CN105372413B - Method and system for measuring total mass transfer coefficient of resin - Google Patents
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- 239000011347 resin Substances 0.000 title claims abstract description 143
- 229920005989 resin Polymers 0.000 title claims abstract description 142
- 238000012546 transfer Methods 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 87
- 238000005342 ion exchange Methods 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 91
- 239000012071 phase Substances 0.000 claims description 19
- 238000005259 measurement Methods 0.000 claims description 14
- 239000007791 liquid phase Substances 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 13
- 238000005070 sampling Methods 0.000 claims description 11
- 238000002955 isolation Methods 0.000 claims description 4
- 230000010354 integration Effects 0.000 claims description 2
- 238000013461 design Methods 0.000 abstract description 8
- 238000011160 research Methods 0.000 abstract description 6
- 238000001514 detection method Methods 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 description 37
- 239000003456 ion exchange resin Substances 0.000 description 13
- 229920003303 ion-exchange polymer Polymers 0.000 description 13
- 239000000243 solution Substances 0.000 description 12
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 9
- 238000009792 diffusion process Methods 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 7
- 238000000691 measurement method Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 3
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
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- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
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- G—PHYSICS
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- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
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Abstract
Description
技术领域technical field
本发明涉及树脂性能检测领域，特别是涉及一种树脂总传质系数测量方法和系统。The invention relates to the field of resin performance detection, in particular to a method and system for measuring the total mass transfer coefficient of resin.
背景技术Background technique
离子交换树脂在水处理领域需求量很大，约占离子交换树脂产量的90％左右，用于水中的各种阴阳离子的去除。目前，离子交换树脂的最大消耗量是用在火力发电厂的纯水处理上，其次是原子能、半导体、电子工业等。Ion exchange resins are in great demand in the field of water treatment, accounting for about 90% of the output of ion exchange resins, and are used to remove various anions and cations in water. At present, the largest consumption of ion exchange resins is used in the pure water treatment of thermal power plants, followed by atomic energy, semiconductors, and electronics industries.
离子交换树脂主要分为凝胶型树脂和大孔型树脂。凝胶型树脂的高分子骨架在干燥的情况下，内部没有毛细孔；而在吸水时会溶胀，在大分子链节间形成很微细的孔隙，通常称为显微孔，湿润树脂的平均孔径为2～4nm。这类树脂较适合用于吸附无机离子。大孔型树脂是在聚合反应时加入致孔剂，形成多孔海绵状构造的骨架，内部有大量永久性的微孔。大孔型树脂并存有微细孔和大网孔，润湿树脂的孔径达100～500nm，而孔道的表面积可以增大到超过1000m2/g。这不仅为离子交换提供了良好的接触条件，缩短了离子扩散的路程，还增加了许多链节活性中心，通过分子间的范德华引力产生分子吸附作用，能够像活性炭那样吸附各种非离子性物质，扩大其功能。Ion exchange resins are mainly divided into gel resins and macroporous resins. When the polymer skeleton of the gel-type resin is dry, there are no capillary pores inside; when it absorbs water, it will swell, forming very fine pores between the macromolecular chains, usually called micropores, and the average pore size of the wet resin 2 ~ 4nm. This type of resin is more suitable for the adsorption of inorganic ions. The macroporous resin is formed by adding a porogen during the polymerization reaction to form a porous sponge-like structure with a large number of permanent micropores inside. Macroporous resins have both micropores and large meshes. The pore diameter of the wetted resin reaches 100-500nm, and the surface area of the pores can increase to more than 1000m 2 /g. This not only provides good contact conditions for ion exchange, shortens the distance of ion diffusion, but also increases the active centers of many chain links, and generates molecular adsorption through the intermolecular van der Waals attraction, which can adsorb various non-ionic substances like activated carbon. , to expand its functionality.
离子交换过程除了受树脂自身性质影响外，还与交换过程有关。离子交换过程主要分为以下几个步骤：(1)水中的离子在水溶液中向树脂颗粒表面的扩散，即到达边界水膜层；(2)离子通过边界水膜的扩散；(3)离子在树脂颗粒网孔内的扩散；(4)溶液中离子和交换基团上的离子进行交换；(5)交换基团上的离子在树脂颗粒网孔内向颗粒表面扩散；(6)交换基团上的离子通过边界水膜的扩散；(7)交换基团上的离子从树脂表面边界水膜向水溶液的扩散。The ion exchange process is not only affected by the properties of the resin itself, but also related to the exchange process. The ion exchange process is mainly divided into the following steps: (1) the diffusion of ions in water to the surface of resin particles in the aqueous solution, that is, reaching the boundary water film layer; (2) the diffusion of ions through the boundary water film; (3) the diffusion of ions in the Diffusion in the mesh of resin particles; (4) The ions in the solution and the ions on the exchange group are exchanged; (5) The ions on the exchange group diffuse to the surface of the particle in the mesh of the resin particle; (6) On the exchange group Diffusion of ions through the boundary water film; (7) Diffusion of ions on the exchange group from the boundary water film on the resin surface to the aqueous solution.
离子交换过程必须相继通过以上几个步骤，其中消耗大部分时间的步骤称为速度控制步骤。通过测定树脂的总传质系数可以有效的判断离子交换过程的速度控制步骤，能够为离子交换器的设计和操作提供必要的基础数据。The ion exchange process must go through the above several steps successively, and the step that consumes most of the time is called the speed controlling step. By measuring the total mass transfer coefficient of the resin, the speed control step of the ion exchange process can be effectively judged, and the necessary basic data can be provided for the design and operation of the ion exchanger.
但是，目前还没有能够简便易行的测定树脂总传质系数的方法和系统。However, there is no method and system that can easily and easily measure the total mass transfer coefficient of resins at present.
发明内容Contents of the invention
基于此，有必要针对上述问题，提供一种树脂总传质系数测量方法和系统，采用该测量方法，能够方便的测定树脂总传质系数。Based on this, it is necessary to provide a method and system for measuring the total mass transfer coefficient of resin to solve the above problems, and the total mass transfer coefficient of resin can be conveniently measured by using the measurement method.
一种树脂总传质系数测量方法，包括以下步骤：A method for measuring resin total mass transfer coefficient, comprising the following steps:
将树脂放置在浅床中，以离子浓度为c1的料液均匀流过树脂，使离子交换反应达到平衡状态，获取流经树脂后料液的离子浓度c2和料液的体积流量q；The resin is placed in a shallow bed, and the feed liquid with an ion concentration of c 1 flows evenly through the resin, so that the ion exchange reaction reaches an equilibrium state, and the ion concentration c 2 of the feed liquid and the volume flow q of the feed liquid after flowing through the resin are obtained;
根据离子交换等温线，获取该离子与树脂相总平均浓度呈平衡的液相浓度c*；According to the ion exchange isotherm, obtain the total average concentration of the ion and the resin phase Equilibrium liquid phase concentration c*;
将上述得到的数据带入下式，计算得到树脂总传质系数Kfa Bring the data obtained above into the following formula to calculate the total mass transfer coefficient K fa of the resin
式中：In the formula:
Kfa为以液相推动力表示的总传质系数，单位为h-1；K fa is the total mass transfer coefficient represented by liquid-phase driving force, and the unit is h -1 ;
q为料液的体积流量，单位为m3/h；q is the volumetric flow rate of the feed liquid, in m 3 /h;
x为树脂量，单位为m3；x is the amount of resin, in m 3 ;
c1为流经树脂前料液的离子浓度，单位为mol/m3；c 1 is the ion concentration flowing through the resin front material liquid, and the unit is mol/m 3 ;
c2为流经树脂后料液的离子浓度，单位为mol/m3；c 2 is the ion concentration of the feed liquid after flowing through the resin, and the unit is mol/m 3 ;
c*为与树脂相总平均浓度呈平衡的液相浓度，单位为mol/m3。c* is the total average concentration of the resin phase Equilibrium liquid phase concentration, the unit is mol/m 3 .
上述树脂总传质系数测量方法的测定原理如下：The measurement principle of the above-mentioned resin total mass transfer coefficient measurement method is as follows:
利用浅床技术是测定交换速率、研究离子交换动力学的重要方法，而离子交换树脂在浅床中的传质过程为：The use of shallow bed technology is an important method to measure the exchange rate and study the kinetics of ion exchange, and the mass transfer process of ion exchange resin in the shallow bed is:
式中：(c-c*)m—Δt时刻内，该交换过程的平均推动力，mol/m3；In the formula: (cc*) m - the average driving force of the exchange process at time Δt, mol/m 3 ;
c—进出浅床料液的平均浓度，mol/m3；c—the average concentration of feed liquid entering and leaving the shallow bed, mol/m 3 ;
—树脂相总平均浓度，mol/m3； - total average concentration of resin phase, mol/m 3 ;
c*—与树脂相总平均浓度呈平衡的液相浓度，mol/m3；c*—total average concentration with resin phase Equilibrium liquid phase concentration, mol/m 3 ;
Kfa—以液相推动力表示的总传质系数，h-1。K fa —the overall mass transfer coefficient represented by liquid phase driving force, h -1 .
在操作过程中，Δt时间内流出液的体积为During operation, the volume of the effluent within Δt time is
ΔV＝q·Δt (2)ΔV=q·Δt (2)
式中：q—料液的体积流量，m3/h；In the formula: q—volume flow rate of feed liquid, m 3 /h;
浅床的物料衡算式为：The material balance formula for the shallow bed is:
式中：x—浅床中的树脂量，m3；In the formula: x—the amount of resin in the shallow bed, m 3 ;
c1—进入浅床前料液的离子浓度，mol/m3；c 1 - the ion concentration of the feed liquid before entering the shallow bed, mol/m 3 ;
c2—离开浅床后料液的离子浓度，mol/m3；c 2 - the ion concentration of the feed liquid after leaving the shallow bed, mol/m 3 ;
故由式(1)、式(4)和式(5)可推出总传质系数表达式Therefore, the expression of the total mass transfer coefficient can be deduced from formula (1), formula (4) and formula (5)
因此，本发明的测量方法中，通过将少量粒度均匀的规则球形树脂放置在浅床中，两端以不锈钢网等构件固定其位置，令一浓度为c1的高速恒流料液通过浅床，通过对流出曲线进行积分，可求出而q、x和c1均为已知，而c*可以从离子交换等温线求得，因此可求得该树脂的总传质系数。Therefore, in the measurement method of the present invention, by placing a small amount of regular spherical resin with uniform particle size in the shallow bed, the two ends fix its position with components such as stainless steel mesh, so that a high - speed constant flow feed liquid with a concentration of c1 passes through the shallow bed , and by integrating the outflow curve, one can find And q, x and c 1 are all known, and c* can be obtained from the ion exchange isotherm, so the total mass transfer coefficient of the resin can be obtained.
在其中一个实施例中，所述与树脂相总平均浓度呈平衡的液相浓度c*通过离子交换等温线计算得到。例如，通常的方法为：将一定比例的两种形态树脂浸泡在与树脂比例对应的溶液中，在恒温摇床中浸泡24小时，实验结束后测定溶液中所研究离子的浓度，并分别计算离子相浓度所占比例，带入实验前设定的树脂相比例，绘制离子交换等温曲线，即可从离子交换等温曲线中得到c*。In one of the embodiments, the total average concentration of the resin phase The equilibrium liquid phase concentration c* was calculated from the ion exchange isotherm. For example, the usual method is: soak a certain proportion of the two forms of resin in a solution corresponding to the proportion of the resin, soak it in a constant temperature shaker for 24 hours, measure the concentration of the ions in the solution after the experiment is over, and calculate the ion concentration respectively. The ratio of the phase concentration is brought into the resin phase ratio set before the experiment, and the ion-exchange isotherm curve is drawn, and c* can be obtained from the ion-exchange isotherm curve.
在其中一个实施例中，所述流经树脂后树脂相总平均浓度通过对流出曲线进行积分得到，具体为：当离子浓度为c1的料液均匀流过树脂后，分别记录流出液体积和测量流出液离子浓度，绘制流出曲线，并对其所组成的曲边梯形进行积分，即可得到树脂相总平均浓度 In one of the embodiments, the total average concentration of the resin phase after the flow through the resin It is obtained by integrating the outflow curve, specifically: when the material liquid with an ion concentration of c 1 flows through the resin evenly, record the volume of the outflow liquid and measure the ion concentration of the outflow liquid, draw the outflow curve, and compare the curved edges formed by it Trapezoidal integration, the total average concentration of the resin phase can be obtained
在其中一个实施例中，控制流经树脂的料液温度和流量保持恒定。确保离子交换反应达到一个稳定平衡的状态，有助于提高测量的稳定性和准确性。In one of the embodiments, the temperature and flow rate of the feed liquid flowing through the resin are controlled to be constant. Ensuring that the ion exchange reaction reaches a stable equilibrium state helps to improve the stability and accuracy of the measurement.
本发明还公开了一种树脂总传质系数测量系统，采用上述的测量方法，该测量系统包括The invention also discloses a measurement system for the total mass transfer coefficient of resin, adopting the above-mentioned measurement method, the measurement system includes
料液罐，用于储存离子浓度为c1的料液；Feed liquid tank, for storing the feed liquid whose ion concentration is c 1 ;
浅床，包括固定在一起的进水装置、连接装置和出水装置，所述连接装置内设有容纳树脂的树脂空腔，所述进水装置内设有与树脂空腔连通的进水通道，该进水通道通过管路连接料液罐，所述出水装置内设有与树脂空腔连通的出水通道，且所述树脂空腔与进水通道和出水通道之间均设有隔离网；The shallow bed includes a water inlet device, a connecting device and a water outlet device fixed together, the connecting device is provided with a resin cavity for containing resin, and the water inlet device is provided with a water inlet channel communicating with the resin cavity, The water inlet channel is connected to the feed liquid tank through a pipeline, and the water outlet device is provided with a water outlet channel communicating with the resin cavity, and an isolation net is provided between the resin cavity, the water inlet channel and the water outlet channel;
流量计，安装于料液流通的管路上，用于记录通过树脂的料液流量；The flow meter is installed on the pipeline in which the material liquid flows, and is used to record the flow rate of the material liquid passing through the resin;
水泵，安装于料液流通的管路上，用于促使料液由料液罐向浅床流动；以及The water pump is installed on the pipeline of the feed liquid, and is used to promote the flow of the feed liquid from the feed liquid tank to the shallow bed; and
取样阀，安装于与浅床出水通道连通的管路上，用于取样测定流经树脂后料液的离子浓度c2。The sampling valve is installed on the pipeline connected with the water outlet channel of the shallow bed, and is used for sampling and measuring the ion concentration c 2 of the feed liquid flowing through the resin.
上述测量系统，提供了一种可用于上述树脂总传质系数测量方法的系统装置，以料液罐储存离子浓度为c1的料液，以浅床提供离子交换反应的适宜环境，以流量计获取液相流的体积流量，以水泵提供液相流的动力，以取样阀提供便利的取样方式，获取流经树脂后料液的离子浓度c2，从而测定得到树脂总传质系数。The above-mentioned measurement system provides a system device that can be used in the method for measuring the total mass transfer coefficient of the above-mentioned resin. The feed liquid with an ion concentration of c1 is stored in a feed liquid tank, and a suitable environment for ion exchange reactions is provided with a shallow bed. The volumetric flow rate of the liquid phase flow is powered by a water pump, and a convenient sampling method is provided by a sampling valve to obtain the ion concentration c 2 of the feed liquid flowing through the resin, so as to measure the total mass transfer coefficient of the resin.
在其中一个实施例中，所述树脂空腔的直径大于所述进水通道和出水通道的直径。即在浅床内部采用锥形的设计，便于料液快速均匀流过树脂，促进反应达到平衡。In one of the embodiments, the diameter of the resin cavity is larger than the diameters of the water inlet channel and the water outlet channel. That is, the conical design is adopted inside the shallow bed, which facilitates the rapid and uniform flow of the feed liquid through the resin and promotes the reaction to reach equilibrium.
在其中一个实施例中，所述进水装置、连接装置和出水装置上均设有法兰凸缘盘，所述法兰凸缘盘上设有对应的连接孔，通过该连接孔和固定件将进水装置、连接装置和出水装置固定安装。该浅床采用法兰式的连接，便于安装和拆卸，以达到快速更换测量用树脂的目的。并且所述进水装置、连接装置和出水装置的法兰凸缘盘密封面之间设有垫片，进一步提高了浅床的密封性。In one of the embodiments, the water inlet device, the connection device and the water outlet device are all provided with a flange flange, and the flange flange is provided with a corresponding connection hole, through which the connection hole and the fixing piece Fix the water inlet device, connection device and water outlet device. The shallow bed adopts flange connection, which is easy to install and disassemble, so as to achieve the purpose of quickly replacing the measuring resin. In addition, gaskets are arranged between the sealing surfaces of the flange flanges of the water inlet device, the connection device and the water outlet device, which further improves the tightness of the shallow bed.
在其中一个实施例中，该测量系统还包括水浴装置，所述料液罐设于该水浴装置内。该水浴装置用于为料液罐加热保温。通过该水浴装置控制流经浅床料液的温度，能够研究不同温度对离子交换树脂总传质系数的影响。In one of the embodiments, the measurement system further includes a water bath device, and the feed liquid tank is arranged in the water bath device. The water bath device is used for heating and insulating the material liquid tank. By controlling the temperature of the feed liquid flowing through the shallow bed through the water bath device, the influence of different temperatures on the total mass transfer coefficient of the ion exchange resin can be studied.
在其中一个实施例中，所述料液罐和浅床之间的管路上还设有回水阀，所述流量计设于所述回水阀和所述浅床之间的管路上。通过流量计和回水阀的设置，可以精确控制料液流速，既能提高料液流速的稳定性，又可以根据研究需要改变流速，研究不同流速对离子交换树脂总传质系数的影响。In one of the embodiments, a return valve is further provided on the pipeline between the feed liquid tank and the shallow bed, and the flow meter is arranged on the pipeline between the return valve and the shallow bed. Through the setting of the flow meter and the return valve, the flow rate of the feed liquid can be precisely controlled, which can not only improve the stability of the flow rate of the feed liquid, but also change the flow rate according to the research needs, and study the influence of different flow rates on the total mass transfer coefficient of the ion exchange resin.
与现有技术相比，本发明具有以下有益效果：Compared with the prior art, the present invention has the following beneficial effects:
本发明的一种树脂总传质系数测量方法，能够通过测量一些易得的参数计算得到树脂总传质系数，为判断离子交换过程的速度控制步骤提供有效依据，并能够为离子交换器的设计和操作提供必要的基础数据，具有重要的研究意义。A method for measuring the total mass transfer coefficient of the resin of the present invention can calculate the total mass transfer coefficient of the resin by measuring some easily obtained parameters, provide an effective basis for judging the speed control steps of the ion exchange process, and can provide a basis for the design of the ion exchanger And operation provides the necessary basic data, which has important research significance.
本发明的一种树脂总传质系数测量系统，提供了一种可用于上述树脂总传质系数测量方法的系统装置，以料液罐、浅床、流量计、水泵和取样阀的配合，降低了树脂总传质系数测量的难度，为研究提供了便利条件。该测量系统能够自由更换浅床内装填的树脂，从而达到研究不同种类树脂的总传质系数的目的。A kind of resin total mass transfer coefficient measurement system of the present invention provides a kind of system device that can be used in the above-mentioned resin total mass transfer coefficient measurement method, with the cooperation of material liquid tank, shallow bed, flow meter, water pump and sampling valve, reduce It eliminates the difficulty of measuring the total mass transfer coefficient of resin and provides convenient conditions for research. The measurement system can freely replace the resin filled in the shallow bed, so as to achieve the purpose of studying the total mass transfer coefficient of different types of resins.
并且，该测量系统还可通过水浴装置、料液罐、回水阀和流量计分别控制流经浅床料液的温度、料液种类及浓度和流速等因素，从而研究不同影响因素对离子交换树脂总传质系数的影响。Moreover, the measurement system can also control the temperature, type, concentration and flow rate of the feed liquid flowing through the shallow bed through the water bath device, the feed liquid tank, the return valve and the flow meter, so as to study the impact of different influencing factors on the ion exchange. Influence of resin overall mass transfer coefficient.
附图说明Description of drawings
图1为实施例1测量系统各部件连接关系示意图；Fig. 1 is the schematic diagram of connection relationship of each component of the measurement system of embodiment 1;
图2为实施例1中浅床结构示意图；Fig. 2 is the shallow bed structure schematic diagram in embodiment 1;
图3为实施例1中浅床的进水装置或出水装置结构示意图；Fig. 3 is the structural representation of the water inlet device or the water outlet device of the shallow bed in embodiment 1;
图4为实施例1中浅床的连接装置结构示意图。Fig. 4 is a schematic structural diagram of the connecting device of the shallow bed in embodiment 1.
其中：100.料液罐；200.浅床；210.进水装置；211.进水通道；220.连接装置；221.树脂空腔；230.出水装置；231.出水通道；240.隔离网；300.流量计；400.水泵；500.取样阀；600.水浴装置；700.回水阀；800.稳压管。Among them: 100. Feed liquid tank; 200. Shallow bed; 210. Water inlet device; 211. Water inlet channel; 220. Connection device; 221. Resin cavity; 230. Water outlet device; 231. Water outlet channel; 240. Isolation net ; 300. Flow meter; 400. Water pump; 500. Sampling valve; 600. Water bath device; 700. Return valve; 800. Regulator tube.
具体实施方式detailed description
为了便于理解本发明，下面将参照相关附图对本发明进行更全面的描述。附图中给出了本发明的较佳实施例。但是，本发明可以以许多不同的形式来实现，并不限于本文所描述的实施例。相反地，提供这些实施例的目的是使对本发明的公开内容的理解更加透彻全面。In order to facilitate the understanding of the present invention, the present invention will be described more fully below with reference to the associated drawings. Preferred embodiments of the invention are shown in the accompanying drawings. However, the present invention can be embodied in many different forms and is not limited to the embodiments described herein. On the contrary, these embodiments are provided to make the understanding of the disclosure of the present invention more thorough and comprehensive.
需要说明的是，当元件被称为“固定”于另一个元件，它可以直接在另一个元件上或者也可以存在居中的元件。当一个元件被认为是“连通”另一个元件，它可以是直接连通到另一个元件或者可能同时存在居中元件。It should be noted that when an element is referred to as being “fixed” to another element, it can be directly on the other element or there can also be an intervening element. When an element is said to be "connected to" another element, it can be directly connected to the other element or intervening elements may also be present.
除非另有定义，本文所使用的所有的技术和科学术语与属于本发明的技术领域的技术人员通常理解的含义相同。本文中在本发明的说明书中所使用的术语只是为了描述具体的实施例的目的，不是旨在于限制本发明。Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the technical field of the invention. The terms used herein in the description of the present invention are for the purpose of describing specific embodiments only, and are not intended to limit the present invention.
实施例1Example 1
一种树脂总传质系数测量系统，如图1所示，包括料液罐100，浅床200，流量计300，水泵400，取样阀500。A system for measuring the total mass transfer coefficient of resin, as shown in FIG.
所述料液罐100用于储存离子浓度为c1的料液。The feed liquid tank 100 is used to store feed liquid with an ion concentration of c1.
如图2所示，所述浅床200包括固定在一起的进水装置210、连接装置220和出水装置230，所述连接装置220内设有容纳树脂的树脂空腔221，所述进水装置210内设有与树脂空腔221连通的进水通道211，该进水通道211通过管路连接料液罐100，所述出水装置230内设有与树脂空腔221连通的出水通道231，且所述树脂空腔221与进水通道211和出水通道231之间均设有隔离网240。As shown in Figure 2, the shallow bed 200 includes a water inlet device 210, a connecting device 220 and a water outlet device 230 fixed together, the connecting device 220 is provided with a resin cavity 221 for containing resin, and the water inlet device 210 is provided with a water inlet channel 211 communicating with the resin cavity 221, the water inlet channel 211 is connected to the feed liquid tank 100 through a pipeline, and the water outlet device 230 is provided with a water outlet channel 231 communicating with the resin cavity 221, and An isolation net 240 is provided between the resin cavity 221 and the water inlet channel 211 and the water outlet channel 231 .
上述树脂空腔221的直径大于所述进水通道211和出水通道231的直径。即在浅床内部采用锥形的设计，便于料液快速均匀流过树脂，使反应达到平衡。The diameter of the resin cavity 221 is larger than the diameters of the water inlet channel 211 and the water outlet channel 231 . That is to say, a conical design is adopted inside the shallow bed, which facilitates the rapid and uniform flow of the feed liquid through the resin and balances the reaction.
在本实施例中，如图3-4所示，所述进水装置210、连接装置220和出水装置230上均设有法兰凸缘盘，所述法兰凸缘盘上设有对应的连接孔，通过该连接孔和固定件将进水装置210、连接装置220和出水装置230固定安装。该浅床采用法兰式的连接，便于安装和拆卸，以达到快速更换测量用树脂的目的。并且所述进水装置、连接装置和出水装置的法兰凸缘盘密封面之间设有垫片，进一步提高了浅床的密封性。In this embodiment, as shown in Figure 3-4, the water inlet device 210, the connection device 220 and the water outlet device 230 are all provided with flange flanges, and the flange flanges are provided with corresponding The connection hole, through which the water inlet device 210, the connection device 220 and the water outlet device 230 are fixedly installed. The shallow bed adopts flange connection, which is easy to install and disassemble, so as to achieve the purpose of quickly replacing the measuring resin. In addition, gaskets are arranged between the sealing surfaces of the flange flanges of the water inlet device, the connection device and the water outlet device, which further improves the tightness of the shallow bed.
所述流量计300安装于料液流通的管路上，用于记录通过树脂的料液流量。The flow meter 300 is installed on the pipeline through which the feed liquid flows, and is used to record the flow rate of the feed liquid passing through the resin.
所述水泵400安装于料液流通的管路上，用于促使料液由料液罐100向浅床200流动。The water pump 400 is installed on the pipeline through which the feed liquid flows, and is used to promote the feed liquid to flow from the feed liquid tank 100 to the shallow bed 200 .
所述取样阀500安装于与浅床出水通道连通的管路上，用于取样测定流经树脂后料液的离子浓度c2。The sampling valve 500 is installed on the pipeline connected with the water outlet channel of the shallow bed, and is used for sampling and measuring the ion concentration c 2 of the feed liquid flowing through the resin.
在本实施例中，该测量系统还包括水浴装置600，所述料液罐100设于该水浴装置600内。该水浴装置600用于为料液罐100加热保温。通过该水浴装置600控制流经浅床料液的温度，能够研究不同温度对离子交换树脂总传质系数的影响。In this embodiment, the measurement system further includes a water bath device 600 , and the feed liquid tank 100 is disposed in the water bath device 600 . The water bath device 600 is used to heat and keep the material liquid tank 100 warm. By controlling the temperature of the feed liquid flowing through the shallow bed through the water bath device 600, the influence of different temperatures on the total mass transfer coefficient of the ion exchange resin can be studied.
在本实施例中，所述料液罐100和浅床200之间的管路上还设有回水阀700，所述流量计300设于所述回水阀700和所述浅床200之间的管路上。通过流量计300和回水阀700的设置，可以精确控制料液流速，既能提高料液流速的稳定性，又可以根据研究需要改变流速，研究不同流速对离子交换树脂总传质系数的影响。In this embodiment, a return valve 700 is also provided on the pipeline between the feed liquid tank 100 and the shallow bed 200, and the flow meter 300 is arranged between the return valve 700 and the shallow bed 200 on the pipeline. Through the setting of the flow meter 300 and the return valve 700, the flow rate of the material liquid can be precisely controlled, which can not only improve the stability of the flow rate of the material liquid, but also change the flow rate according to the research needs, and study the influence of different flow rates on the total mass transfer coefficient of the ion exchange resin .
在本实施例中，所述料液罐100内还设有稳压管800。In this embodiment, the feed liquid tank 100 is further provided with a voltage stabilizing pipe 800 .
采用本实施例的测量系统对树脂总传质系数进行测量，其方法步骤如下：The measurement system of the present embodiment is used to measure the total mass transfer coefficient of the resin, and the method steps are as follows:
首先，在浅床连接装置的树脂空腔内装入少量待测树脂，该树脂空腔两端放置不锈钢网(优选316L不锈钢)，将树脂限定于该树脂空腔内。再采用螺栓和螺母等固定件通过进水装置、连接装置和出水装置法兰凸缘盘上的连接孔将进水装置、连接装置和出水装置组合固定，并将该浅床安装在树脂总传质系数测量系统中。First, put a small amount of resin to be tested in the resin cavity of the shallow bed connection device, and place stainless steel mesh (preferably 316L stainless steel) at both ends of the resin cavity to limit the resin in the resin cavity. Then use fixing parts such as bolts and nuts to fix the water inlet device, connection device and water outlet device through the connection holes on the flange flanges of the water inlet device, connection device and water outlet device, and install the shallow bed on the resin main transmission In the quality coefficient measurement system.
其次，在料液罐中装入所需浓度c1的料液，调节恒温的水浴装置，达到实验所需温度，通过回水阀和流量计控制流经浅床的料液流速。Secondly, fill the feed liquid tank with the required concentration c1, adjust the constant temperature water bath device to reach the temperature required for the experiment, and control the flow rate of the feed liquid flowing through the shallow bed through the return valve and flow meter.
然后，定时从取样阀收集流出液，并测定其中待测物质的含量。于实验结束后，测定浅床内树脂中待测物质含量。Then, periodically collect the effluent from the sampling valve, and determine the content of the substance to be tested therein. After the experiment, the content of the substance to be tested in the resin in the shallow bed was measured.
最后，通过下式分析并计算离子交换树脂的总传质系数。Finally, the overall mass transfer coefficient of the ion exchange resin was analyzed and calculated by the following formula.
式中：In the formula:
Kfa为以液相推动力表示的总传质系数，单位为h-1；K fa is the total mass transfer coefficient represented by liquid-phase driving force, and the unit is h -1 ;
q为料液的体积流量，单位为m3/h；q is the volumetric flow rate of the feed liquid, in m 3 /h;
x为浅床内的树脂量，单位为m3；x is the amount of resin in the shallow bed, in m 3 ;
c1为流经树脂前料液的离子浓度，单位为mol/m3；c 1 is the ion concentration flowing through the resin front material liquid, and the unit is mol/m 3 ;
c2为流经树脂后料液的离子浓度，单位为mol/m3；c 2 is the ion concentration of the feed liquid after flowing through the resin, and the unit is mol/m 3 ;
c*为与树脂相总平均浓度呈平衡的液相浓度，单位为mol/m3。c* is the total average concentration of the resin phase Equilibrium liquid phase concentration, the unit is mol/m 3 .
下面以凝胶型阳离子树脂处理CuCl2溶液为例进行详细说明：实验采用的CuCl2溶液浓度为2mmol/L(即c1)，料液的体积流量为2.1L/h(即q)，浅床内树脂量为0.393cm3(即x)。The following is an example of the treatment of CuCl 2 solution with gel-type cationic resin for detailed description: the concentration of CuCl 2 solution used in the experiment is 2mmol/L (ie c 1 ), and the volume flow rate of the feed liquid is 2.1L/h (ie q). The amount of resin in the bed was 0.393 cm 3 (ie x).
将上述离子浓度c1为2mmol/L的CuCl2溶液均匀流过树脂，流出树脂的料液体积和离子浓度如表1所示。The above - mentioned CuCl solution with an ion concentration c1 of 2mmol/L evenly flows through the resin, and the volume and ion concentration of the resin flowing out of the resin are shown in Table 1.
表1流出树脂的料液体积和离子浓度Table 1 The feed liquid volume and ion concentration of outflow resin
根据表1绘制曲线，对所构成的曲边梯形进行积分，所得面积为故可求得与树脂相总平均浓度 Draw the curve according to Table 1, integrate the formed curved trapezoid, and the obtained area is Therefore, the total average concentration of the resin phase can be obtained
离子交换选择性系数采用静态浸泡法测定，即在二元体系中把一定组成的树脂放在总浓度固定，总体积不变的含两种离子的溶液中，保持温度恒定，维持一定时间，待达到交换平衡后，根据溶液中离子浓度的变化，来推测树脂中离子浓度的变化，并以此计算出该条件下的选择性系数。选择性系数计算公式如式(7)所示。The ion exchange selectivity coefficient is measured by the static immersion method, that is, in the binary system, a certain composition of resin is placed in a solution containing two ions with a fixed total concentration and a constant total volume, and the temperature is kept constant for a certain period of time. After reaching the exchange equilibrium, according to the change of the ion concentration in the solution, the change of the ion concentration in the resin is estimated, and the selectivity coefficient under this condition is calculated. The formula for calculating the selectivity coefficient is shown in formula (7).
式中：q全—树脂的全交换容量，mmol/ml；In the formula: qfull — the total exchange capacity of the resin, mmol/ml;
XCu—溶液中Cu2+的浓度分率,XCu＝c*/c1；X Cu —concentration fraction of Cu 2+ in the solution, X Cu ＝c*/c 1 ;
YCu—树脂相中Cu型树脂的浓度分率, Y Cu —concentration fraction of Cu type resin in the resin phase,
平衡过程是在恒温摇床中进行的，在摇动搅拌条件下维持24h，使离子交换达到充分平衡。实验结束后，测定溶液中Cu2+浓度，从而计算出溶液中Cu2+所占比率。离子交换实验设计如表2所示。实验结果如表3所示。The balance process is carried out in a constant temperature shaker, and maintained for 24 hours under the condition of shaking and stirring, so that the ion exchange can reach a full balance. After the experiment, the concentration of Cu 2+ in the solution was measured to calculate the proportion of Cu 2+ in the solution. The ion exchange experiment design is shown in Table 2. The experimental results are shown in Table 3.
表2.RH-Cu平衡体系设计数据Table 2. Design data of RH-Cu equilibrium system
注：C1为溶液的总浓度，QT为树脂相的全交换容量，qR2Cu、qRH分别为铜型离子交换树脂和氢型离子交换树脂的交换容量。Note: C 1 is the total concentration of the solution, Q T is the total exchange capacity of the resin phase, q R2Cu and q RH are the exchange capacities of the copper-type ion-exchange resin and the hydrogen-type ion-exchange resin, respectively.
表3.RH-Cu平衡体系选择性系数Table 3. Selectivity coefficient of RH-Cu equilibrium system
将上述测得的树脂相总平均浓度带入到离子交换树脂选择性系数计算方程中，即可求得与树脂相总平均浓度呈平衡的液相浓度c*。将c*带入式(6)中即可计算出相应的总传质系数，具体数据如表4所示。The total average concentration of the resin phase measured above Bringing it into the calculation equation of the selectivity coefficient of the ion exchange resin, the total average concentration of the resin phase can be obtained Equilibrium liquid phase concentration c*. The corresponding total mass transfer coefficient can be calculated by bringing c* into formula (6), and the specific data are shown in Table 4.
表4.总传质系数计算Table 4. Overall Mass Transfer Coefficient Calculation
通过上述方法步骤，本发明能够通过测量一些易得的参数计算得到树脂总传质系数，为判断离子交换过程的速度控制步骤提供有效依据，并能够为离子交换器的设计和操作提供必要的基础数据，具有重要的研究意义。Through the above method steps, the present invention can calculate the total mass transfer coefficient of the resin by measuring some easily obtained parameters, provide an effective basis for judging the speed control steps of the ion exchange process, and provide the necessary basis for the design and operation of the ion exchanger The data have important research significance.
以上所述实施例的各技术特征可以进行任意的组合，为使描述简洁，未对上述实施例中的各个技术特征所有可能的组合都进行描述，然而，只要这些技术特征的组合不存在矛盾，都应当认为是本说明书记载的范围。The technical features of the above-mentioned embodiments can be combined arbitrarily. To make the description concise, all possible combinations of the technical features in the above-mentioned embodiments are not described. However, as long as there is no contradiction in the combination of these technical features, should be considered as within the scope of this specification.
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。The above-mentioned embodiments only express several implementation modes of the present invention, and the descriptions thereof are relatively specific and detailed, but should not be construed as limiting the patent scope of the invention. It should be noted that those skilled in the art can make several modifications and improvements without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the patent for the present invention should be based on the appended claims.
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