing; If the gas phase fluid is used for the degradation test, use a gas chromatograph or a dedicated gas detector for the corresponding gas). The above-mentioned pressure sensor 9 , flow sensor 10 , electromagnetic regulating valve 11 , pressure increaser and pressure reducer 12 , detector 4 and temperature sensor 7 are all electrically connected to the computer 8 .

参见图1、图2和图3,光催化分离膜性能测试装置的测试方法为:Referring to Figure 1, Figure 2 and Figure 3, the test method of the photocatalytic separation membrane performance test device is:

实施例1:按以下步骤依次完成测试:a)根据测试二氧化钛光催化分离膜降解液相亚甲基蓝的活性之目的,配制20μmol/L的亚甲基蓝溶液后将其置于待测物容器中。b)选择检测器为紫外-可见光分光光度计,用于测试反应后的亚甲基蓝溶液的浓度。c)将待测试的光催化分离膜安装于相连通的待降解物容器和反应物容器之间,并将其相隔离。确定光源为紫外光,其波长选为365nm、光子流量选为每秒6.94×10-7摩尔光子,将该紫外光源安装在待降解物容器一侧,且与光催化分离膜平行设置。d)由计算机按设定的1m3/h的流量控制光降解的过程,计算机根据实际流量与设定流量的差发出信号调节电磁调节阀以保持流量的稳定。其中的亚甲基蓝在紫外光源和光催化分离膜的共同作用下被降解,降解后的亚甲基蓝溶液流经紫外-可见光分光光度计得到反应物容器出口处的亚甲基蓝浓度变化曲线,紫外-可见光分光光度计的输出由计算机记录并控制降解的进程。e)由计算机根据亚甲基蓝溶液降解前后的浓度差,得出反应速率为每秒反应1.388×10-8摩尔分子,光催化分离膜的光催化量子效率为2%(由公式

Figure A20071001956200071
计算出)。f)由计算机以待测试的光催化分离膜于无光照时对亚甲基蓝引起的浓度变化曲线是其对亚甲基蓝的吸附曲线,计算出被测试的光催化分离膜的吸附量为0.01mg,从而获得所测试的光催化分离膜的性能。Embodiment 1: Complete the test in sequence according to the following steps: a) According to the purpose of testing the activity of the titanium dioxide photocatalytic separation membrane to degrade the liquid phase methylene blue, after preparing a 20 μmol/L methylene blue solution, place it in the container of the test object. b) The detector is selected as an ultraviolet-visible spectrophotometer, which is used to test the concentration of the methylene blue solution after the reaction. c) installing the photocatalytic separation membrane to be tested between the connected container of the degraded substance and the reactant container, and isolating them. Determine that the light source is ultraviolet light with a wavelength of 365nm and a photon flux of 6.94×10 -7 moles of photons per second. The ultraviolet light source is installed on the side of the container of the degraded product and arranged in parallel with the photocatalytic separation membrane. d) The process of photodegradation is controlled by the computer according to the set flow rate of 1m 3 /h, and the computer sends a signal to adjust the electromagnetic regulating valve according to the difference between the actual flow rate and the set flow rate to maintain the flow rate stability. Wherein the methylene blue is degraded under the joint action of the ultraviolet light source and the photocatalytic separation membrane, and the methylene blue solution after the degradation flows through the ultraviolet-visible light spectrophotometer to obtain the methylene blue concentration change curve at the outlet of the reactant container, and the output of the ultraviolet-visible light spectrophotometer The degradation process is recorded and controlled by a computer. e) According to the concentration difference before and after the degradation of the methylene blue solution by the computer, the reaction rate is 1.388×10 -8 mole molecules per second, and the photocatalytic quantum efficiency of the photocatalytic separation membrane is 2% (by the formula
Figure A20071001956200071
Calculate). f) The concentration change curve caused by the photocatalytic separation membrane to be tested to methylene blue in the absence of light is its adsorption curve to methylene blue by the computer, and the adsorption amount of the tested photocatalytic separation membrane is calculated to be 0.01mg, thereby obtaining the obtained The performance of the photocatalytic separation membrane was tested.

实施例2:按以下步骤依次完成测试:a)根据测试二氧化钛光催化分离膜降解液相苯酚的活性之目的,配制20mg/L的苯酚溶液后将其置于待测物容器中。b)选择检测器为紫外-可见光分光光度计,用于测试反应后的苯酚溶液的浓度。c)将待测试的光催化分离膜安装于相连通的待降解物容器和反应物容器之间,并将其相隔离。确定光源为紫外光,其波长选为254nm、光子流量选为每秒8.02×10-7摩尔光子,将该紫外光源安装在待降解物容器一侧,且与光催化分离膜平行设置。d)由计算机按设定的0.5m3/h的流量控制光降解的过程,计算机根据实际流量与设定流量的差发出信号调节电磁调节阀以保持流量的稳定。其中的苯酚在紫外光源和光催化分离膜的共同作用下被降解,降解后的苯酚溶液流经紫外-可见光分光光度计得到反应物容器出口处的苯酚浓度变化曲线,紫外-可见光分光光度计的输出由计算机记录并控制降解的进程。e)由计算机根据苯酚溶液降解前后的浓度差,得出反应速率为每秒反应1.604×10-9摩尔分子,光催化分离膜的光催化量子效率为0.2%(由公式

Figure A20071001956200081
计算出)。f)由计算机以待测试的光催化分离膜于无光照时对苯酚引起的浓度变化曲线是其对苯酚的吸附曲线,计算出被测试的光催化分离膜的吸附量为10-4mg,从而获得所测试的光催化分离膜的性能。Embodiment 2: Complete the test in sequence according to the following steps: a) According to the purpose of testing the activity of titanium dioxide photocatalytic separation membrane to degrade phenol in the liquid phase, a 20 mg/L phenol solution is prepared and then placed in the container to be tested. b) The detector is selected as an ultraviolet-visible spectrophotometer, which is used to test the concentration of the phenol solution after the reaction. c) installing the photocatalytic separation membrane to be tested between the connected container of the degraded substance and the reactant container, and isolating them. Determine that the light source is ultraviolet light with a wavelength of 254nm and a photon flux of 8.02×10 -7 moles of photons per second. The ultraviolet light source is installed on the side of the container of the degraded product and arranged in parallel with the photocatalytic separation membrane. d) The process of photodegradation is controlled by the computer according to the set flow rate of 0.5m 3 /h, and the computer sends a signal to adjust the electromagnetic regulating valve according to the difference between the actual flow rate and the set flow rate to maintain the stability of the flow rate. The phenol therein is degraded under the combined action of the ultraviolet light source and the photocatalytic separation membrane, and the degraded phenol solution flows through the ultraviolet-visible light spectrophotometer to obtain the phenol concentration change curve at the outlet of the reactant container, and the output of the ultraviolet-visible light spectrophotometer The degradation process is recorded and controlled by a computer. e) According to the concentration difference before and after the degradation of the phenol solution by the computer, the reaction rate is 1.604×10 -9 mole molecules per second, and the photocatalytic quantum efficiency of the photocatalytic separation membrane is 0.2% (by the formula
Figure A20071001956200081
Calculate). f) The concentration curve of phenol caused by the photocatalytic separation membrane to be tested is the adsorption curve of phenol by the computer, and the adsorption capacity of the tested photocatalytic separation membrane is calculated to be 10 -4 mg, thus The performance of the tested photocatalytic separation membrane was obtained.

实施例3:按以下步骤依次完成测试:a)根据测试二氧化钛光催化分离膜降解气相甲醛的活性之目的,配制5μmol/L的甲醛气体后将其置于待测物容器中。b)选择检测器为甲醛专用气体检测仪,用于测试反应后的甲醛气体的浓度。c)将待测试的光催化分离膜安装于相连通的待降解物容器和反应物容器之间,并将其相隔离。确定光源为紫外光,其波长选为254nm、光子流量选为每秒6.94×10-7摩尔光子,将该紫外光源安装在待降解物容器一侧,且与光催化分离膜平行设置。d)由计算机按设定的1m3/h的流量控制光降解的过程,计算机根据实际流量与设定流量的差发出信号调节电磁调节阀以保持流量的稳定。其中的甲醛气体在紫外光源和光催化分离膜的共同作用下被降解,降解后的甲醛气体流经甲醛专用气体检测仪得到反应物容器出口处的甲醛浓度变化曲线,甲醛专用气体检测仪的输出由计算机记录并控制降解的进程。e)由计算机根据甲醛气体降解前后的浓度差,得出反应速率为每秒反应3.47×10-8摩尔分子,光催化分离膜的光催化量子效率为5%(由公式

Figure A20071001956200091
计算出)。f)由计算机以待测试的光催化分离膜于无光照时对甲醛引起的浓度变化曲线是其对甲醛的吸附曲线,计算出被测试的光催化分离膜的吸附量为10-6mg,从而获得所测试的光催化分离膜的性能。Example 3: The test was completed in sequence according to the following steps: a) According to the purpose of testing the activity of the titanium dioxide photocatalytic separation membrane to degrade formaldehyde in the gas phase, 5 μmol/L of formaldehyde gas was prepared and placed in the container of the test object. b) The detector is selected as a special gas detector for formaldehyde, which is used to test the concentration of formaldehyde gas after the reaction. c) installing the photocatalytic separation membrane to be tested between the connected container of the degraded substance and the reactant container, and isolating them. Determine that the light source is ultraviolet light, its wavelength is selected as 254nm, and the photon flux is selected as 6.94×10 -7 moles of photons per second. The ultraviolet light source is installed on the side of the container of the degraded product, and is arranged in parallel with the photocatalytic separation membrane. d) The process of photodegradation is controlled by the computer according to the set flow rate of 1m 3 /h, and the computer sends a signal to adjust the electromagnetic regulating valve according to the difference between the actual flow rate and the set flow rate to maintain the flow rate stability. The formaldehyde gas in it is degraded under the joint action of the ultraviolet light source and the photocatalytic separation membrane. The degraded formaldehyde gas flows through the special gas detector for formaldehyde to obtain the formaldehyde concentration change curve at the outlet of the reactant container. The output of the special gas detector for formaldehyde is obtained by A computer records and controls the progress of degradation. e) According to the concentration difference before and after the degradation of formaldehyde gas by the computer, the reaction rate is 3.47×10 -8 mole molecules per second, and the photocatalytic quantum efficiency of the photocatalytic separation membrane is 5% (by the formula
Figure A20071001956200091
Calculate). f) The concentration change curve of the photocatalytic separation membrane to be tested to formaldehyde in the absence of light is its adsorption curve to formaldehyde by the computer, and the adsorption capacity of the tested photocatalytic separation membrane is calculated to be 10 -6 mg, thus The performance of the tested photocatalytic separation membrane was obtained.

实施例4:按以下步骤依次完成测试:a)根据测试掺杂的二氧化钛光催化分离膜降解气相三氯乙烯的活性之目的,配制5μmol/L的三氯乙烯气体后将其置于待测物容器中。b)选择检测器为气相色谱仪,用于测试反应后的三氯乙烯气体的浓度。c)将待测试的光催化分离膜安装于相连通的待降解物容器和反应物容器之间,并将其相隔离。确定光源为紫外光,其波长选为500nm、光子流量选为每秒5.12×10-7摩尔光子,将该紫外光源安装在待降解物容器一侧,且与光催化分离膜平行设置。d)由计算机按设定的1m3/h的流量控制光降解的过程,计算机根据实际流量与设定流量的差发出信号调节电磁调节阀以保持流量的稳定。其中的三氯乙烯气体在紫外光源和光催化分离膜的共同作用下被降解,降解后的三氯乙烯气体流经气相色谱仪得到反应物容器出口处的三氯乙烯浓度变化曲线,气相色谱仪的输出由计算机记录并控制降解的进程。e)由计算机根据三氯乙烯气体降解前后的浓度差,得出反应速率为每秒反应1.536×10-8摩尔分子,光催化分离膜的光催化量子效率为3%(由公式

Figure A20071001956200092
计算出)。f)由计算机以待测试的光催化分离膜于无光照时对三氯乙烯引起的浓度变化曲线是其对三氯乙烯的吸附曲线,计算出被测试的光催化分离膜的吸附量为10-5mg,从而获得所测试的光催化分离膜的性能。Embodiment 4: complete the test in sequence according to the following steps: a) According to the purpose of testing the activity of the titanium dioxide photocatalytic separation membrane degrading the gas phase trichlorethylene, after preparing 5 μ mol/L of trichlorethylene gas, place it on the test object in the container. b) The detector is selected as a gas chromatograph, which is used to test the concentration of the reacted trichlorethylene gas. c) installing the photocatalytic separation membrane to be tested between the connected container of the degraded substance and the reactant container, and isolating them. Determine that the light source is ultraviolet light, its wavelength is selected as 500nm, and the photon flux is selected as 5.12×10 -7 moles of photons per second. The ultraviolet light source is installed on the side of the container of the degraded product, and is arranged in parallel with the photocatalytic separation membrane. d) The process of photodegradation is controlled by the computer according to the set flow rate of 1m 3 /h, and the computer sends a signal to adjust the electromagnetic regulating valve according to the difference between the actual flow rate and the set flow rate to maintain the flow rate stability. The trichlorethylene gas is degraded under the joint action of the ultraviolet light source and the photocatalytic separation membrane, and the degraded trichlorethylene gas flows through the gas chromatograph to obtain the trichlorethylene concentration change curve at the outlet of the reactant container, and the gas chromatograph The output is recorded by computer and the progress of degradation is controlled. e) According to the concentration difference before and after the degradation of trichlorethylene gas by the computer, the reaction rate is 1.536×10 -8 mole molecules per second, and the photocatalytic quantum efficiency of the photocatalytic separation membrane is 3% (by the formula
Figure A20071001956200092
Calculate). f) The concentration change curve caused by the photocatalytic separation membrane to be tested to trichlorethylene when there is no light is its adsorption curve to trichlorethylene by the computer, and the adsorption capacity of the tested photocatalytic separation membrane is calculated to be 10 − 5 mg to obtain the performance of the tested photocatalytic separation membrane.

显然,本领域的技术人员可以对本发明的光催化分离膜性能测试装置及其测试方法进行各种改动和变型而不脱离本发明的精神和范围。这样,倘若本发明的这些修改和变型属于本发明权利要求及其等同技术的范围之内,则本发明也意图包含这些改动和变型在内。Apparently, those skilled in the art can make various changes and modifications to the photocatalytic separation membrane performance testing device and testing method of the present invention without departing from the spirit and scope of the present invention. Thus, if these modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalent technologies, the present invention also intends to include these modifications and variations.

Claims (10)

1. a photocatalysis separation film performance test device comprises light source (1), reaction vessel and its built-in photocatalysis thing, it is characterized in that:
(a) said reaction vessel comprise be connected treat degradation product container (2) and reaction vessel (6), said photocatalysis thing is photocatalysis separation film (3), said photocatalysis separation film (3) places said treating between degradation product container (2) and the reaction vessel (6), and will treat that degradation product container (2) and reaction vessel (6) are isolated;
(b) said light source (1) places and treats degradation product container (2) one sides, and be arranged in parallel with photocatalysis separation film (3);
(c) the said inflow point of degradation product container (2) that treats is connected with flow sensor (10), solenoid valve (11), increase and decrease depressor (12) and determinand container (13) in turn, the exit of said reaction vessel (6) is connected with detecting device (4), and said flow sensor (10), solenoid valve (11), increase and decrease depressor (12) and detecting device (4) all are electrically connected with computing machine (8).
2. photocatalysis separation film performance test device according to claim 1 is characterized in that light source (1) is visible light or ultraviolet light.
3. photocatalysis separation film performance test device according to claim 2 is characterized in that visible light is that wavelength is the visible light of 500nm, and ultraviolet light is that wavelength is that ultraviolet light or the wavelength of 365nm is the ultraviolet light of 254nm.
4. photocatalysis separation film performance test device according to claim 1 is characterized in that treating being equipped with in the degradation product container (2) pressure transducer (9), and said pressure transducer (9) is electrically connected with computing machine (8).
5. photocatalysis separation film performance test device according to claim 1 is characterized in that being equipped with in the reaction vessel (6) temperature sensor (7), and said temperature sensor (7) is electrically connected with computing machine (8).
6. photocatalysis separation film performance test device according to claim 1 is characterized in that detecting device (4) is ultraviolet-visible spectrophotometer or gas chromatograph.
7. according to claim 1 or 6 described photocatalysis separation film performance test devices, it is characterized in that detecting device (4) is connected with container (5).
8. the method for testing of photocatalysis separation film performance test device according to claim 1 comprises the preparation for the treatment of degradation product and the catalysis of light, it is characterized in that said method comprises following steps:
(a) according to test purpose, prepare corresponding fluid, for the photocatalytic degradation reaction of liquid phase, obtain solution is for the photocatalytic degradation reaction of gas phase, preparation gas;
(b) according to the test needs, select the relevant detection device,, select ultraviolet-visible spectrophotometer,, select gas chromatograph for the photocatalytic degradation reaction of gaseous fluid for the photocatalytic degradation reaction of liquid phase fluid;
(c), determine that light source is visible light or ultraviolet light according to the type of photocatalysis separation film to be measured;
(d) record degradation data by the photodegradative process of flow control of computing machine, and by detecting device by setting;
(e) by computing machine according to the concentration of formulated fluids and the data that record, by formula Calculate the photocatalysis quantum efficiency of photocatalysis separation film, in the formula: the quantum yield of ρ catalyzer, r be reaction rate,
Figure A2007100195620003C2
Be the photon flow;
(f) calculate the adsorbance of photocatalysis separation film by computing machine by adsorption curve, thereby obtain the performance of the photocatalysis separation film tested.
9. the method for testing of photocatalysis separation film performance test device according to claim 8 is characterized in that solution is the methylene blue fluid of 20pmol/L or the phenol fluid of 20mg/L.
10. the method for testing of photocatalysis separation film performance test device according to claim 8 is characterized in that gas is the formaldehyde fluid of 5 μ mol/L or the triclene fluid of 5 μ mol/L.
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CN107748136B (en) * 2017-09-26 2020-04-28 河海大学 Multifunctional photocatalytic film performance test system and test method thereof

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