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CN104330451A - Manufacturing method of salt bridge used in low temperature environment - Google Patents

Manufacturing method of salt bridge used in low temperature environment Download PDF

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Publication number
CN104330451A
CN104330451A CN201410430574.2A CN201410430574A CN104330451A CN 104330451 A CN104330451 A CN 104330451A CN 201410430574 A CN201410430574 A CN 201410430574A CN 104330451 A CN104330451 A CN 104330451A
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China
Prior art keywords
salt bridge
low temperature
temperature environment
flexible pipe
making
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CN201410430574.2A
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Chinese (zh)
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CN104330451B (en
Inventor
马换玉
李春景
陈飞
方明学
杨惠强
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Tianneng Group Jiangsu Technology Co Ltd
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Tianneng Group Jiangsu Technology Co Ltd
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Abstract

The invention discloses a manufacturing method of a salt bridge used in low temperature environment. The mixture in the salt bridge is composed of the following components: a saturated potassium nitrate solution, soluble starch, and diluted sulfuric acid with a density of 1.2 to 1.35 g/cm3 according to a weight ratio of 5-11:4-10:1-5. The salt bridge is made of plastic soft pipe. The manufacture of the salt bridge is simple, the raw material consumption is little, the length of the salt bridge can be adjusted at will, and the soluble starch has good solubility. The salt bridge has the advantages of stable chemical property, strong absorbing force, good fluidity, and proper gelation speed, and can be used in low temperature environment with a temperature of -20 to 0 DEG C, and the test results are precise and stable. Moreover the shortages of conventional salt bridges are overcome.

Description

The salt bridge method for making that a kind of low temperature environment uses
Technical field
The present invention relates to salt bridge method for making field, be specifically related to the salt bridge method for making that a kind of low temperature environment uses.
Background technology
For the experimental cell of low temperature discharge capacity difference, positive plate problem or negative plate problem to analyze poor performance at low temperatures reason further, often measure both positive and negative polarity electrode potential by means of contrast electrode, judge the quality condition of battery positive/negative plate in charge and discharge process according to its relative value, improve the reason analyzing battery capacity and fault generation.The method of current single electrode potential test is by carrying out the rear external container of punching on battery shell wall, then in container, the electrolytic solution identical with inside battery is added, make it formation path, relend and help contrast electrode to test, but like this by punch method trouble, and punching affects the outward appearance of battery.Substitute punch method with salt bridge, salt bridge forms galvanic circle by the migration of ion, and between two kinds of solution, inserting salt bridge, original container is outer directly to be contacted with inside battery solution to replace, and the more important thing is and can be used for eliminating liquid junction potential.
The selection of salt bridge is in fact electrolytical selection in salt bridge, as long as the migration velocity approximately equal of water-soluble electrolytes anions and canons, and does not react with the electrolyte in battery and all can be elected to be the electrolyte of salt bridge.It is crucial that at low ambient temperatures, electrolyte can not freeze or crystallization, otherwise the salt bridge made can have a strong impact on ionic transfer speed under low temperature environment.By conventional salt bridge electrolyte as KCL, NH 4cL, NH 4nO 3, KNO 3deng being made into saturated solution under 25 DEG C of environment, and at one time in put into-18 DEG C of cryogenic boxes, 30min takes out and finds not freeze except KCL, and other are several freezes or crystallization.But agar-KCL salt bridge can not use again in the solution containing the high dense material such as acid, ammonia, because of the dense acid of height, ammonia all can with agar effect, destroy salt bridge, stain solution; And chlorion can produce self discharge, bad to battery performance.
The preparation of salt bridge tradition is generally at saturated KCL, NH 4cL, NH 4nO 3, KNO 3add agar in aqueous solution and make gel, injecting the cooling of U pipe can become salt bridge, and U-tube two ends prevent the siphon between electrolyte solution with husky core (or absorbent cotton) sealing of porous.Tradition method for making comes with some shortcomings: 1, U-tube size is single cannot meet experiment needs, and the salt bridge needed for single lattice defect test needs to intercept in advance, makes troubles for salt bridge makes.2, easily in U-tube, remain bubble when agar is filled while hot, affect experiment effect.3, agar easily solidifies, and the speed pouring U-tube into wants fast, inculcates inconvenience.4, there is the situation of not gel sometimes.5, inculcate while hot U-tube can be caused to break.6, fill with U-tube again as after slightly cooling, there will be also not filling with below, that fills with above in U-tube solidifies.7, according to ropy agar, easily produce in preparation process and be difficult to heating for dissolving because being mixed with insoluble impurity, make salt bridge prepare very complicated, waste time and energy, easily failure, wastes experimental period, also makes experimental result lack scientific and reliability.
Summary of the invention
The technical problem to be solved in the present invention is to provide the salt bridge method for making used in a kind of low temperature environment, salt bridge can use under 0 DEG C ~-20 DEG C low temperature environments, can not only Measurement accuracy battery positive/negative plate problem at low ambient temperatures, and overcome during traditional salt bridge makes the above-mentioned deficiency occurred.
The present invention is achieved through the following technical solutions:
The salt bridge method for making that low temperature environment uses, in described salt bridge tube, potpourri is formulated by the component of following weight ratio, saturated potassium nitrate solution: soluble starch: density 1.2 ~ 1.35g/cm 3dilute sulfuric acid be 5 ~ 11:4 ~ 10:1 ~ 5;
Comprise the following steps, by above-mentioned parts by weight of component,
One, measure dilute sulfuric acid slowly to pour in the beaker that saturated potassium nitrate solution is housed and stir, then measure soluble starch and pour in beaker and stir, in muddy supernatant liquid;
Two, above-mentioned beaker is placed on the muffle furnace that design temperature is 150 DEG C of preheatings, then stirs 1-2min, muddy supernatant liquid is heated the ecru pasty mixture that is translucent, stop heating;
Three, get one section of flexible pipe one end to be connected with syringe, the other end submerges and is translucent in ecru pasty mixture, with syringe, whole piece flexible pipe is filled while hot when mixture temperature is not less than 50 DEG C, be cooled to room temperature, intercepted length as required, flexible pipe two ends plug is blocked, makes salt bridge.
The further improvement project of the present invention is, is poured into by the potpourri heated in the little graduated cylinder of preprepared 25ml in step 2 from beaker.Reduce contact floorage, increase height, plastic flexible pipe can be made to put into so more stable, effectively avoid bubble.
The present invention further improvement project is, electrolytical consistent in density in the density of described dilute sulfuric acid and battery.Both density is consistent, ensures ionic transfer speed.
The present invention further improvement project is, described flexible pipe uses front distilled water to carry out injection cleaning.Mix foreign ion in prevention pipe, cause measuring error.
The present invention further improvement project is, described plug is AGM separator paper or filter paper.
The present invention has following obvious advantage:
One, KCL does not freeze at low temperatures, but agar-KCL salt bridge can not use in the solution containing the high dense material such as acid, ammonia, because of the dense acid of height, ammonia all can with agar effect, destroy salt bridge, stain solution; Chlorion can produce self power generation simultaneously, bad to battery performance.The present invention selects saturated potassium nitrate, soluble starch to make, and adds micro-dilute sulfuric acid and prevent saturated potassium nitrate solution to freeze at low ambient temperatures in manufacturing process; Soluble starch dissolubility is good, stable chemical nature, and absorption affinity is strong, good fluidity and also gelation rate moderate.
Two, U-tube size is single cannot meet experiment needs, and the salt bridge needed for single lattice defect test needs to intercept in advance, makes troubles for salt bridge makes.The present invention adopts plastic flexible pipe as making, intercepts specification as required.
Three, the present invention's syringe is filled electrolyte in salt bridge by whole piece flexible pipe while hot, avoids in pipe and produces bubble, and inculcates conveniently, and can not break flexible pipe, fillingly before and after infusion procedure also there will not be solidifies inconsistent phenomenon, intercept after cooling make simple.
Accompanying drawing explanation
Fig. 1 is that the present invention detects positive/negative plate connection layout.
Wherein: 1, charging set 11, positive and negative power supply line 12, dividing potential drop 1, dividing potential drop 2 14, dividing potential drop 32, battery 3, electrolytic solution (density is with inside battery electrolytic solution) 4, salt bridge 5, cadmium electrode.
Fig. 2 is embodiment one-18 DEG C of low temperature discharge both positive and negative polarity electrode potential.
Fig. 3 is embodiment 20 DEG C ~ 18 DEG C low temperature discharge both positive and negative polarity electrode potentials.
Embodiment
1, preliminary work
1.1, prepare to grow up the plastic flexible pipe 1-2 section being about half meter, described plastic flexible pipe has acid resistance, syringe 1; First fill distilled water with syringe before using, then carry out injection cleaning 3-5 time facing to plastic flexible pipe, mix foreign ion in prevention pipe, introduce measuring error.
1.2, prepare each 1 of large small beaker 30mL, 250mL, 1, the little graduated cylinder of 25mL, and clean with distilled water, back-off dries for subsequent use.
1.3, muffle furnace is connected power source and carry out first preheating, temperature is set in about 150 DEG C.
Embodiment one:
The salt bridge used under described low temperature environment, its parts by weight of raw materials component proportioning is, saturated potassium nitrate solution: soluble starch: density is 1.34g/cm 3dilute sulfuric acid be 8:7:4.
One, 8 grams of saturated KNO are first measured 3solution is put in the small beaker of 30mL, and measuring density is 1.34g/cm 3dilute sulfuric acid 4 grams slowly pour into saturated KNO be housed 3in the small beaker of solution, stir with glass bar.Measure 7 grams of soluble starches again, pour into and saturated KNO is housed 3in the small beaker of solution, extremely even for second by glass bar stirred for several, present muddy supernatant liquid state.
Two, ensure that beaker bottom drying is put on the muffle furnace of prior preheating, then stir 1-2min with glass bar, muddy supernatant liquid shape starch is heated and presents translucent ecru pasty state, stop stirring, close muffle furnace power supply.
Three, put on proximity gloves, the pasty state of the translucent state heated is poured in the little graduated cylinder of cut-and-dried 25ml from beaker, reduce contact floorage, increase height, plastic flexible pipe can be made to put into so more stable, effectively avoid bubble.Be connected with syringe one end of flexible pipe, the other end submerges in the little graduated cylinder of starch fluid again, with syringe, whole piece flexible pipe is filled pasty state starch fluid while hot when starch fluid temperature is not less than 50 DEG C, exists in flexible pipe without air bubble.Be cooled to room temperature, pipe two ends AGM separator paper is blocked.
The salt bridge for preparing is intercepted the length of 100mm by demand, connect by Fig. 1 connected mode, and insert in low temperature-18 DEG C of environment and leave standstill 12 hours, be discharged to the mono-lattice of 1.75V/ by technique electric current 6A, then use 0.18C 2the mono-lattice constant current constant voltage of A pressure limiting 2.5V/ fills 12 hours.Both positive and negative polarity electrode potential measured by process, maps by contrasting with punch method in the past, as shown in Figure 2.
Embodiment one, the result of Fig. 2 test draws, the discharge curve that the salt bridge test result using the method to obtain and punch method in the past record is basically identical, and finds out that this battery is that the downtrending of negative pole current potential is very fast when discharging at low ambient temperatures, and explanation is negative pole problem.
Embodiment two:
The salt bridge used under described low temperature environment, its parts by weight of raw materials component proportioning is, saturated potassium nitrate solution: soluble starch: density is 1.34g/cm 3dilute sulfuric acid be 10:10:2.
Preparation process is as embodiment one.
The salt bridge for preparing is intercepted the length of 100mm by demand, connect by Fig. 1 connected mode, and insert in different environment 0 DEG C ~-18 DEG C and leave standstill 12 hours, be discharged to the mono-lattice of 1.75V/ by technique electric current 6A, then use 0.18C 2the mono-lattice constant current constant voltage of A pressure limiting 2.5V/ fills 12 hours.Both positive and negative polarity electrode potential measured by process, maps by contrasting with punch method in the past, as shown in Figure 3.
From embodiment two, the result of Fig. 3 test draws, the discharge curve that records of 0 DEG C ~-18 DEG C test results and punch method is in the past basically identical under various circumstances to use the salt bridge that obtains of the method, and find out that this battery is that the downtrending of negative pole current potential is very fast when discharging at low ambient temperatures, explanation is negative pole problem.
It is simple that practice shows that the method makes, and chemical consumption is few, and salt bridge length can arbitrarily control, soluble starch dissolubility is good, stable chemical nature, and absorption affinity is strong, good fluidity and gelation rate moderate, in the checking through different temperature, its test result comparatively accurately, stable.

Claims (5)

1. a salt bridge method for making for low temperature environment use, is characterized in that: in described salt bridge tube, potpourri is formulated by the component of following weight ratio, saturated potassium nitrate solution: soluble starch: density 1.2 ~ 1.35g/cm 3dilute sulfuric acid be 5 ~ 11:4 ~ 10:1 ~ 5;
Comprise the following steps, by above-mentioned weight ratio ingredient,
One, measure dilute sulfuric acid slowly to pour in the beaker that saturated potassium nitrate solution is housed and stir, then measure soluble starch and pour in beaker and stir, in muddy supernatant liquid;
Two, above-mentioned beaker is placed on the muffle furnace that design temperature is 150 DEG C of preheatings, then stirs 1-2min, muddy supernatant liquid is heated the ecru pasty mixture that is translucent, stop heating;
Three, get one section of flexible pipe one end to be connected with syringe, the other end submerges and is translucent in ecru pasty mixture, with syringe, whole piece flexible pipe is filled while hot when mixture temperature is not less than 50 DEG C, be cooled to room temperature, intercepted length as required, flexible pipe two ends plug is blocked, makes salt bridge.
2. the salt bridge method for making of a kind of low temperature environment use according to claim 1, is characterized in that: poured into from beaker by the potpourri heated in step 2 in the little graduated cylinder of preprepared 25ml.
3. the salt bridge method for making that uses of a kind of low temperature environment according to claim 1, is characterized in that: electrolytical consistent in density in the density of described dilute sulfuric acid and battery.
4. the salt bridge method for making of a kind of low temperature environment use according to claim 1, is characterized in that: described flexible pipe uses front distilled water to carry out injection cleaning.
5. the salt bridge method for making of a kind of low temperature environment use according to claim 1, is characterized in that: described plug is AGM separator paper or filter paper.
CN201410430574.2A 2014-08-28 2014-08-28 The salt bridge manufacture method that a kind of low temperature environment is used Expired - Fee Related CN104330451B (en)

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN106226705A (en) * 2016-08-29 2016-12-14 超威电源有限公司 A kind of lead-acid battery electrode potentiometric detection method
CN107807332A (en) * 2017-10-10 2018-03-16 超威电源有限公司 lead-acid battery electrode potential detection device and detection method
CN108226239A (en) * 2017-12-28 2018-06-29 南京钢铁股份有限公司 A kind of preparation method of filament type salt bridge
CN109830730A (en) * 2019-02-17 2019-05-31 熵零技术逻辑工程院集团股份有限公司 A kind of chemical energy device for converting electric energy

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106226705A (en) * 2016-08-29 2016-12-14 超威电源有限公司 A kind of lead-acid battery electrode potentiometric detection method
CN106226705B (en) * 2016-08-29 2019-09-20 超威电源有限公司 A kind of lead-acid battery electrode potentiometric detection method
CN107807332A (en) * 2017-10-10 2018-03-16 超威电源有限公司 lead-acid battery electrode potential detection device and detection method
CN108226239A (en) * 2017-12-28 2018-06-29 南京钢铁股份有限公司 A kind of preparation method of filament type salt bridge
CN109830730A (en) * 2019-02-17 2019-05-31 熵零技术逻辑工程院集团股份有限公司 A kind of chemical energy device for converting electric energy

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