CN115683767A - A method and device for evaluating the high-temperature dispersion performance of a dispersant for nuclear power plants - Google Patents

A method and device for evaluating the high-temperature dispersion performance of a dispersant for nuclear power plants Download PDF

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CN115683767A
CN115683767A CN202211251636.4A CN202211251636A CN115683767A CN 115683767 A CN115683767 A CN 115683767A CN 202211251636 A CN202211251636 A CN 202211251636A CN 115683767 A CN115683767 A CN 115683767A
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kettle
solution
temperature
dispersant
sampling
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刘佳露
但体纯
陈银强
桂春
吴申奥
操容
王骏
叶张瀚
李江鹏
张君伟
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China Nuclear Power Operation Technology Corp Ltd
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Abstract

The invention relates to the field of deposit management, in particular to a method and a device for evaluating high-temperature dispersion performance of a dispersing agent for a nuclear power station. The automatic temperature measuring device comprises a kettle body, wherein the kettle body comprises a heating furnace, the upper part of the heating furnace is covered with a kettle cover, the kettle cover is respectively connected with a kettle inner gas outlet pipe, a kettle inner sampling pipe, a kettle inner sample inlet pipe, a temperature measuring sleeve pipe and a kettle inner gas inlet pipe, the middle of the kettle cover is connected with a stirrer, the kettle inner sample inlet pipe is connected with a needle valve through a pipeline, the needle valve is connected with a metering pump through a pipeline, and the metering pump is connected with a spring type safety valve through a pipeline; the pressure gauge on the sample inlet pipeline is connected with the water tank through a pipeline; the sampling pipe in the kettle is connected with one end of the cooler and a ball valve through pipelines, the ball valve is arranged between the sampling pipe in the kettle and the cooler, and the other end of the cooler is connected with the ball valve; the temperature measuring sleeve is connected with the control cabinet, and the control cabinet is connected with the pressure transmitter and the stirrer. The advantages are that: the evaluation of the dispersing effect of a single dispersant product can be achieved.

Description

一种核电站用分散剂的高温分散性能评价方法及装置A method and device for evaluating the high-temperature dispersion performance of a dispersant for nuclear power plants

技术领域technical field

本发明涉及核电厂蒸汽发生器的沉积物管理技术领域,具体涉及一种核电站用分散剂的高温分散性能评价方法及装置。The invention relates to the technical field of deposit management of steam generators in nuclear power plants, in particular to a method and device for evaluating the high-temperature dispersion performance of dispersants used in nuclear power plants.

背景技术Background technique

压水堆核电站通常采用两种措施来使蒸汽发生器(SG)内表面上沉积物最小化:源项控制和末端清除;前者宗旨是减少进入SG的给水中腐蚀产物的量,后者则是利用化学或机械手段从SG去除现有沉积物(例如化学清洗、水力冲洗等)。采用以上措施可以使SG主给水中腐蚀产物含量显著降低,然而在机组正常功率运行期间腐蚀产物一旦进入SG,就没有有效的化学措施可用于抑制其在SG二次侧的沉积;因此,进入SG的腐蚀产物高达90%均沉积在其表面上。滞留在SG二次侧的泥渣若长时间未清除,则会导致SG传热管传热效率的降低、SG出口压力的下降等问题,严重情况下甚至导致传热管的腐蚀穿孔等,威胁SG的安全运行。为此,核电领域发展了一种在核电机组功率运行期间抑制腐蚀产物沉积的分散剂积污控制技术;常规做法是在核电机组功率运行期间将分散剂在线添加至SG给水系统中,以抑制腐蚀产物的沉积并防止腐蚀产物粘附到SG构件表面上,并最终通过SG排污系统有效地将腐蚀产物从SG中排出。这种技术主要依靠分散剂产品对腐蚀产物的高效分散性能。现有分散剂的评价方法主要集中于其阻垢性能,如国家标准GB/T 16632-2008“水处理剂阻垢性能的测定碳酸钙沉积法”;但是,核电站用分散剂的作用对象大部分是铁氧化物(如Fe3O4等)颗粒,其应用工况多为高温高压(如280℃饱和蒸汽)条件。Pressurized water reactor nuclear power plants usually adopt two measures to minimize deposits on the inner surface of the steam generator (SG): source term control and terminal removal; the purpose of the former is to reduce the amount of corrosion products in the feed water entering the SG, and the latter is to Remove existing deposits from SG using chemical or mechanical means (e.g. chemical cleaning, hydroflushing, etc.). The above measures can significantly reduce the content of corrosion products in the SG main feed water. However, once the corrosion products enter the SG during the normal power operation of the unit, there are no effective chemical measures to inhibit their deposition on the secondary side of the SG; therefore, the corrosion products entering the SG Up to 90% of the corrosion products are deposited on its surface. If the sludge remaining on the secondary side of the SG is not removed for a long time, it will lead to problems such as a decrease in the heat transfer efficiency of the SG heat transfer tube and a drop in the outlet pressure of the SG. In severe cases, it may even lead to corrosion and perforation of the heat transfer tube, threatening Safe operation of SG. For this reason, the field of nuclear power has developed a dispersant fouling control technology that inhibits the deposition of corrosion products during the power operation of nuclear power units; the conventional practice is to add dispersants online to the SG water supply system during power operation of nuclear power units to inhibit corrosion The deposition of products prevents corrosion products from adhering to the surface of SG components, and finally effectively discharges corrosion products from SG through the SG sewage system. This technology mainly relies on the efficient dispersion performance of dispersant products for corrosion products. The evaluation methods of existing dispersants mainly focus on their scale inhibition performance, such as the national standard GB/T 16632-2008 "Calcium Carbonate Deposition Method for Determination of Scale Inhibition Performance of Water Treatment Agents"; however, most of the dispersants used in nuclear power plants are It is iron oxide (such as Fe 3 O 4 , etc.) particles, and its application conditions are mostly high temperature and high pressure (such as 280°C saturated steam) conditions.

发明内容Contents of the invention

本发明的目的是提供一种核电站用分散剂的高温分散性能评价方法及装置,能够有效解决散剂产品分散效果的评价问题。The purpose of the present invention is to provide a method and device for evaluating the high-temperature dispersion performance of a dispersant for nuclear power plants, which can effectively solve the problem of evaluating the dispersion effect of powder products.

本发明的技术方案如下:一种核电站用分散剂的高温分散性能评价装置,包括釜体,釜体包括加热炉,加热炉上部盖有釜盖,釜盖上分别连接有釜内出气管、釜内取样管、釜内进样管、测温套管和釜内进气管,压力表、爆破式安全阀和压力变送器通过管线连接釜盖,釜盖的中间连接有搅拌器,釜内进样管通过管线连接针阀,针阀通过管线连接计量泵,计量泵通过管线连接弹簧式安全阀;进样管线上压力表通过管线与水箱连接;釜内取样管通过管线与冷却器的一端以及一个球阀连接,釜内取样管与冷却器之间设置球阀,冷却器的另一端与球阀连接;测温套管与控制柜连接,控制柜与压力变送器和搅拌器连接。The technical scheme of the present invention is as follows: a high-temperature dispersion performance evaluation device for a dispersant used in a nuclear power plant, comprising a kettle body, the kettle body includes a heating furnace, the upper part of the heating furnace is covered with a kettle cover, and the kettle cover is respectively connected with a gas outlet pipe in the kettle, a kettle The inner sampling pipe, the sampling pipe in the kettle, the temperature measuring sleeve and the inlet pipe in the kettle, the pressure gauge, the explosion safety valve and the pressure transmitter are connected to the kettle cover through pipelines, and the middle of the kettle cover is connected with a stirrer, and the inside of the kettle is The sample tube is connected to the needle valve through the pipeline, the needle valve is connected to the metering pump through the pipeline, and the metering pump is connected to the spring safety valve through the pipeline; the pressure gauge on the sampling pipeline is connected to the water tank through the pipeline; A ball valve is connected, a ball valve is set between the sampling pipe in the kettle and the cooler, and the other end of the cooler is connected to the ball valve; the temperature measuring sleeve is connected to the control cabinet, and the control cabinet is connected to the pressure transmitter and the agitator.

所述的测温套管、釜内取样管和釜内进气管插入到加热炉的下部,釜内进样管和釜内出气管插入到加热炉的上部。The temperature measuring sleeve, the sampling pipe in the kettle and the inlet pipe in the kettle are inserted into the lower part of the heating furnace, and the sampling pipe in the kettle and the gas outlet pipe in the kettle are inserted into the upper part of the heating furnace.

所述的搅拌器的转轴和搅拌桨深入到加热炉的底部。The rotating shaft and stirring paddle of the agitator go deep into the bottom of the heating furnace.

一种核电站用分散剂的高温分散性能评价方法,包含以下步骤:A method for evaluating the high-temperature dispersion performance of a dispersant for nuclear power plants, comprising the following steps:

步骤1:溶液配置及物料准备;Step 1: Solution configuration and material preparation;

步骤2:试验装置的调试及运行;Step 2: Commissioning and operation of the test device;

步骤3:取样样品的测试及分析。Step 3: Test and analyze the sample.

所述的步骤1包括配置浓度为200~1000μg/L的联氨溶液,用10%氨水调溶液pH25℃至8~10,标记为“溶液A”,作为背景溶液;The step 1 includes configuring a hydrazine solution with a concentration of 200-1000 μg/L, adjusting the pH of the solution from 25°C to 8-10 with 10% ammonia water, and marking it as "solution A" as a background solution;

配置ppb~ppm级别浓度的分散剂溶液,用氨水或乙醇胺调溶液pH25℃至8~10,标记为“溶液B”,作为分散剂试验溶液;Prepare a dispersant solution with a concentration of ppb~ppm, adjust the pH of the solution from 25°C to 8~10 with ammonia water or ethanolamine, and mark it as "solution B" as a dispersant test solution;

配置纳米级或微米级铁氧化物溶液,标记为“溶液C”。Prepare a nanoscale or microscale iron oxide solution, labeled as "Solution C".

所述的步骤2包括如下:Described step 2 comprises as follows:

步骤21:依次将“溶液A”和定量“溶液C”倒入清洗干净的高压釜内,搅拌混匀,此时釜内氧化物颗粒相应元素浓度值记录为C。将定量“溶液A”倒入在线补给装置的水箱中,用于装置运行期间高压釜内液体的补给;Step 21: Pour "Solution A" and quantitative "Solution C" into the cleaned autoclave in turn, stir and mix well, and record the corresponding element concentration value of the oxide particles in the autoclave as C. Pour the quantitative "solution A" into the water tank of the online replenishment device for the replenishment of the liquid in the autoclave during the operation of the device;

步骤22:按照高压釜操作规程拧紧釜盖,将进/出导气管、搅拌、在线补给、在线取样装置连接组装完毕。Step 22: Tighten the lid of the autoclave according to the operating procedures of the autoclave, and connect and assemble the inlet/outlet air duct, stirring, online supply, and online sampling devices.

步骤23:关闭液体取样/补给阀门,打开进/出气阀,在进气阀处连接氮气储存装置,向釜内通入N2以除去釜内空气和液体中溶解氧,除氧完毕后依次关闭N2气瓶、出气阀、进气阀;Step 23: Close the liquid sampling/supply valve, open the air inlet/outlet valve, connect the nitrogen gas storage device at the inlet valve, and feed N2 into the kettle to remove the air in the kettle and the dissolved oxygen in the liquid, and close them in turn after deoxygenation is completed N 2 cylinders, outlet valve, inlet valve;

步骤24:打开搅拌装置,设置较低的搅拌速率(20~100r/min),对釜内液体进行低速搅拌。Step 24: Turn on the stirring device, set a low stirring rate (20-100r/min), and stir the liquid in the kettle at a low speed.

步骤25:按照高压釜温度设定程序设置升温速率和运行温度,待釜内液体升温至设定温度且温度/压力稳定后,每隔一定时间在线取样一次,每次将取出来的样品转入干净的取样瓶中,分别标记为样品Z0-1、Z0-2、Z0-3…Z0-n,储存待测。每次取样后观察显示器上温度/压力值的变化,若温度偏离超过1℃或压力偏离超过0.2MPa时,及时补充因取样而损失的釜内液体量;以上步骤21~步骤25即为第一阶段试验;Step 25: Set the heating rate and operating temperature according to the autoclave temperature setting program. After the liquid in the autoclave is heated up to the set temperature and the temperature/pressure is stable, take samples online at regular intervals, and transfer the taken out samples into the In clean sampling bottles, marked as samples Z 0-1 , Z 0-2 , Z 0-3 ... Z 0-n , and stored for testing. Observe the change of the temperature/pressure value on the display after each sampling. If the temperature deviates by more than 1°C or the pressure deviates by more than 0.2MPa, timely replenish the amount of liquid in the kettle lost due to sampling; the above steps 21 to 25 are the first stage test;

步骤26:将在线补给水箱中液体更换为“溶液B”,利用在线补给泵向釜内补给定量“溶液B”,使釜内分散剂与颗粒的质量比控制在100:1~1:100,待温度/压力稳定后,每隔一定时间在线取样一次,每次将取出来的样品转入干净的取样瓶中,分别标记为样品Zt-1、Zt-2、Zt-3…Zt-n,储存待测。每次取样后观察显示器上温度/压力值的变化,若温度偏离超过2℃或压力偏离超过0.2MPa时,及时补充因取样而损失的釜内液体量;即为第二阶段试验;Step 26: Replace the liquid in the online make-up water tank with "solution B", and use the online make-up pump to supply a certain amount of "solution B" into the kettle, so that the mass ratio of dispersant to particles in the kettle is controlled at 100:1~1:100, After the temperature/pressure is stabilized, take samples online at regular intervals, transfer the taken samples into clean sampling bottles each time, and mark them as samples Z t-1 , Z t-2 , Z t-3 ... Z tn , stored for testing. Observe the change of temperature/pressure value on the display after each sampling. If the temperature deviates by more than 2°C or the pressure deviates by more than 0.2MPa, timely replenish the amount of liquid in the kettle lost due to sampling; it is the second stage of the test;

步骤27:试验结束,待釜内液体自然冷却至室温后,依次打开排气阀和釜盖,排尽釜内液体,将高压釜清洗干净,备用。Step 27: After the test is over, after the liquid in the autoclave is naturally cooled to room temperature, open the exhaust valve and the lid of the autoclave in turn, drain the liquid in the autoclave, clean the autoclave, and set it aside.

所述的步骤3包括如下:Described step 3 comprises as follows:

将取样样品酸化,使颗粒完全溶解,然后可采用电感耦合等离子体原子发射光谱仪测定相关元素含量,样品Z0-1、Z0-2、Z0-3…Z0-n的测试结果分别记录为C0-1、C0-2、C0-3…C0-n,样品Zt-1、Zt-2、Zt-3…Zt-n的测试结果分别记录为Ct-1、Ct-2、Ct-3…Ct-nAcidify the sampling sample to completely dissolve the particles, then use an inductively coupled plasma atomic emission spectrometer to measure the content of relevant elements, and record the test results of samples Z 0-1 , Z 0-2 , Z 0-3 ... Z 0-n respectively C 0-1 , C 0-2 , C 0-3 ... C 0-n , the test results of samples Z t-1 , Z t-2 , Z t-3 ... Z tn are recorded as C t-1 , Ct -2 , Ct -3 ... Ctn ;

第一阶段试验过程中,空白组颗粒的悬浮率η0计算公式为:During the first phase of the test, the suspension rate η of the blank group particles The calculation formula is:

Figure BDA0003887953060000041
Figure BDA0003887953060000041

第二阶段试验过程中,测试组颗粒的悬浮率ηt计算公式为:During the second stage of the test, the calculation formula of the suspension rate η t of the test group particles is:

Figure BDA0003887953060000042
Figure BDA0003887953060000042

分散剂的分散效率η计算公式为:The formula for calculating the dispersion efficiency η of the dispersant is:

η=ηt0 η=η t0

其中,η0代表上述试验工况条件下未添加分散剂时因搅拌等背景因素导致的釜内溶液中颗粒的悬浮率,ηt代表上述试验工况条件下添加分散剂后釜内溶液中颗粒的悬浮率,两者差值η代表上述试验工况条件下因分散剂作用导致的釜内溶液中颗粒的悬浮率。Wherein, η 0 represents the suspension rate of particles in the solution in the kettle caused by background factors such as stirring when no dispersant is added under the above-mentioned test working conditions, and η t represents the particles in the solution in the kettle after adding the dispersant under the above-mentioned test working conditions The suspension rate of the two, and the difference η represents the suspension rate of the particles in the solution in the kettle caused by the action of the dispersant under the above-mentioned test conditions.

本发明的有益效果在于:按照本发明的方法可以评价分散剂在模拟核电机组功率运行工况下的高温分散效果,不仅可以实现单一分散剂产品分散效果的评价,而且可以实现不同分散剂产品分散效果的对比分析。此评价方法为核电站用分散剂产品的高温分散效果评价提供一种切实可行的实施方案和计算方法。The beneficial effect of the present invention is that: according to the method of the present invention, the high-temperature dispersion effect of the dispersant under the power operation condition of the simulated nuclear power unit can be evaluated, not only the evaluation of the dispersion effect of a single dispersant product can be realized, but also the dispersion of different dispersant products can be realized. Comparative analysis of effects. This evaluation method provides a feasible implementation plan and calculation method for the evaluation of high temperature dispersion effect of dispersant products used in nuclear power plants.

附图说明Description of drawings

图1为本发明所提供的一种核电站用分散剂的高温分散性能评价装置示意图。Fig. 1 is a schematic diagram of a high-temperature dispersion performance evaluation device for a nuclear power plant dispersant provided by the present invention.

图中:1釜盖,2釜体,3加热炉,4控制柜,5测温套管,6搅拌器,7釜盖上压力表,8爆破式安全阀,9压力变送器,10釜内取样管,11冷却器,12球阀,13釜内进样管,14针阀,15计量泵,16进样管线上压力表,17弹簧式安全阀,18水箱,19釜内进气管,20釜内出气管。In the figure: 1 kettle cover, 2 kettle body, 3 heating furnace, 4 control cabinet, 5 temperature measuring sleeve, 6 agitator, 7 pressure gauge on the kettle cover, 8 blasting safety valve, 9 pressure transmitter, 10 kettle Inner sampling pipe, 11 cooler, 12 ball valve, 13 sampling pipe in the kettle, 14 needle valve, 15 metering pump, 16 pressure gauge on the sampling pipeline, 17 spring safety valve, 18 water tank, 19 inlet pipe in the kettle, 20 The outlet pipe in the kettle.

具体实施方式Detailed ways

下面结合附图及具体实施例对本发明作进一步详细说明。The present invention will be described in further detail below in conjunction with the accompanying drawings and specific embodiments.

如图1所示,一种核电站用分散剂的高温分散性能评价装置,包括釜体2,釜体2包括加热炉3,加热炉3上部盖有釜盖1,釜盖1上分别连接有釜内出气管20、釜内取样管10、釜内进样管13、测温套管5和釜内进气管19,其中,测温套管5、釜内取样管10和釜内进气管19插入到加热炉3的下部,釜内进样管13和釜内出气管20插入到加热炉3的上部,釜盖上压力表7、爆破式安全阀8和压力变送器9通过管线连接釜盖1,釜盖1的中间连接有搅拌器6,搅拌器6的转轴和搅拌桨深入到加热炉3的底部,釜内进样管13通过管线连接针阀14,针阀14通过管线连接计量泵15,计量泵15通过管线连接弹簧式安全阀17;进样管线上压力表16通过管线与水箱18连接;釜内取样管10通过管线与冷却器11的一端以及一个球阀连接,釜内取样管10与冷却器11之间设置球阀,冷却器11的另一端与球阀12连接;测温套管5与控制柜4连接,控制柜4与压力变送器9和搅拌器6连接。As shown in Figure 1, a high-temperature dispersion performance evaluation device for a dispersant used in a nuclear power plant includes a kettle body 2, the kettle body 2 includes a heating furnace 3, the upper part of the heating furnace 3 is covered with a kettle cover 1, and the kettle cover 1 is respectively connected with a kettle Inner outlet pipe 20, sampling pipe 10 in the kettle, sampling pipe 13 in the kettle, temperature measuring sleeve 5 and air inlet pipe 19 in the kettle, wherein, the temperature measuring sleeve 5, sampling pipe 10 in the kettle and air inlet pipe 19 in the kettle are inserted To the lower part of the heating furnace 3, the sample inlet pipe 13 in the kettle and the gas outlet pipe 20 in the kettle are inserted into the upper part of the heating furnace 3, and the pressure gauge 7, explosion safety valve 8 and pressure transmitter 9 on the kettle cover are connected to the kettle cover through pipelines 1. An agitator 6 is connected to the middle of the kettle cover 1. The rotating shaft and the stirring paddle of the agitator 6 go deep into the bottom of the heating furnace 3. The sampling pipe 13 in the kettle is connected to the needle valve 14 through the pipeline, and the needle valve 14 is connected to the metering pump through the pipeline. 15, the metering pump 15 is connected to the spring safety valve 17 through the pipeline; the pressure gauge 16 on the sampling pipeline is connected to the water tank 18 through the pipeline; the sampling pipe 10 in the kettle is connected to one end of the cooler 11 and a ball valve through the pipeline, and the sampling pipe in the kettle A ball valve is set between 10 and cooler 11, and the other end of cooler 11 is connected to ball valve 12; temperature measuring sleeve 5 is connected to control cabinet 4, and control cabinet 4 is connected to pressure transmitter 9 and agitator 6.

本发明提供的一种核电站用分散剂的高温分散性能评价方法,包含以下步骤:A method for evaluating the high-temperature dispersion performance of a dispersant for nuclear power plants provided by the invention comprises the following steps:

步骤1:溶液配置及物料准备Step 1: Solution configuration and material preparation

配置一定浓度(200~1000μg/L)的联氨溶液,用10%氨水调溶液pH25℃至8~10,标记为“溶液A”,作为背景溶液。Prepare a hydrazine solution with a certain concentration (200-1000 μg/L), adjust the pH of the solution from 25°C to 8-10 with 10% ammonia water, and mark it as "solution A" as the background solution.

配置一定浓度(ppb~ppm级别)的分散剂溶液,用氨水或乙醇胺调溶液pH25℃至8~10,标记为“溶液B”,作为分散剂试验溶液。Prepare a dispersant solution with a certain concentration (ppb-ppm level), adjust the pH of the solution from 25°C to 8-10 with ammonia water or ethanolamine, and mark it as "solution B" as the dispersant test solution.

准确称取定量纳米级或微米级铁氧化物(如Fe3O4等,也可以是Fe2O3、CuO、MgO、Al2O3、CaCO3、SiO2等颗粒,之所以优先选择Fe3O4,是因为核电站SG排污泥渣的90%以上是Fe3O4)颗粒,转移至锥形瓶中,摇均,搅拌超声2h,标记为“溶液C”。分散剂与颗粒质量比控制在100:1~1:100范围内。Accurately weigh and quantify nanoscale or micronscale iron oxides (such as Fe 3 O 4 , etc., or Fe 2 O 3 , CuO, MgO, Al 2 O 3 , CaCO 3 , SiO 2 , etc., the reason why Fe is preferred 3 O 4 , because more than 90% of the nuclear power plant SG sludge is Fe 3 O 4 ) particles, transferred to a Erlenmeyer flask, shaken evenly, stirred and ultrasonicated for 2 hours, and marked as "solution C". The mass ratio of dispersant to particles is controlled within the range of 100:1 to 1:100.

步骤2:试验装置的调试及运行Step 2: Commissioning and operation of the test device

本试验方法用到一种附带在线搅拌、补给和取样功能的高压釜装置,装置示意图如图1所示。This test method uses an autoclave device with on-line stirring, replenishment and sampling functions. The schematic diagram of the device is shown in Figure 1.

借助上述高压釜进行高温分散性能评价的试验,详细步骤如下:With the help of the above-mentioned autoclave, the test of high-temperature dispersion performance evaluation is carried out, and the detailed steps are as follows:

步骤21:依次将“溶液A”和定量“溶液C”倒入清洗干净的高压釜内,搅拌混匀,此时釜内氧化物颗粒相应元素浓度值记录为C。将定量“溶液A”(上述配置好的背景溶液)倒入在线补给装置的水箱18中,用于装置运行期间高压釜内液体的补给。Step 21: Pour "Solution A" and quantitative "Solution C" into the cleaned autoclave in turn, stir and mix well, and record the corresponding element concentration value of the oxide particles in the autoclave as C. Pour the quantitative "solution A" (the above-mentioned prepared background solution) into the water tank 18 of the online replenishment device for the replenishment of the liquid in the autoclave during the operation of the device.

步骤22:按照高压釜常规操作规程拧紧釜盖,将进/出导气管、搅拌、在线补给、在线取样装置连接组装完毕。Step 22: Tighten the lid of the autoclave according to the normal operating procedures of the autoclave, and connect and assemble the inlet/outlet air duct, stirring, online supply, and online sampling devices.

步骤23:关闭液体取样/补给阀门,打开进/出气阀,在进气阀处连接氮气储存装置,向釜内通入N2以除去釜内空气和液体中溶解氧,除氧完毕后依次关闭N2气瓶、出气阀、进气阀。Step 23: Close the liquid sampling/supply valve, open the air inlet/outlet valve, connect the nitrogen gas storage device at the inlet valve, and feed N2 into the kettle to remove the air in the kettle and the dissolved oxygen in the liquid, and close them in turn after deoxygenation is completed N 2 gas cylinder, outlet valve, inlet valve.

步骤24:打开搅拌装置,设置较低的搅拌速率(20~100r/min),对釜内液体进行低速搅拌。Step 24: Turn on the stirring device, set a low stirring rate (20-100r/min), and stir the liquid in the kettle at a low speed.

步骤25:按照高压釜温度设定程序设置升温速率和运行温度,待釜内液体升温至设定温度(如200~300℃,优选280℃温度是核电站正常功率运行时SG二次侧温度,是分散剂应用环境温度)且温度/压力(如280℃/6.8MPa,对应的是核电机组满功率运行状态时SG二次侧蒸汽温度及压力)稳定后,每隔一定时间在线取样一次(取样量在10~30mL,为了避免取样过程对釜内压力波动的影响,尽量控制较小的取样量),每次将取出来的样品转入干净的取样瓶中,分别标记为样品Z0-1、Z0-2、Z0-3…Z0-n,储存待测。每次取样后观察显示器上温度/压力值的变化,若温度偏离超过1℃或压力偏离超过0.2MPa时,及时补充因取样而损失的釜内液体量。以上步骤21~步骤25即为第一阶段(空白组)试验。Step 25: Set the heating rate and operating temperature according to the autoclave temperature setting program, and wait until the liquid in the autoclave is heated up to the set temperature (such as 200-300°C, preferably 280°C). After the dispersant application ambient temperature) and temperature/pressure (such as 280°C/6.8MPa, corresponding to the temperature and pressure of the SG secondary side steam when the nuclear power unit is in full power operation) are stable, take online samples at regular intervals (sample volume In the range of 10-30mL, in order to avoid the influence of the sampling process on the pressure fluctuation in the kettle, try to control the smaller sampling volume), transfer the taken samples into clean sampling bottles each time, and mark them as samples Z 0-1 , Z 0-2 , Z 0-3 ... Z 0-n , stored for testing. Observe the change of the temperature/pressure value on the display after each sampling. If the temperature deviates by more than 1°C or the pressure deviates by more than 0.2MPa, timely replenish the amount of liquid in the kettle lost due to sampling. The above steps 21 to 25 are the first stage (blank group) test.

步骤26:将在线补给水箱中液体更换为“溶液B”。利用在线补给泵(图1中15)向釜内补给定量“溶液B”(高浓度的分散剂溶液),使釜内分散剂与颗粒的质量比控制在100:1~1:100范围内,待温度/压力稳定后,每隔一定时间在线取样一次(取样量在10~30mL,为了避免取样过程对釜内压力波动的影响,尽量控制较小的取样量),每次将取出来的样品转入干净的取样瓶中,分别标记为样品Zt-1、Zt-2、Zt-3…Zt-n,储存待测。每次取样后观察显示器上温度/压力值的变化,若温度偏离超过2℃或压力偏离超过0.2MPa时,及时补充因取样而损失的釜内液体量。注:若分散剂在高温条件下会发生热分解而失效,在实验时每隔一定时间测试取样液体中分散剂的浓度,若浓度偏离理论值过多,需通过在线补给装置向釜内补充损失的分散剂量。步骤26即为第二阶段(测试组)试验。Step 26: Replace the liquid in the online make-up water tank with "Solution B". Use the online replenishment pump (15 in Figure 1) to supply a certain amount of "solution B" (a high-concentration dispersant solution) to the kettle, so that the mass ratio of the dispersant to the particles in the kettle is controlled within the range of 100:1 to 1:100, After the temperature/pressure is stabilized, take a sample online at regular intervals (the sampling volume is 10-30mL, in order to avoid the influence of the sampling process on the pressure fluctuation in the kettle, try to control the small sampling volume), each time the sample taken out Transfer them into clean sampling bottles, mark them as samples Z t-1 , Z t-2 , Z t-3 ... Z tn , and store them for testing. Observe the change of the temperature/pressure value on the display after each sampling. If the temperature deviates by more than 2°C or the pressure deviates by more than 0.2MPa, timely replenish the amount of liquid in the kettle lost due to sampling. Note: If the dispersant will be thermally decomposed under high temperature conditions and become invalid, test the concentration of the dispersant in the sampled liquid at regular intervals during the experiment. If the concentration deviates too much from the theoretical value, it is necessary to replenish the loss in the kettle through the online supply device dispersant dose. Step 26 is the second stage (test group) experiment.

步骤27:试验结束,待釜内液体自然冷却至室温后,依次打开排气阀和釜盖,排尽釜内液体,将高压釜清洗干净,备用。Step 27: After the test is over, after the liquid in the autoclave is naturally cooled to room temperature, open the exhaust valve and the lid of the autoclave in turn, drain the liquid in the autoclave, clean the autoclave, and set it aside.

步骤3:取样样品的测试及分析Step 3: Test and analysis of sample

将取样样品酸化,使颗粒完全溶解,然后可采用电感耦合等离子体原子发射光谱仪(ICP-AES)测定相关元素含量。样品Z0-1、Z0-2、Z0-3…Z0-n的测试结果分别记录为C0-1、C0-2、C0-3…C0-n,样品Zt-1、Zt-2、Zt-3…Zt-n的测试结果分别记录为Ct-1、Ct-2、Ct-3…Ct-nThe sample is acidified to completely dissolve the particles, and then the content of related elements can be measured by inductively coupled plasma atomic emission spectrometer (ICP-AES). The test results of samples Z 0-1 , Z 0-2 , Z 0-3 …Z 0-n are respectively recorded as C 0-1 , C 0-2 , C 0-3 …C 0-n , sample Z t- 1 , Z t-2 , Z t-3 ... Z tn test results are recorded as C t-1 , C t-2 , C t-3 ... C tn respectively.

第一阶段试验过程中,空白组颗粒的悬浮率η0计算公式为:During the first phase of the test, the suspension rate η of the blank group particles The calculation formula is:

Figure BDA0003887953060000081
Figure BDA0003887953060000081

第二阶段试验过程中,测试组颗粒的悬浮率ηt计算公式为:During the second stage of the test, the calculation formula of the suspension rate η t of the test group particles is:

Figure BDA0003887953060000082
Figure BDA0003887953060000082

分散剂的分散效率η计算公式为:The formula for calculating the dispersion efficiency η of the dispersant is:

η=ηt0 η=η t0

本评价方法中,η0代表上述试验工况条件下未添加分散剂时因搅拌等背景因素导致的釜内溶液中颗粒的悬浮率,ηt代表上述试验工况条件下添加分散剂后釜内溶液中颗粒的悬浮率,两者差值η代表上述试验工况条件下因分散剂作用导致的釜内溶液中颗粒的悬浮率。In this evaluation method, η 0 represents the suspension rate of particles in the solution in the kettle caused by background factors such as stirring when no dispersant is added under the above-mentioned test working conditions, and η represents the suspension rate in the kettle after adding the dispersant under the above-mentioned test working conditions. The suspension rate of the particles in the solution, the difference η between the two represents the suspension rate of the particles in the solution in the kettle caused by the action of the dispersant under the above test conditions.

为了更好理解本发明内容,特别说明如下:In order to better understand the content of the present invention, it is specially explained as follows:

①本发明不仅仅局限于280℃高温,可用于20~300℃范围任一温度条件下,相应高压釜内压力的要求为釜内温度对应的饱和蒸汽压力以上。① The present invention is not limited to the high temperature of 280°C, but can be used at any temperature in the range of 20-300°C, and the corresponding pressure requirement in the autoclave is above the saturated steam pressure corresponding to the temperature in the autoclave.

②本发明所用分散剂不仅仅局限于目前核电领域的丙烯酸聚合物,也可以是甲基丙烯酸聚合物、丙烯酸酯聚合物、甲基丙烯酸酯聚合物及其共聚物、三元共聚物,或者丙烯酸酯/丙烯酰胺共聚物、丙烯酸酯/甲基丙烯酸酯共聚物、三元共聚物及其混合物。2. The dispersant used in the present invention is not only limited to the acrylic acid polymers in the field of nuclear power, but also methacrylic acid polymers, acrylate polymers, methacrylate polymers and their copolymers, terpolymers, or acrylic acid polymers Esters/acrylamide copolymers, acrylate/methacrylate copolymers, terpolymers and mixtures thereof.

③本发明所用颗粒物不仅仅局限于Fe3O4颗粒,也可以是Fe2O3、CuO、MgO、Al2O3、CaCO3、SiO2等颗粒,或者是核电站SG真实泥渣,或者是核电领域任一管道位置处的泥渣,也可以是以上颗粒或泥渣的混合。颗粒或泥渣的D50尺寸在纳米级或微米级均可。③ The particles used in the present invention are not limited to Fe 3 O 4 particles, but can also be particles such as Fe 2 O 3 , CuO, MgO, Al 2 O 3 , CaCO 3 , SiO 2 , or the real sludge of nuclear power plant SG, or The sludge at any pipeline position in the field of nuclear power can also be a mixture of the above particles or sludge. The D50 size of the particles or sludge can be in the nanoscale or microscale.

④本发明所用背景溶液可以是高纯水,也可以是核电站二回路水化学系统溶液(其中包含氨水、乙醇胺、联氨等物质),也可以包含其他常规阴阳离子(钾、钠、钙、镁、氯、硫酸根、硝酸根、磷酸根等),不做要求。4. the used background solution of the present invention can be high-purity water, also can be nuclear power plant secondary circuit water chemical system solution (wherein comprise substances such as ammoniacal liquor, ethanolamine, hydrazine), also can comprise other conventional anions and cations (potassium, sodium, calcium, magnesium, chlorine , sulfate, nitrate, phosphate, etc.), no requirement.

Claims (7)

1. A high-temperature dispersibility evaluation device for a dispersant for a nuclear power plant is characterized in that: the device comprises a kettle body, wherein the kettle body comprises a heating furnace, the upper part of the heating furnace is covered with a kettle cover, the kettle cover is respectively connected with an in-kettle gas outlet pipe, an in-kettle sampling pipe, an in-kettle sample inlet pipe, a temperature measuring sleeve pipe and an in-kettle gas inlet pipe, a pressure gauge, an explosion type safety valve and a pressure transmitter are connected with the kettle cover through pipelines, the middle of the kettle cover is connected with a stirrer, the in-kettle sample inlet pipe is connected with a needle valve through a pipeline, the needle valve is connected with a metering pump through a pipeline, and the metering pump is connected with a spring type safety valve through a pipeline; the pressure gauge on the sample inlet pipeline is connected with the water tank through a pipeline; the sampling pipe in the kettle is connected with one end of the cooler and a ball valve through pipelines, the ball valve is arranged between the sampling pipe in the kettle and the cooler, and the other end of the cooler is connected with the ball valve; the temperature measuring sleeve is connected with the control cabinet, and the control cabinet is connected with the pressure transmitter and the stirrer.
2. The apparatus for evaluating high-temperature dispersibility of a dispersant for a nuclear power plant according to claim 1, wherein: the temperature measuring sleeve, the sampling tube in the kettle and the air inlet tube in the kettle are inserted into the lower part of the heating furnace, and the sampling tube in the kettle and the air outlet tube in the kettle are inserted into the upper part of the heating furnace.
3. The apparatus for evaluating the high-temperature dispersibility of a dispersant for a nuclear power plant according to claim 1, wherein: the rotating shaft and the stirring paddle of the stirrer extend into the bottom of the heating furnace.
4. A method for evaluating high-temperature dispersibility of a dispersant for a nuclear power plant, comprising the steps of:
step 1: solution preparation and material preparation;
step 2: debugging and running the test device;
and 3, step 3: testing and analyzing the sampled sample.
5. The method for evaluating the high-temperature dispersibility of the dispersant for the nuclear power plant as claimed in claim 4, wherein: the step 1 comprises preparing hydrazine solution with concentration of 200-1000 mug/L, and adjusting pH of the solution with 10% ammonia water 25℃ When the concentration is 8-10, marking as 'solution A', and taking the solution A as a background solution;
preparing a dispersant solution with ppb-ppm level concentration, and adjusting the pH value of the solution by using ammonia water or ethanolamine 25℃ When the concentration is 8-10, marking as 'solution B', and using the solution as a dispersant test solution;
preparing nano-scale or micron-scale iron oxide solution, and marking as 'solution C'.
6. The method for evaluating the high-temperature dispersing ability of a dispersant for nuclear power plants as defined in claim 4, wherein said step 2 comprises the steps of:
step 21: and sequentially pouring the solution A and a certain amount of the solution C into a cleaned high-pressure kettle, and stirring and uniformly mixing, wherein the concentration value of the corresponding element of the oxide particles in the kettle is recorded as C. Pouring a certain amount of the solution A into a water tank of an online replenishing device, and replenishing liquid in the high-pressure kettle during the operation of the device;
step 22: and screwing down the kettle cover according to the operating specification of the high-pressure kettle, and connecting and assembling the inlet/outlet gas guide pipe, the stirring device, the online supply device and the online sampling device.
Step 23: closing the liquid sampling/replenishing valve, opening the gas inlet/outlet valve atThe air inlet valve is connected with a nitrogen storage device, and N is introduced into the kettle 2 To remove dissolved oxygen in air and liquid in the kettle, and sequentially closing N after the oxygen removal is finished 2 The gas cylinder, the gas outlet valve and the gas inlet valve;
and step 24: and opening the stirring device, setting a lower stirring speed (20-100 r/min) and stirring the liquid in the kettle at a low speed.
Step 25: setting the heating rate and the operating temperature according to the temperature setting program of the autoclave, sampling on line once every certain time after the liquid in the autoclave is heated to the set temperature and the temperature/pressure is stable, transferring the taken sample into a clean sampling bottle every time, and respectively marking the sample as a sample Z 0-1 、Z 0-2 、Z 0-3 …Z 0-n And storing the test sample. Observing the change of the temperature/pressure value on the display after sampling every time, and replenishing the liquid amount in the kettle lost due to sampling in time if the temperature deviation exceeds 1 ℃ or the pressure deviation exceeds 0.2 MPa; the above steps 21 to 25 are the first stage tests;
step 26: replacing liquid in an online replenishing water tank with 'solution B', replenishing quantitative 'solution B' into a kettle by using an online replenishing pump, controlling the mass ratio of dispersing agent to particles in the kettle to be 100 t-1 、Z t-2 、Z t-3 …Z t-n And storing the test sample. Observing the change of the temperature/pressure value on the display after sampling each time, and supplementing the liquid amount in the kettle lost due to sampling in time if the temperature deviation exceeds 2 ℃ or the pressure deviation exceeds 0.2 MPa; namely the second stage test;
step 27: after the test is finished, after the liquid in the autoclave is naturally cooled to room temperature, opening the exhaust valve and the autoclave cover in sequence, draining the liquid in the autoclave, and cleaning the autoclave for later use.
7. The method for evaluating the high-temperature dispersing ability of a dispersant for a nuclear power plant as set forth in claim 4, wherein said step 3 comprises the steps of:
sampling the sampleAcidifying to dissolve the particles completely, and measuring the content of related elements by inductively coupled plasma atomic emission spectrometer, sample Z 0-1 、Z 0-2 、Z 0-3 …Z 0-n The test results of (A) are respectively recorded as C 0-1 、C 0-2 、C 0-3 …C 0-n Sample Z t-1 、Z t-2 、Z t-3 …Z t-n The test results of (A) are respectively recorded as C t-1 、C t-2 、C t-3 …C t-n
Suspension ratio eta of blank particles during the first stage of the test 0 The calculation formula is as follows:
Figure FDA0003887953050000031
in the second stage of the test, the suspension rate eta of the group particles is tested t The calculation formula is as follows:
Figure FDA0003887953050000032
the dispersion efficiency η of the dispersant is calculated by the formula:
η=η t0
wherein eta is 0 Representing the suspension rate, eta, of particles in the solution in the kettle caused by background factors such as stirring and the like when no dispersant is added under the test working condition t Representing the suspension rate of particles in the solution in the kettle after the dispersant is added under the test working condition, and the difference eta between the two represents the suspension rate of the particles in the solution in the kettle caused by the action of the dispersant under the test working condition.
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