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Synthesis method of electrolyte sample for sodium expansion rate test

A technology of sodium expansion rate and synthesis method, applied in the field of electrolytic cells, can solve the problems of electrolyte molecular ratio, large content difference, high cost, uncertainty of test results, etc., and achieve the effect of meeting the preparation requirements

Active Publication Date: 2019-11-22
GUIZHOU BRANCH CHINA ALUMINUM IND
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] The sodium expansion rate index of the cathode is an important index to measure whether the electrolytic cell can withstand electrolyte erosion. At present, there are many problems in the test of this index. First, the cost of the test is high. The graphite crucible, thermocouple, and electrolyte reagents are all disposable. Consumables, the cost of doing a test is relatively high; secondly, the electrolyte reagents required for the test are currently purchased abroad, each reagent needs more than 2,000 yuan, and only one sample can be tested
However, if a self-prepared electrolyte reagent is used for the test, the molecular ratio and content of the overall electrolyte vary greatly. In addition, due to the small volume density, the electrolyte sample of the same quality cannot be loaded into the graphite crucible, so it can only be added less or the crucible The size is enlarged to solve it, which brings more uncertainty to the test results

Method used

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preparation example Construction

[0010] The synthesis method of the electrolyte sample used for the sodium expansion rate test of the present invention comprises the following steps: batching cryolite, sodium fluoride, calcium fluoride and aluminum oxide according to a certain ratio, then mixing the mixture and pouring it into a graphite crucible Heating to 950°C-1000°C and keeping it warm for 0.5h-1h, stirring continuously to let the air bubbles escape; then scoop out the melt and cool it down to form an electrolyte sample block, and use a jaw crusher to rough the electrolyte sample block Crushed to less than 3mm, the crushed sample is divided into two parts: one part is crushed to 1mm-2mm with a roller crusher, and one part is ground with a sample mill to completely pass through a 0.075mm test sieve. Samples are mixed in a certain proportion to obtain electrolyte samples that satisfy the determination of sodium expansion ratio.

[0011] The specific steps are:

[0012] 1. Firstly mix cryolite (purity not l...

Embodiment 1

[0020] 1. Firstly mix cryolite (purity not less than 99.7%), sodium fluoride (purity not less than 99.7%), calcium fluoride (purity not less than 97%) and alumina (purity not less than 98%) according to the weight ratio of 71.5% :14.5%:5.0%:9.0% The ratio is fully mixed:

[0021] 2. Pour the mixture into a graphite crucible and heat it to 950°C and keep it warm for 0.5h. During this period, stir continuously to make the bubbles fully escape;

[0022] 3. Then use a heat-resistant stainless steel sampling tool and sample mold to invert the electrolyte melt and cool it down to become an electrolyte sample block. The recommended size is φ65mm×50mm;

[0023] 4. Use a jaw crusher to roughly crush the sample block to less than 3 mm, and divide the crushed sample into two parts: one part is crushed to about 1 mm by a double-roller crusher, and is used as component A; the other part is ground by a vibratory mill 30s, make all the samples pass through the test sieve of 0.075mm, as comp...

Embodiment 2

[0026] 1. Firstly mix cryolite (purity not less than 99.7%), sodium fluoride (purity not less than 99.7%), calcium fluoride (purity not less than 97%) and alumina (purity not less than 98%) according to the weight ratio of 71.5% :14.5%:5.0%:9.0% The ratio is fully mixed:

[0027] 2. Pour the mixture into a graphite crucible and heat it to 980°C and keep it warm for 1 hour. During this period, keep stirring to make the bubbles fully escape;

[0028] 3. Then use a heat-resistant stainless steel sampling tool and sample mold to invert the electrolyte melt and cool it down to become an electrolyte sample block. The recommended size is φ65mm×50mm;

[0029] 4. Use a jaw crusher to roughly crush the sample block to less than 3 mm, and divide the crushed sample into two parts: one part is crushed to about 2 mm by a double-roller crusher, and is used as component A; the other part is ground by a vibratory mill 30s, make all the samples pass through the test sieve of 0.075mm, as compon...

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Abstract

The invention relates to a synthesis method of an electrolyte sample for sodium expansion rate test. The method comprises: proportioning cryolite, sodium fluoride, calcium fluoride and aluminum oxideaccording to a certain ratio, uniformly mixing the mixture, pouring the mixture into a graphite crucible, heating the mixture to a melting temperature, keeping the temperature for a certain time, andcontinuously stirring to escape bubbles during the period; and scooping out a melt by using a proper sampling tool, cooling the melt, and pouring the melt into a mold to form an electrolyte sample block, coarsely crushing a sample block to be less than 3mm by using a jaw crusher, dividing the sample into two parts, crushing one part to be about 1mm-2mm by using a double-roll crusher, grinding theother part by using a sample grinding machine to substances that can completely pass a 0.075 mm test sieve, and mixing the two parts of samples according to a certain ratio to obtain an electrolyte sample meeting the measurement of the sodium expansion rate. According to the method, the electrolyte sample for sodium expansion rate test is prepared by melting and particle size mixing, and the finalelectrolyte reagent can replace imported ones, is more economical and applicable, and can meet the preparation requirements of crucibles with different sizes.

Description

technical field [0001] The invention belongs to the technical field of electrolyzers, and in particular relates to a method for preparing electrolyte samples for sodium expansion rate testing by means of melting and particle size mixing. Background technique [0002] The sodium expansion rate index of the cathode is an important index to measure whether the electrolytic cell can withstand electrolyte erosion. At present, there are many problems in the test of this index. First, the cost of the test is high. The graphite crucible, thermocouple, and electrolyte reagents are all disposable. Consumables, the cost of doing a test is relatively high; secondly, the electrolyte reagents required for the test are currently purchased abroad, each reagent needs more than 2,000 yuan, and only one sample can be tested. However, if a self-prepared electrolyte reagent is used for the test, the molecular ratio and content of the overall electrolyte vary greatly. In addition, due to the smal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28
CPCG01N1/28
Inventor 仓向辉张树朝卢成王锦寇帆
Owner GUIZHOU BRANCH CHINA ALUMINUM IND
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