CN108827820A - The detection method of suspension content in a kind of electrolyte - Google Patents
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- CN108827820A CN108827820A CN201810722817.8A CN201810722817A CN108827820A CN 108827820 A CN108827820 A CN 108827820A CN 201810722817 A CN201810722817 A CN 201810722817A CN 108827820 A CN108827820 A CN 108827820A
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- 239000003792 electrolyte Substances 0.000 title claims abstract description 59
- 238000001514 detection method Methods 0.000 title claims abstract description 29
- 239000000725 suspension Substances 0.000 title claims 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000012153 distilled water Substances 0.000 claims abstract description 12
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims description 27
- 238000003860 storage Methods 0.000 claims description 20
- 238000004140 cleaning Methods 0.000 claims 1
- 238000005303 weighing Methods 0.000 claims 1
- 239000007787 solid Substances 0.000 abstract description 25
- 238000001914 filtration Methods 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 6
- 239000010949 copper Substances 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000012535 impurity Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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Abstract
一种电解液中悬浮物含量的检测方法,包括以下步骤:(1)将滤纸放入恒温箱中恒温,记录恒温后的滤纸的重量m1;(2)从电解系统中取10L电解液,将滤纸置于检测装置中,将电解液倒入检测装置的漏斗中进行过滤;(3)用蒸馏水清洗过滤后的滤纸,直至洗出液的pH=7.0为止;(4)将清洗后的滤纸再次置于60±1℃的恒温箱中保温50‑70min,并将恒温后的滤纸称重,记录滤纸的重量m2;(5)计算电解液中悬浮物的含量,悬浮物的重量为m=m2‑ m1,电解液中悬浮物的含量为m/10=0.1m;本发明简便易行,流程简单,自动化程度高,同时可以精确检测电解液中悬浮物的含量,具有良好的应用和推广前景。
A method for detecting the content of suspended solids in an electrolyte, comprising the following steps: (1) Put filter paper in a constant temperature box to maintain a constant temperature, and record the weight m 1 of the filter paper after constant temperature; (2) Take 10L of electrolyte from an electrolysis system, Put the filter paper in the detection device, pour the electrolyte into the funnel of the detection device for filtration; (3) wash the filtered filter paper with distilled water until the pH of the eluate = 7.0; (4) put the washed filter paper Place it again in a constant temperature box at 60±1°C for 50-70 minutes, weigh the filter paper after constant temperature, and record the weight of the filter paper in m2 ; (5) Calculate the content of suspended solids in the electrolyte, and the weight of the suspended solids is m =m 2 ‑ m 1 , the content of suspended solids in the electrolyte is m/10=0.1m; the present invention is simple and easy to implement, has a simple process and a high degree of automation, and can accurately detect the content of suspended solids in the electrolyte, and has good Application and promotion prospects.
Description
技术领域technical field
本发明涉及化工检测技术领域,具体是一种电解液中悬浮物含量的检测方法。The invention relates to the technical field of chemical detection, in particular to a detection method for the content of suspended matter in an electrolyte.
背景技术Background technique
在铜电解精炼中,是将粗铜作为阳极,不锈钢板或者铜始极片作为阴极,置于电解液的电解槽里进行通电生产。随着电解的进行,阳极溶解,铜从阴极中析出。阳极中铜大部分析出到阴极,阳极的部分杂质沉到电解槽底部,少量杂质溶解到电解液中。溶解到电解液中的杂质相互结合,形成漂浮物颗粒。由于电解液中悬浮物过多会严重影响阴极铜的质量,在生产过程中需要及时监控电解液中悬浮物的变化趋势,以便对生产工艺进行调整。电解液的成分为Cu2+ 40~55g/L ,H2SO4 160~210g/L ,Cl- 0.01~0.09g/L,As 3~15g/L,Sb0.2~1.5g/L,Bi 0.1~0.5g/L,Ni 8~15g/L。由于电解液成分复杂,其中悬浮物的含量一般为5-30mg/L,且有强烈的腐蚀性,无法用仪器直接接触,取少量的电解液直接过滤也不易精确检测。In copper electrolytic refining, the blister copper is used as the anode, and the stainless steel plate or the copper starting plate is used as the cathode, which is placed in the electrolytic cell of the electrolyte for energized production. As electrolysis proceeds, the anode dissolves and copper is precipitated from the cathode. Most of the copper in the anode is precipitated to the cathode, part of the impurities in the anode sink to the bottom of the electrolytic cell, and a small amount of impurities dissolve into the electrolyte. Impurities dissolved into the electrolyte combine with each other to form floating particles. Since too much suspended matter in the electrolyte will seriously affect the quality of cathode copper, it is necessary to monitor the change trend of the suspended matter in the electrolyte in time during the production process in order to adjust the production process. The composition of the electrolyte is Cu 2+ 40~55g/L, H 2 SO 4 160~210g/L, Cl - 0.01~0.09g/L, As 3~15g/L, Sb0.2~1.5g/L, Bi 0.1~0.5g/L, Ni 8~15g/L. Due to the complex composition of the electrolyte, the content of suspended solids is generally 5-30mg/L, and it is highly corrosive, so it cannot be directly contacted with an instrument, and it is not easy to accurately detect a small amount of electrolyte and directly filter it.
基于目前电解液腐蚀性强,无法用仪器自动检测悬浮物,同时悬浮物含量较低、分布不均匀,少量电解液过滤也无法精确检测。因此,研发一种电解液中悬浮物含量的检测方法具有十分重要的意义。Due to the strong corrosiveness of the current electrolyte, it is impossible to automatically detect suspended solids with an instrument. At the same time, the content of suspended solids is low and the distribution is uneven, and a small amount of electrolyte filtration cannot be accurately detected. Therefore, it is of great significance to develop a detection method for the content of suspended solids in the electrolyte.
发明内容Contents of the invention
本发明的目的就是针对电解液的腐蚀性强,无法用仪器自动检测悬浮物,同时悬浮物的含量低、分布不均匀,少量电解液无法精确检测等问题,提供一种操作简便、成本低廉的电解液中悬浮物含量的检测方法。The purpose of the present invention is to solve the problems that the electrolyte is highly corrosive, the suspended matter cannot be automatically detected by the instrument, and the content of the suspended matter is low, the distribution is uneven, and a small amount of electrolyte cannot be accurately detected. The detection method of the content of suspended matter in the electrolyte.
本发明的一种电解液中悬浮物含量的检测方法,包括以下步骤:A method for detecting suspended matter content in an electrolyte of the present invention comprises the following steps:
(1)将滤纸放入温度为60±1℃的恒温箱中保温30min,并将恒温后的滤纸称重,记录滤纸的重量m1;(1) Put the filter paper into an incubator with a temperature of 60±1°C and keep it warm for 30 minutes, weigh the filter paper after constant temperature, and record the weight m 1 of the filter paper;
(2)从电解系统中取10L电解液,将称重后的滤纸置于检测装置中,将电解液倒入检测装置的漏斗中进行过滤;(2) Take 10L of electrolyte from the electrolysis system, place the weighed filter paper in the detection device, pour the electrolyte into the funnel of the detection device for filtration;
(3)用蒸馏水清洗过滤后的滤纸,直至洗出液的pH=7.0为止;(3) Wash the filtered filter paper with distilled water until the pH of the eluate = 7.0;
(4)将清洗后的滤纸再次置于60±1℃的恒温箱中保温50-70min,并将恒温后的滤纸称重,记录滤纸的重量m2;(4) Place the cleaned filter paper in a constant temperature box at 60±1°C for 50-70 minutes, weigh the filter paper after constant temperature, and record the weight m2 of the filter paper;
(5)计算电解液中悬浮物的含量,悬浮物的重量为m = m2- m1,电解液中悬浮物的含量为m/10= 0.1m。(5) Calculate the content of suspended solids in the electrolyte. The weight of suspended solids is m = m 2 - m 1 , and the content of suspended solids in the electrolyte is m/10= 0.1m.
本发明中所述检测装置具有pH计、PLC控制器和储液槽,所述储液槽的顶部设有液位检测器,底部设有储液槽出口,储液槽出口装有电磁阀,储液槽出口的正下方设有漏斗,所述漏斗的出口设有真空泵,漏斗上还设有蒸馏水进水管,所述pH计、真空泵和液位检测器均通过电缆与PLC控制器连接。The detection device described in the present invention has a pH meter, a PLC controller and a liquid storage tank, the top of the liquid storage tank is provided with a liquid level detector, the bottom is provided with a liquid storage tank outlet, and the outlet of the liquid storage tank is equipped with a solenoid valve. A funnel is arranged directly below the outlet of the liquid storage tank, a vacuum pump is arranged at the outlet of the funnel, and a distilled water inlet pipe is arranged on the funnel, and the pH meter, the vacuum pump and the liquid level detector are all connected to the PLC controller through cables.
优选地,本发明中所述储液槽的体积≥10L。Preferably, the volume of the liquid storage tank in the present invention is ≥10L.
本发明的工作原理是:先从电解系统中取10L电解液倒入储液槽中,并将恒温后的滤纸置于漏斗中,打开储液槽出口的电磁阀,同时打开PLC控制器的开关,真空泵开始工作,电解液从储液槽流入漏斗中进行过滤,滤液从漏斗中流出,悬浮物留在滤纸上,过滤完成之后,打开蒸馏水进水管,用蒸馏水冲洗滤纸,用pH计测量洗出液的pH值,待洗出液的pH=7,停止清洗,将滤纸取出并置于恒温箱中进行恒温,恒温后称重。滤纸过滤前和过滤后的质量差即为悬浮物的重量,计算即可得到电解液中悬浮物的浓度。The working principle of the present invention is: first take 10L electrolyte from the electrolysis system and pour it into the liquid storage tank, put the filter paper after constant temperature in the funnel, open the electromagnetic valve at the outlet of the liquid storage tank, and open the switch of the PLC controller at the same time , the vacuum pump starts to work, the electrolyte flows from the storage tank into the funnel for filtration, the filtrate flows out from the funnel, and the suspended matter remains on the filter paper. After the filtration is completed, open the distilled water inlet pipe, rinse the filter paper with distilled water, and measure the washed out with a pH meter. When the pH of the eluate is 7, stop washing, take out the filter paper and place it in an incubator for constant temperature, and weigh after constant temperature. The mass difference between the filter paper before and after filtration is the weight of the suspended matter, and the concentration of the suspended matter in the electrolyte can be obtained by calculation.
本发明中的PLC控制器可以采集储液槽中液位检测器检测的液位信息、pH计的测量信息,同时PLC控制器输出开关量指令信号,控制真空泵和电磁阀的启停,通过液位检测器给出储液槽出口电解液的流速,通过电磁阀调节信号,控制漏斗中的电解液维持速度稳定,使电解液不溢流。The PLC controller in the present invention can collect the liquid level information detected by the liquid level detector in the liquid storage tank and the measurement information of the pH meter. The position detector gives the flow rate of the electrolyte at the outlet of the storage tank, and the electromagnetic valve adjusts the signal to control the electrolyte in the funnel to maintain a stable speed so that the electrolyte does not overflow.
本发明的检测方法简便易行,流程简单,自动化程度高,同时可以精确检测电解液中悬浮物的含量,具有良好的应用和推广前景。The detection method of the present invention is simple and easy to operate, has a simple process and a high degree of automation, and at the same time can accurately detect the content of suspended solids in the electrolyte, and has good application and popularization prospects.
附图说明Description of drawings
图1是本发明中的检测装置结构示意图;Fig. 1 is a schematic structural view of a detection device in the present invention;
其中:1-pH计,2- PLC控制器,3-储液槽,4-液位检测器,5-储液槽出口,6-电磁阀,7-漏斗,8-真空泵,9-蒸馏水进水管,10-电缆,11-滤纸。Among them: 1-pH meter, 2-PLC controller, 3-liquid storage tank, 4-liquid level detector, 5-liquid storage tank outlet, 6-solenoid valve, 7-funnel, 8-vacuum pump, 9-distilled water inlet Water pipe, 10-cable, 11-filter paper.
具体实施方式Detailed ways
实施例1Example 1
本实施例的一种电解液中悬浮物含量的检测方法,其中电解液的成分为Cu2+ 43.29g/L,H2SO4 186.3g/L,Cl- 0.07g/L,As 4.3g/L,Sb 1.26g/L,Bi 0.35g/L,Ni 13.5g/L,Pb0.02g/L,Fe 1.29g/L,包括以下步骤:A method for detecting suspended solids in the electrolyte of this embodiment, wherein the composition of the electrolyte is Cu 2+ 43.29g/L, H 2 SO 4 186.3g/L, Cl - 0.07g/L, As 4.3g/L L, Sb 1.26g/L, Bi 0.35g/L, Ni 13.5g/L, Pb0.02g/L, Fe 1.29g/L, including the following steps:
(1)将滤纸11放入温度为60±1℃的恒温箱中保温30min,并将恒温后的滤纸11称重,记录滤纸11的重量为m1 = 2147mg;(1) Put the filter paper 11 into an incubator with a temperature of 60±1°C and keep it warm for 30 minutes, weigh the filter paper 11 after constant temperature, and record the weight of the filter paper 11 as m 1 = 2147mg;
(2)从电解系统中取10L电解液,将称重后的滤纸11置于检测装置中,将电解液倒入检测装置的漏斗7中过滤;(2) Take 10L of electrolyte from the electrolysis system, place the weighed filter paper 11 in the detection device, pour the electrolyte into the funnel 7 of the detection device to filter;
(3)用蒸馏水清洗过滤后的滤纸11,直至洗出液的pH=7.0为止;(3) Wash the filtered filter paper 11 with distilled water until the pH of the eluate is 7.0;
(4)将清洗后的滤纸再次置于60±1℃的恒温箱中保温60min,并将恒温后的滤纸称重,记录滤纸的重量为m2=2262mg;(4) Place the cleaned filter paper in a constant temperature box at 60±1°C for 60 minutes, and weigh the filter paper after constant temperature, and record the weight of the filter paper as m 2 =2262mg;
(5)计算电解液中悬浮物的含量,悬浮物的重量为m=m2- m1= 2262-2147 =115mg,电解液中悬浮物的含量为m/10 = 0.1m=0.1×115=11.5(mg/L)。(5) Calculate the content of suspended solids in the electrolyte, the weight of suspended solids is m=m 2 - m 1 = 2262-2147 =115mg, the content of suspended solids in the electrolyte is m/10 = 0.1m=0.1×115= 11.5 (mg/L).
本实施例中所述检测装置参见图1,具有pH计1、PLC控制器2和储液槽3,所述储液槽3的顶部设有液位检测器4,底部设有储液槽出口5,储液槽出口5装有电磁阀6,储液槽出口5的正下方设有漏斗7,所述漏斗7的出口设有真空泵8,漏斗7上还设有蒸馏水进水管9,所述pH计1、真空泵8和液位检测器4均通过电缆10与PLC控制器2连接。Referring to Fig. 1, the detection device described in this embodiment has a pH meter 1, a PLC controller 2 and a liquid storage tank 3, the top of the liquid storage tank 3 is provided with a liquid level detector 4, and the bottom is provided with a liquid storage tank outlet 5. The outlet 5 of the liquid storage tank is equipped with a solenoid valve 6, and a funnel 7 is provided directly below the outlet 5 of the liquid storage tank. The outlet of the funnel 7 is provided with a vacuum pump 8, and the funnel 7 is also provided with a distilled water inlet pipe 9. The pH meter 1 , the vacuum pump 8 and the liquid level detector 4 are all connected to the PLC controller 2 through the cable 10 .
优选地,本实施例中所述储液槽3的体积为15L。Preferably, the volume of the liquid storage tank 3 in this embodiment is 15L.
实施例2Example 2
本实施例的一种电解液中悬浮物含量的检测方法,其中电解液的成分为Cu2+ 52.13g/L,H2SO4 170.2g/L,Cl- 0.05g/L,As 6.3g/L,Sb 0.72g/L,Bi 0.24g/L,Ni 10.2g/L,Pb0.07g/L,Fe 2.35g/L,包括以下步骤:A detection method for the content of suspended solids in the electrolyte of this embodiment, wherein the composition of the electrolyte is Cu 2+ 52.13g/L, H 2 SO 4 170.2g/L, Cl - 0.05g/L, As 6.3g/L L, Sb 0.72g/L, Bi 0.24g/L, Ni 10.2g/L, Pb0.07g/L, Fe 2.35g/L, including the following steps:
(1)将滤纸11放入温度为60±1℃的恒温箱中保温30min,并将恒温后的滤纸11称重,记录滤纸11的重量为m1 = 2144mg;(1) Put the filter paper 11 into an incubator with a temperature of 60±1°C and keep it warm for 30 minutes, weigh the filter paper 11 after constant temperature, and record the weight of the filter paper 11 as m 1 = 2144mg;
(2)从电解系统中取10L电解液,将称重后的滤纸11置于检测装置中,将电解液倒入检测装置中的漏斗7过滤;(2) Take 10L of electrolyte from the electrolysis system, place the weighed filter paper 11 in the detection device, pour the electrolyte into the funnel 7 in the detection device to filter;
(3)用蒸馏水清洗过滤后的滤纸11,直至洗出液的pH=7.0为止;(3) Wash the filtered filter paper 11 with distilled water until the pH of the eluate is 7.0;
(4)将清洗后的滤纸11再次置于60±1℃的恒温箱中保温70min,并将恒温后的滤纸11称重,记录滤纸的重量为m2=2217mg;(4) Place the cleaned filter paper 11 again in an incubator at 60±1°C for 70 minutes, and weigh the filter paper 11 after constant temperature, and record the weight of the filter paper as m 2 =2217mg;
(5)计算电解液中悬浮物的含量,悬浮物的重量为m=m2- m1= 2217-2144 =73mg,电解液中悬浮物的含量为m/10 = 0.1m=0.1×73=7.3(mg/L)。(5) Calculate the content of suspended solids in the electrolyte, the weight of suspended solids is m=m 2 - m 1 = 2217-2144 =73mg, the content of suspended solids in the electrolyte is m/10 = 0.1m=0.1×73= 7.3 (mg/L).
本实施例中所述的检测装置同实施例1。The detection device described in this embodiment is the same as that in Embodiment 1.
实施例3Example 3
本实施例的一种电解液中悬浮物含量的检测方法,其中电解液的成分为Cu2+ 52.13g/L,H2SO4 170.2g/L,Cl- 0.05g/L,As 6.3g/L,Sb 0.72g/L,Bi 0.24g/L,Ni 10.2g/L,Pb0.07g/L,Fe 2.35g/L,包括以下步骤:A detection method for the content of suspended solids in the electrolyte of this embodiment, wherein the composition of the electrolyte is Cu 2+ 52.13g/L, H 2 SO 4 170.2g/L, Cl - 0.05g/L, As 6.3g/L L, Sb 0.72g/L, Bi 0.24g/L, Ni 10.2g/L, Pb0.07g/L, Fe 2.35g/L, including the following steps:
(1)将滤纸11放入温度为60±1℃的恒温箱中保温30min,并将恒温后的滤纸11称重,记录滤纸11的重量为m1 = 2142mg;(1) Put the filter paper 11 into an incubator with a temperature of 60±1°C and keep it warm for 30 minutes, weigh the filter paper 11 after constant temperature, and record the weight of the filter paper 11 as m 1 = 2142mg;
(2)从电解系统中取10L电解液,将称重后的滤纸11置于检测装置中,将电解液倒入检测装置中过滤;(2) Take 10L of electrolyte from the electrolysis system, place the weighed filter paper 11 in the detection device, pour the electrolyte into the detection device and filter;
(3)用蒸馏水清洗过滤后的滤纸11,直至洗出液的pH=7.0为止;(3) Wash the filtered filter paper 11 with distilled water until the pH of the eluate is 7.0;
(4)将清洗后的滤纸11再次置于60±1℃的恒温箱中保温50min,并将恒温后的滤纸11称重,记录滤纸的重量为m2=2323mg;(4) Place the cleaned filter paper 11 again in a constant temperature box at 60±1°C for 50 minutes, and weigh the filter paper 11 after constant temperature, and record the weight of the filter paper as m 2 =2323mg;
(5)计算电解液中悬浮物的含量,悬浮物的重量为m=m2- m1= 2323-2142 =181mg,电解液中悬浮物的含量为m/10 = 0.1m=0.1×181=18.1(mg/L)。(5) Calculate the content of suspended solids in the electrolyte, the weight of suspended solids is m=m 2 - m 1 = 2323-2142 =181mg, the content of suspended solids in the electrolyte is m/10 = 0.1m=0.1×181= 18.1 (mg/L).
本实施例中所述的检测装置同实施例1。The detection device described in this embodiment is the same as that in Embodiment 1.
Claims (3)
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