CN110456118A - A kind of preparation method for adsorbing fused salt mixt carbon felt electrode - Google Patents
A kind of preparation method for adsorbing fused salt mixt carbon felt electrode Download PDFInfo
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- CN110456118A CN110456118A CN201910744901.4A CN201910744901A CN110456118A CN 110456118 A CN110456118 A CN 110456118A CN 201910744901 A CN201910744901 A CN 201910744901A CN 110456118 A CN110456118 A CN 110456118A
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- measuring cup
- carbon felt
- fused salt
- salt mixt
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R3/00—Apparatus or processes specially adapted for the manufacture or maintenance of measuring instruments, e.g. of probe tips
Abstract
The invention belongs to conductivity measurement technique fields, especially a kind of preparation method for adsorbing fused salt mixt carbon felt electrode, include the following steps S1: taking the measuring cup between 10-20L to be placed on room temperature is between 20-25 DEG C, indoor humidity is operated in the indoor environment between 30%-50%, S2: the aqueous solution of 8-12L is poured into measuring cup, 80-100 ㎎ lithium nitrate and sodium nitrate 30-60 ㎎ are poured into measuring cup and are stirred 10-15min again, S3: 70-110 ㎎ sodium nitrite is poured into measuring cup and quickly stirs 3-5min, after stirring finishes, stood 10-20min, S4: solid nitric acid barium 10-25 ㎎ is pulverized, it pulverizes and powdered barium nitrate is used into 20-30 mesh sieve after finishing It is sieved.The method of the present invention preparation absorption fused salt mixt carbon felt as measure solid electrolyte ion conductivity electrode material, avoid metallic sodium as measuring electrode bring security risk and environmental problem in high temperature measurement.
Description
Technical field
The present invention relates to conductivity measurement technique field more particularly to a kind of preparation sides for adsorbing fused salt mixt carbon felt electrode
Method.
Background technique
Conductivity, physics concept, is referred to as conductivity.The amount and the product of electric field strength E, which are equal to, in the medium passes
Conductive current density J.For isotropic medium, conductivity is scalar;For anisotropic medium, conductivity is tensor.Ecology
In, conductivity is the ability of solution conduction electric current numerically.Unit is indicated with every meter of Siemens (S/m).
Solid electrolyte Al2O3 ceramic material has good Na+ ionic conduction performance, at normal temperature its ionic conductivity
The order of magnitude that can reach 10-2S/cm is mainly used as the ion-conducting separator of sodium-sulphur battery and the diaphragm element of gas sensor,
It is the core component of sodium-sulphur battery and other a variety of electrochemical devices.In application process, β ' '-Al2O3 solid electrolytic
Matter ionic conductivity with higher.The sodium sode cell made of metallic sodium is generallyd use as β ' '-Al2O3 solid electrolyte
Ionic conductivity measuring electrode, but the molten sodium in hot environment is very active, is prepared into sode cell test β ' '-Al2O3
Solid electrolyte sodium ion conductivity, if solid electrolyte is off quality, the danger easily exploded, so it is proposed that
A kind of preparation method for adsorbing fused salt mixt carbon felt electrode, solving the problems, such as above-mentioned propose.
Summary of the invention
The purpose of the present invention is to solve a kind of absorption that the prior art exists in the prior art, and proposes to mix
Close the preparation method of fused salt carbon felt electrode.
To achieve the goals above, present invention employs following technical solutions:
A kind of preparation method for adsorbing fused salt mixt carbon felt electrode, comprising the following steps:
S1: taking the measuring cup between 10-20L to be placed on room temperature is between 20-25 DEG C, and indoor humidity is between 30%-50%
Indoor environment in operated;
S2: the aqueous solution of 8-12L is poured into measuring cup, then by 80-100 ㎎ lithium nitrate and the sodium nitrate 30-60 ㎎ amount of being poured into
10-15min is stirred in cup;
S3: 70-110 ㎎ sodium nitrite being poured into measuring cup and quickly stirs 3-5min, after stirring finishes, is stood 10-
20min;
S4: solid nitric acid barium 10-25 ㎎ is pulverized, and pulverizes and powdered barium nitrate is used 20-30 mesh after finishing
Son is sieved;
S5: the powdered barium nitrate after excessively complete sieve is put into measuring cup, is then stirred 7- to the solution in measuring cup
12min just obtains fused salt mixt at this time;
S6: taking a length of 3-5cm, and width is placed in measuring cup for the carbon felt of 6-8cm to be impregnated;
S7: the opening in measuring cup is blocked using sealing cover, while measuring cup being vacuumized;
S8: pressurizeing to measuring cup, so that fused salt mixt is pressed into carbon felt;
S9: after impregnating 10-20min to carbon felt, can dry carbon felt, just form fused salt mixt carbon felt electricity at this time
Pole.
Preferably, in the S1, measuring cup is made of transparent glass material, and visual containing mark is provided in measuring cup.
Preferably, in the S2, when the solution in measuring cup being mixed using rubber bar, and according to suitable when stirring
It ceaselessly stirs in one direction of hour hands.
Preferably, it in the S3, when being stirred the solution in its measuring cup using quick agitating mode, needs to reach
80-120 circle moving rubber bar per minute is stirred.
Preferably, in the S4, solid nitric acid barium is placed on clean blank sheet of paper, then wraps blank sheet of paper to it
It wraps up in, solid nitric acid barium can push repeatedly and be pulverized by operator using waddy at this time.
Preferably, in the S5, the powdered barium nitrate after excessively complete sieve is put into measuring cup, then in measuring cup
Solution is stirred 8-11min, just obtains fused salt mixt at this time.
Preferably, in the S6, when carbon felt to be placed in measuring cup, carbon felt 10-15s is first stirred, so that fused salt mixt
It can sufficiently be put into and immerse in carbon felt.
Preferably, in the S7, measuring cup can be vacuumized using evacuator.
Preferably, it in the S8, can be pressurizeed to measuring cup using pressuring machine.
Preferably, in the S8, after 11-18min being impregnated to carbon felt, carbon felt can be put into drying box and is carried out
Drying.
In the present invention, taking the measuring cup between 10-20L to be placed on room temperature is between 20-25 DEG C, and indoor humidity is
It is operated in indoor environment between 30%-50%, the aqueous solution of 8-12L is poured into measuring cup, then by 80-100 ㎎ nitre
Sour lithium and sodium nitrate 30-60 ㎎ are poured into measuring cup and are stirred 10-15min, and 70-110 ㎎ sodium nitrite is poured into measuring cup
In quickly stir 3-5min, after stirring finishes, is stood 10-20min, solid nitric acid barium 10-25 ㎎ is pulverized, stone roller
It is broken finish after powdered barium nitrate is sieved using 20-30 mesh sieve, the powdered barium nitrate after excessively complete sieve
It puts into measuring cup, 7-12min then is stirred to the solution in measuring cup, just obtains fused salt mixt at this time, take a length of 3-
5cm, width is placed in measuring cup for the carbon felt of 6-8cm to be impregnated, and is blocked the opening in measuring cup using sealing cover, this simultaneously will
Measuring cup is vacuumized, and is pressurizeed to measuring cup so that fused salt mixt is pressed into carbon felt, to carbon felt impregnate 10-20min it
Afterwards, carbon felt can be dried, just forms fused salt mixt carbon felt electrode at this time.
Electrode material of the absorption fused salt mixt carbon felt of the method for the present invention preparation as measurement solid electrolyte ion conductivity
Material, avoid metallic sodium as measuring electrode bring security risk and environmental problem in high temperature measurement.
Specific embodiment
Below in conjunction with the method in the embodiment of the present invention, technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.
Embodiment one
A kind of preparation method for adsorbing fused salt mixt carbon felt electrode, comprising the following steps:
S1: taking the measuring cup between 10L to be placed on room temperature is between 20 DEG C, and indoor humidity is in the indoor environment between 30%
It is operated;
S2: the aqueous solution of 8L is poured into measuring cup, then 80 ㎎ lithium nitrates and 30 ㎎ of sodium nitrate are poured into measuring cup and are stirred
Mix 10min;
S3: 70-110 ㎎ sodium nitrite being poured into measuring cup and quickly stirs 3min, after stirring finishes, is stood 10min;
S4: 10 ㎎ of solid nitric acid barium is pulverized, and is pulverized and is carried out powdered barium nitrate using 20 mesh sieve after finishing
Screening;
S5: the powdered barium nitrate after excessively complete sieve is put into measuring cup, is then stirred 7min to the solution in measuring cup,
Fused salt mixt is just obtained at this time;
S6: taking a length of 3cm, and width is placed in measuring cup for the carbon felt of 6cm to be impregnated;
S7: the opening in measuring cup is blocked using sealing cover, while measuring cup being vacuumized;
S8: pressurizeing to measuring cup, so that fused salt mixt is pressed into carbon felt;
S9: after impregnating 10min to carbon felt, carbon felt can be dried, just forms fused salt mixt carbon felt electrode at this time.
In the present embodiment, in S1, measuring cup is made of transparent glass material, and visual containing mark is provided in measuring cup.
In the present embodiment, in S2, when the solution in measuring cup being mixed using rubber bar, and according to suitable when stirring
It ceaselessly stirs in one direction of hour hands.
In the present embodiment, in S3, when being stirred the solution in its measuring cup using quick agitating mode, need to reach
80 circle moving rubber bar per minute is stirred.
In the present embodiment, in S4, solid nitric acid barium is placed on clean blank sheet of paper, then wraps blank sheet of paper to it
It wraps up in, solid nitric acid barium can push repeatedly and be pulverized by operator using waddy at this time.
In the present embodiment, in S5, the powdered barium nitrate after excessively complete sieve is put into measuring cup, then in measuring cup
Solution is stirred 8min, just obtains fused salt mixt at this time.
In the present embodiment, in S6, when carbon felt to be placed in measuring cup, carbon felt 10s is first stirred, so that fused salt mixt can be with
It is sufficiently put into and immerses in carbon felt.
In the present embodiment, in S7, measuring cup can be vacuumized using evacuator.
In the present embodiment in S8, it can be pressurizeed to measuring cup using pressuring machine.
In the present embodiment, in S8, after 11min being impregnated to carbon felt, carbon felt can be put into drying box and be dried
It is dry.
Embodiment two
A kind of preparation method for adsorbing fused salt mixt carbon felt electrode, comprising the following steps:
S1: taking the measuring cup between 15L to be placed on room temperature is between 22 DEG C, and indoor humidity is in the indoor environment between 40%
It is operated;
S2: the aqueous solution of 10L is poured into measuring cup, then 90 ㎎ lithium nitrates and 45 ㎎ of sodium nitrate are poured into measuring cup and are stirred
Mix 12min;
S3: 70-110 ㎎ sodium nitrite being poured into measuring cup and quickly stirs 4min, after stirring finishes, is stood 15min;
S4: 20 ㎎ of solid nitric acid barium is pulverized, and is pulverized and is carried out powdered barium nitrate using 25 mesh sieve after finishing
Screening;
S5: the powdered barium nitrate after excessively complete sieve is put into measuring cup, is then stirred to the solution in measuring cup
10min just obtains fused salt mixt at this time;
S6: taking a length of 4cm, and width is placed in measuring cup for the carbon felt of 7cm to be impregnated;
S7: the opening in measuring cup is blocked using sealing cover, while measuring cup being vacuumized;
S8: pressurizeing to measuring cup, so that fused salt mixt is pressed into carbon felt;
S9: after impregnating 15min to carbon felt, carbon felt can be dried, just forms fused salt mixt carbon felt electrode at this time.
In the present embodiment, in S1, measuring cup is made of transparent glass material, and visual containing mark is provided in measuring cup.
In the present embodiment, in S2, when the solution in measuring cup being mixed using rubber bar, and according to suitable when stirring
It ceaselessly stirs in one direction of hour hands.
In the present embodiment, in S3, when being stirred the solution in its measuring cup using quick agitating mode, need to reach
100 circle moving rubber bar per minute is stirred.
In the present embodiment, in S4, solid nitric acid barium is placed on clean blank sheet of paper, then wraps blank sheet of paper to it
It wraps up in, solid nitric acid barium can push repeatedly and be pulverized by operator using waddy at this time.
In the present embodiment, in S5, the powdered barium nitrate after excessively complete sieve is put into measuring cup, then in measuring cup
Solution is stirred 9min, just obtains fused salt mixt at this time.
In the present embodiment, in S6, when carbon felt to be placed in measuring cup, carbon felt 12s is first stirred, so that fused salt mixt can be with
It is sufficiently put into and immerses in carbon felt.
In the present embodiment, in S7, measuring cup can be vacuumized using evacuator.
In the present embodiment in S8, it can be pressurizeed to measuring cup using pressuring machine.
In the present embodiment, in S8, after 14min being impregnated to carbon felt, carbon felt can be put into drying box and be dried
It is dry.
Embodiment three
A kind of preparation method for adsorbing fused salt mixt carbon felt electrode, comprising the following steps:
S1: taking the measuring cup between 20L to be placed on room temperature is between 25 DEG C, and indoor humidity is in the indoor environment between 50%
It is operated;
S2: the aqueous solution of 12L is poured into measuring cup, then 100 ㎎ lithium nitrates and 60 ㎎ of sodium nitrate are poured into measuring cup and are carried out
Stir 15min;
S3: 110 ㎎ sodium nitrites being poured into measuring cup and quickly stir 5min, after stirring finishes, is stood 20min;
S4: 25 ㎎ of solid nitric acid barium is pulverized, and is pulverized and is carried out powdered barium nitrate using 30 mesh sieve after finishing
Screening;
S5: the powdered barium nitrate after excessively complete sieve is put into measuring cup, is then stirred to the solution in measuring cup
12min just obtains fused salt mixt at this time;
S6: taking a length of 5cm, and width is placed in measuring cup for the carbon felt of 8cm to be impregnated;
S7: the opening in measuring cup is blocked using sealing cover, while measuring cup being vacuumized;
S8: pressurizeing to measuring cup, so that fused salt mixt is pressed into carbon felt;
S9: after impregnating 20min to carbon felt, carbon felt can be dried, just forms fused salt mixt carbon felt electrode at this time.
In the present embodiment, in S1, measuring cup is made of transparent glass material, and visual containing mark is provided in measuring cup.
In the present embodiment, in S2, when the solution in measuring cup being mixed using rubber bar, and according to suitable when stirring
It ceaselessly stirs in one direction of hour hands.
In the present embodiment, in S3, when being stirred the solution in its measuring cup using quick agitating mode, need to reach
120 circle moving rubber bar per minute is stirred.
In the present embodiment, in S4, solid nitric acid barium is placed on clean blank sheet of paper, then wraps blank sheet of paper to it
It wraps up in, solid nitric acid barium can push repeatedly and be pulverized by operator using waddy at this time.
In the present embodiment, in S5, the powdered barium nitrate after excessively complete sieve is put into measuring cup, then in measuring cup
Solution is stirred 11min, just obtains fused salt mixt at this time.
In the present embodiment, in S6, when carbon felt to be placed in measuring cup, carbon felt 10-15s is first stirred, so that fused salt mixt
It can sufficiently be put into and immerse in carbon felt.
In the present embodiment, in S7, measuring cup can be vacuumized using evacuator.
In the present embodiment in S8, it can be pressurizeed to measuring cup using pressuring machine.
In the present embodiment, in S8, after 18min being impregnated to carbon felt, carbon felt can be put into drying box and be dried
It is dry.
Performance comparative experiments is carried out to embodiment 1-3, compares conventional carbon felt electrode, it is shown that the experimental data are shown in the following table:
By above table it is found that the present invention, which can be improved the preparation speed of carbon felt electrode and improve Ai Zhiliang, stablizes percentage,
And embodiment three is most preferred embodiment.
More than, it is merely preferred embodiments of the present invention, but scope of protection of the present invention is not limited thereto, it is any
Those familiar with the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its invents
Design is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of preparation method for adsorbing fused salt mixt carbon felt electrode, which comprises the following steps:
S1: taking the measuring cup between 10-20L to be placed on room temperature is between 20-25 DEG C, and indoor humidity is between 30%-50%
Indoor environment in operated;
S2: the aqueous solution of 8-12L is poured into measuring cup, then by 80-100 ㎎ lithium nitrate and the sodium nitrate 30-60 ㎎ amount of being poured into
10-15min is stirred in cup;
S3: 70-110 ㎎ sodium nitrite being poured into measuring cup and quickly stirs 3-5min, after stirring finishes, is stood 10-
20min;
S4: solid nitric acid barium 10-25 ㎎ is pulverized, and pulverizes and powdered barium nitrate is used 20-30 mesh after finishing
Son is sieved;
S5: the powdered barium nitrate after excessively complete sieve is put into measuring cup, is then stirred 7- to the solution in measuring cup
12min just obtains fused salt mixt at this time;
S6: taking a length of 3-5cm, and width is placed in measuring cup for the carbon felt of 6-8cm to be impregnated;
S7: the opening in measuring cup is blocked using sealing cover, while measuring cup being vacuumized;
S8: pressurizeing to measuring cup, so that fused salt mixt is pressed into carbon felt;
S9: after impregnating 10-20min to carbon felt, can dry carbon felt, just form fused salt mixt carbon felt electricity at this time
Pole.
2. a kind of preparation method for adsorbing fused salt mixt carbon felt electrode according to claim 1, which is characterized in that the S1
In, measuring cup is made of transparent glass material, and visual containing mark is provided in measuring cup.
3. a kind of preparation method for adsorbing fused salt mixt carbon felt electrode according to claim 1, which is characterized in that the S2
In, when the solution in measuring cup being mixed using rubber bar, and ceaselessly stirred when stirring according to a direction clockwise
It mixes.
4. a kind of preparation method for adsorbing fused salt mixt carbon felt electrode according to claim 1, which is characterized in that the S3
In, when being stirred using quick agitating mode to the solution in its measuring cup, need to reach 80-120 circle moving rubber per minute
Glue stick is stirred.
5. a kind of preparation method for adsorbing fused salt mixt carbon felt electrode according to claim 1, which is characterized in that the S4
In, solid nitric acid barium is placed on clean blank sheet of paper, then wraps up it blank sheet of paper, operator can utilize wood at this time
Solid nitric acid barium push repeatedly by rod to be pulverized.
6. a kind of preparation method for adsorbing fused salt mixt carbon felt electrode according to claim 1, which is characterized in that the S5
In, the powdered barium nitrate after excessively complete sieve is put into measuring cup, 8-11min then is stirred to the solution in measuring cup,
Fused salt mixt is just obtained at this time.
7. a kind of preparation method for adsorbing fused salt mixt carbon felt electrode according to claim 1, which is characterized in that the S6
In, when carbon felt to be placed in measuring cup, carbon felt 10-15s is first stirred, fused salt mixt is allowed sufficiently to be put into immersion carbon felt
In.
8. a kind of preparation method for adsorbing fused salt mixt carbon felt electrode according to claim 1, which is characterized in that the S7
In, measuring cup can be vacuumized using evacuator.
9. a kind of preparation method for adsorbing fused salt mixt carbon felt electrode according to claim 1, which is characterized in that the S8
In, it can be pressurizeed to measuring cup using pressuring machine.
10. a kind of preparation method for adsorbing fused salt mixt carbon felt electrode according to claim 1, which is characterized in that described
In S8, after 11-18min being impregnated to carbon felt, carbon felt can be put into drying box and be dried.
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CN102347486A (en) * | 2011-10-26 | 2012-02-08 | 吴润秀 | Method for preparing barium-activated lithium iron phosphate cathode material |
CN103116046A (en) * | 2012-12-12 | 2013-05-22 | 上海电气钠硫储能技术有限公司 | Preparation method for absorbing mixed fused salt carbon felt electrodes |
CN104716343A (en) * | 2015-01-07 | 2015-06-17 | 河南师范大学 | High-performance composite carbon felt |
CN105527467A (en) * | 2015-12-21 | 2016-04-27 | 上海电气钠硫储能技术有限公司 | Carbon felt clamp and carbon felt compaction method |
CN106129335A (en) * | 2016-07-14 | 2016-11-16 | 钟凤珍 | A kind of anode preparation method of lithium battery |
CN108134096A (en) * | 2017-12-10 | 2018-06-08 | 长沙无道工业设计有限公司 | A kind of method of modifying of carbon felt for vanadium redox battery electrode |
CN109473685A (en) * | 2018-11-12 | 2019-03-15 | 湖南国昶能源科技有限公司 | A kind of preparation method of the compound carbon felt of graphene |
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2019
- 2019-08-13 CN CN201910744901.4A patent/CN110456118A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102347486A (en) * | 2011-10-26 | 2012-02-08 | 吴润秀 | Method for preparing barium-activated lithium iron phosphate cathode material |
CN103116046A (en) * | 2012-12-12 | 2013-05-22 | 上海电气钠硫储能技术有限公司 | Preparation method for absorbing mixed fused salt carbon felt electrodes |
CN104716343A (en) * | 2015-01-07 | 2015-06-17 | 河南师范大学 | High-performance composite carbon felt |
CN105527467A (en) * | 2015-12-21 | 2016-04-27 | 上海电气钠硫储能技术有限公司 | Carbon felt clamp and carbon felt compaction method |
CN106129335A (en) * | 2016-07-14 | 2016-11-16 | 钟凤珍 | A kind of anode preparation method of lithium battery |
CN108134096A (en) * | 2017-12-10 | 2018-06-08 | 长沙无道工业设计有限公司 | A kind of method of modifying of carbon felt for vanadium redox battery electrode |
CN109473685A (en) * | 2018-11-12 | 2019-03-15 | 湖南国昶能源科技有限公司 | A kind of preparation method of the compound carbon felt of graphene |
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Application publication date: 20191115 |