CN110373113A - A kind of preparation method of fusing point adjustable high-efficiency sealant - Google Patents
A kind of preparation method of fusing point adjustable high-efficiency sealant Download PDFInfo
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- CN110373113A CN110373113A CN201910443443.0A CN201910443443A CN110373113A CN 110373113 A CN110373113 A CN 110373113A CN 201910443443 A CN201910443443 A CN 201910443443A CN 110373113 A CN110373113 A CN 110373113A
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- sealant
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J1/00—Adhesives based on inorganic constituents
Abstract
The present invention relates to a kind of preparation method of fusing point adjustable high-efficiency sealant, belong to fuel cell and it is secondary can charge and discharge battery need to completely cut off the sealing material fields such as gaseous environment.The preparation method of the fusing point adjustable high-efficiency sealant is by MgO, BaO, SiO2, five kinds of oxides of Bi2O3 and H3BO3 or more are scattered in acetone in planetary ball mill high speed ball milling, it ensure that the uniform grinding of preceding material, the mechanical activation of particle before heat treatment is also ensured, so that powder becomes micro-nano granules；The high-temperature heat treatment time after ball milling greatly shortens, and heat treatment temperature and time substantially reduce.The great advantage of the sealant of the preparation method preparation of the fusing point adjustable high-efficiency sealant is purity is high, and operating temperature window is extremely wide to can reach -30-1115 DEG C, and sealing performance is excellent, fusing point is adjustable, can apply in multiple atmosphere and under environment, chemical stability is high, service life is long, cheap.
Description
Technical field
The present invention relates to a kind of preparation method of fusing point adjustable high-efficiency sealant, belong to fuel cell and it is secondary can charge and discharge
Battery needs to completely cut off the sealing material fields such as gaseous environment.
Background technique
Conventional seals glue, which refers to, to be not easy to trickle, and has the sealing material of certain caking property.It is for filling configuration gap, to rise
To the adhesive of sealing function.Have the effects that anti-leak, waterproof, vibration proof and sound insulation, heat-insulated.Usually with pitch object, natural
The dope of the stemness such as resin or synthetic resin, natural rubber or synthetic rubber or non-dry is base-material, cooperation talcum powder, white
The inert fillers such as soil, carbon black, titanium dioxide and asbestos add plasticizer, solvent, curing agent, promotor etc. and are made.It is widely used in
Building, communications and transportation, the sealing of electronic instrument and components.But in high temperature solid oxide fuel cell and can charge and discharge
In the sodium-sulphur battery and the equipment such as metal-air battery of electricity, because the component of colloid has an organic components, oxygen is at high temperature quickly
Colloid is fallen in oxidation corrosion, so that gas leaks, equipment failure, and or even the danger of thermal runaway explosion on fire occurs.
Summary of the invention
In order to overcome defect present in background technique, the technical solution adopted by the present invention to solve the technical problems is:
A kind of preparation method of fusing point adjustable high-efficiency sealant, it is characterised in that the steps include:
Step 1: high speed ball milling admixture activation sealant material presoma, by MgO, BaO, SiO2, Bi2O3 and H3BO3 or more five
Kind oxide is that the stoichiometric ratio of 3:2:1:1:2 to molar ratio 3:2:5:1:2 are scattered in acetone in molar ratio, acetone liquid level
Higher than powder uniformly to mix, then oxide in five and acetone are fitted into ball grinder together, in planetary ball mill high speed
Ball milling, revolving speed turn for 200-600 per minute, and Ball-milling Time is 2-6 hours, before then being cleaned, filtered with acetone, dried, being obtained
It is spare to drive body powder；
Step 2: precursor powder prepared by high temperature heat treatment step one, obtained precursor powder is moved in platinum crucible,
Using elevator furnace calcination in air atmosphere, heating rate is 5-10 DEG C/min, and holding temperature range is 1500 DEG C -1600 DEG C,
Soaking time is to obtain melt liquid in 1-2 hours；
Step 3: fusant is taken out from elevator furnace, within 5 seconds, crystallisation by cooling in normal-temperature water is poured into, the volume of water is
10 times or more of fusant volume；
Step 4: cooling crystal is taken out, it is fitted into ball mill crushing in ball grinder；In planetary ball mill high speed ball milling, planet ball
The revolving speed of grinding machine turns for 550-650 per minute, and Ball-milling Time is 6-10 hours, is then cleaned, filtered, dried with acetone, obtained
Finished product.
Holding temperature range in the preferred step 2 is 1530 DEG C -1560 DEG C.
A kind of preparation method of fusing point adjustable high-efficiency sealant according to the present invention, the fusing point adjustable high-efficiency sealant
The great advantage of the sealant of preparation method preparation is purity is high, and operating temperature window is extremely wide to can reach -30-1115 DEG C, sealing
It has excellent performance, fusing point is adjustable, can apply in multiple atmosphere and under environment, chemical stability is high, and the service life is long, cheap.
Using it as the equipment of sealing material, for many years without evaporating, emitting, dripping or leaking of liquid or gas phenomenon, securely and reliably, the preparation method of sequencing is simple and effective, can
Expand rapidly large-scale production.Furthermore the preparation method of the fusing point adjustable high-efficiency sealant also has the advantage that
1, it disperses five kinds of oxides of MgO, BaO, SiO2, Bi2O3 and H3BO3 or more in acetone in planetary ball mill high speed
Ball milling ensure that the uniform grinding of preceding material, also ensure the mechanical activation of particle before heat treatment, so that powder becomes micro-nano
Particle.
2, the high-temperature heat treatment time after ball milling greatly shortens, and heat treatment temperature and time substantially reduce.
3, rapid cooling treatment makes the solidification of melt liquid moment and dusting, and forms the crystal form of needs, after being conducive to
Continuous mechanical ball mill prepares nano-powder, easy to operate in sealant use process.
4, using the ball mill and electric heating equipment for having industrial standard, expansion scale is suitble to carry out industrial production, drop
Low cost can simultaneously use under the atmospheres such as acid and alkalinity.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is the X ray diffracting spectrum for the sealant that embodiment 1-5 is prepared；
Fig. 2 is the transmission electron microscope map for the sealant that embodiment 2 is prepared；
Fig. 3 is the transmission electron microscope map for the sealant that embodiment 4 is prepared；
Fig. 4 is the scanning electron microscope map for the sealant that embodiment 1 is prepared；
Fig. 5 is the scanning electron microscope map for the sealant that embodiment 3 is prepared；
Fig. 6 is the sealant thermogravimetric and differential thermal experiment curv for the sealant that embodiment 1 is prepared；
Fig. 7 is the sealant thermogravimetric and differential thermal experiment curv for the sealant that embodiment 2 is prepared；
Fig. 8 is the sealant thermogravimetric and differential thermal experiment curv for the sealant that embodiment 3 is prepared；
Fig. 9 is the sealant thermogravimetric and differential thermal experiment curv for the sealant that embodiment 4 is prepared；
Figure 10 is the sealant thermogravimetric and differential thermal experiment curv for the sealant that embodiment 5 is prepared；
Figure 11 is the finished product photo for the sealant that embodiment 1-5 is prepared.
Specific embodiment
In conjunction with the accompanying drawings, the present invention is further explained in detail.Attached drawing is simplified schematic diagram, only with signal side
Formula illustrates basic structure of the invention, therefore it only shows the composition relevant to the invention.
Specific embodiment one please refers to Fig. 1, Fig. 4, Fig. 6 and Figure 11, a kind of preparation side of fusing point adjustable high-efficiency sealant
Method the steps include:
Step 1: high speed ball milling admixture activation sealant material presoma, by MgO, BaO, SiO2, Bi2O3 and H3BO3 or more five
Kind oxide is that the stoichiometric ratio of 3:2:3:1:2 is scattered in acetone in molar ratio, and acetone liquid level is higher than powder uniformly to mix
It closes, is then fitted into oxide in five and acetone in ball grinder together, in planetary ball mill high speed ball milling, revolving speed is per minute
200 turns, Ball-milling Time is 6 hours, is then cleaned, is filtered with acetone, dried, to obtain precursor powder spare；
Step 2: precursor powder prepared by high temperature heat treatment step one, obtained precursor powder is moved in platinum crucible,
Using elevator furnace calcination in air atmosphere, heating rate is 5 DEG C/min, and holding temperature range is 1550 DEG C, soaking time 1
Hour obtains melt liquid；
Step 3: fusant is taken out from elevator furnace, within 5 seconds, crystallisation by cooling in normal-temperature water is poured into, the volume of water is
15 times of fusant volume；
Step 4: cooling crystal is taken out, it is fitted into ball mill crushing in ball grinder；In planetary ball mill high speed ball milling, planet ball
The revolving speed of grinding machine is 550 turns per minute, and Ball-milling Time is 10 hours, is then cleaned, filtered, dried with acetone, obtains finished product.
Specific embodiment two please refers to Fig. 1, Fig. 2, Fig. 7 and Figure 11, a kind of preparation side of fusing point adjustable high-efficiency sealant
Method the steps include:
Step 1: high speed ball milling admixture activation sealant material presoma, by MgO, BaO, SiO2, Bi2O3 and H3BO3 or more five
Kind oxide is that the stoichiometric ratio of 3:2:2:1:2 is scattered in acetone in molar ratio, and acetone liquid level is higher than powder uniformly to mix
It closes, is then fitted into oxide in five and acetone in ball grinder together, in planetary ball mill high speed ball milling, revolving speed is per minute
300 turns, Ball-milling Time is 5 hours, is then cleaned, is filtered with acetone, dried, to obtain precursor powder spare；
Step 2: precursor powder prepared by high temperature heat treatment step one, obtained precursor powder is moved in platinum crucible,
Using elevator furnace calcination in air atmosphere, heating rate is 5 DEG C/min, and holding temperature range is 1550 DEG C, soaking time 1
Hour obtains melt liquid；
Step 3: fusant is taken out from elevator furnace, within 5 seconds, crystallisation by cooling in normal-temperature water is poured into, the volume of water is
15 times of fusant volume；
Step 4: cooling crystal is taken out, it is fitted into ball mill crushing in ball grinder；In planetary ball mill high speed ball milling, planet ball
The revolving speed of grinding machine is 550 turns per minute, and Ball-milling Time is 8 hours, is then cleaned, filtered, dried with acetone, obtains finished product.
Specific embodiment three please refers to Fig. 1, Fig. 5, Fig. 8 and Figure 11, a kind of preparation side of fusing point adjustable high-efficiency sealant
Method the steps include:
Step 1: high speed ball milling admixture activation sealant material presoma, by MgO, BaO, SiO2, Bi2O3 and H3BO3 or more five
Kind oxide is that the stoichiometric ratio of 3:2:1:1:2 is scattered in acetone in molar ratio, and acetone liquid level is higher than powder uniformly to mix
It closes, is then fitted into oxide in five and acetone in ball grinder together, in planetary ball mill high speed ball milling, revolving speed is per minute
400 turns, Ball-milling Time is 2 hours, is then cleaned, is filtered with acetone, dried, to obtain precursor powder spare；
Step 2: precursor powder prepared by high temperature heat treatment step one, obtained precursor powder is moved in platinum crucible,
Using elevator furnace calcination in air atmosphere, heating rate is 10 DEG C/min, and holding temperature range is 1500 DEG C, and soaking time is
Obtain melt liquid within 1 hour；
Step 3: fusant is taken out from elevator furnace, within 5 seconds, crystallisation by cooling in normal-temperature water is poured into, the volume of water is
15 times of fusant volume；
Step 4: cooling crystal is taken out, it is fitted into ball mill crushing in ball grinder；In planetary ball mill high speed ball milling, planet ball
The revolving speed of grinding machine is 600 turns per minute, and Ball-milling Time is 10 hours, is then cleaned, filtered, dried with acetone, obtains finished product.
Specific embodiment four please refers to Fig. 1, Fig. 3, Fig. 9 and Figure 11, a kind of preparation side of fusing point adjustable high-efficiency sealant
Method the steps include:
Step 1: high speed ball milling admixture activation sealant material presoma, by MgO, BaO, SiO2, Bi2O3 and H3BO3 or more five
Kind oxide is that the stoichiometric ratio of 3:2:4:1:2 is scattered in acetone in molar ratio, and acetone liquid level is higher than powder uniformly to mix
It closes, is then fitted into oxide in five and acetone in ball grinder together, in planetary ball mill high speed ball milling, revolving speed is per minute
500 turns, Ball-milling Time is 3 hours, is then cleaned, is filtered with acetone, dried, to obtain precursor powder spare；
Step 2: precursor powder prepared by high temperature heat treatment step one, obtained precursor powder is moved in platinum crucible,
Using elevator furnace calcination in air atmosphere, heating rate is 6 DEG C/min, and holding temperature range is 1600 DEG C, soaking time 2
Hour obtains melt liquid；
Step 3: fusant is taken out from elevator furnace, within 5 seconds, crystallisation by cooling in normal-temperature water is poured into, the volume of water is
15 times of fusant volume；
Step 4: cooling crystal is taken out, it is fitted into ball mill crushing in ball grinder；In planetary ball mill high speed ball milling, planet ball
The revolving speed of grinding machine is 600 turns per minute, and Ball-milling Time is 7 hours, is then cleaned, filtered, dried with acetone, obtains finished product.
Specific embodiment five, please refers to Fig. 1, Figure 10 and Figure 11, a kind of preparation method of fusing point adjustable high-efficiency sealant,
Step are as follows:
Step 1: high speed ball milling admixture activation sealant material presoma, by MgO, BaO, SiO2, Bi2O3 and H3BO3 or more five
Kind oxide is that the stoichiometric ratio of 3:2:5:1:2 is scattered in acetone in molar ratio, and acetone liquid level is higher than powder uniformly to mix
It closes, is then fitted into oxide in five and acetone in ball grinder together, in planetary ball mill high speed ball milling, revolving speed is per minute
200 turns, Ball-milling Time is 2 hours, is then cleaned, is filtered with acetone, dried, to obtain precursor powder spare；
Step 2: precursor powder prepared by high temperature heat treatment step one, obtained precursor powder is moved in platinum crucible,
Using elevator furnace calcination in air atmosphere, heating rate is 8 DEG C/min, and holding temperature range is 1600 DEG C, soaking time 1
Hour obtains melt liquid；
Step 3: fusant is taken out from elevator furnace, within 5 seconds, crystallisation by cooling in normal-temperature water is poured into, the volume of water is
15 times of fusant volume；
Step 4: cooling crystal is taken out, it is fitted into ball mill crushing in ball grinder；In planetary ball mill high speed ball milling, planet ball
The revolving speed of grinding machine is 650 turns per minute, and Ball-milling Time is 6 hours, is then cleaned, filtered, dried with acetone, obtains finished product.
A kind of preparation method of fusing point adjustable high-efficiency sealant according to the present invention, the fusing point adjustable high-efficiency sealant
The great advantage of the sealant of preparation method preparation is purity is high, and operating temperature window is extremely wide to can reach -30-1115 DEG C, sealing
It has excellent performance, fusing point is adjustable, can apply in multiple atmosphere and under environment, chemical stability is high, and the service life is long, cheap.
Using it as the equipment of sealing material, for many years without evaporating, emitting, dripping or leaking of liquid or gas phenomenon, securely and reliably, the preparation method of sequencing is simple and effective, can
Expand rapidly large-scale production.Furthermore the preparation method of the fusing point adjustable high-efficiency sealant also has the advantage that
1, it disperses five kinds of oxides of MgO, BaO, SiO2, Bi2O3 and H3BO3 or more in acetone in planetary ball mill high speed
Ball milling ensure that the uniform grinding of preceding material, also ensure the mechanical activation of particle before heat treatment, so that powder becomes micro-nano
Particle.
2, the high-temperature heat treatment time after ball milling greatly shortens, and heat treatment temperature and time substantially reduce.
3, rapid cooling treatment makes the solidification of melt liquid moment and dusting, and forms the crystal form of needs, after being conducive to
Continuous mechanical ball mill prepares nano-powder, easy to operate in sealant use process.
4, using the ball mill and electric heating equipment for having industrial standard, expansion scale is suitble to carry out industrial production, drop
Low cost can simultaneously use under the atmospheres such as acid and alkalinity.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (2)
1. a kind of preparation method of fusing point adjustable high-efficiency sealant, it is characterised in that the steps include: Step 1: high speed ball milling mixing
Sealant material presoma is activated, is in molar ratio 3:2 by MgO, BaO, SiO2, Bi2O3 and five kinds of oxides of H3BO3 or more:
The stoichiometric ratio of 1:1:2 to molar ratio 3:2:5:1:2 are scattered in acetone, and acetone liquid level is higher than powder uniformly to mix, and are connect
Oxide in five and acetone are fitted into ball grinder together, in planetary ball mill high speed ball milling, revolving speed is 200- per minute
600 turns, Ball-milling Time is 2-6 hours, is then cleaned, is filtered with acetone, dried, to obtain precursor powder spare；Step 2: high
Precursor powder prepared by heat treatment steps one, obtained precursor powder is moved in platinum crucible, is existed using elevator furnace
Calcination under air atmosphere, heating rate are 5-10 DEG C/min, and holding temperature range is 1500 DEG C -1600 DEG C, soaking time 1-2
Hour obtains melt liquid；Step 3: fusant is taken out from elevator furnace, within 5 seconds, cooling knot in normal-temperature water is poured into
Crystalline substance, the volume of water are 10 times of fusant volume or more；Step 4: cooling crystal is taken out, it is fitted into ball mill crushing in ball grinder；
Turning in the revolving speed of planetary ball mill high speed ball milling, planetary ball mill for 550-650 per minute, Ball-milling Time is 6-10 hours,
Then it is cleaned, filtered, dried with acetone, obtain finished product.
2. a kind of preparation method of fusing point adjustable high-efficiency sealant according to claim 1, which is characterized in that the step
Holding temperature range in two is 1530 DEG C -1560 DEG C.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910443443.0A CN110373113A (en) | 2019-05-27 | 2019-05-27 | A kind of preparation method of fusing point adjustable high-efficiency sealant |
| PCT/CN2020/098830 WO2020239136A1 (en) | 2019-05-27 | 2020-06-29 | Preparation method for high-efficiency sealant having adjustable melting point |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910443443.0A CN110373113A (en) | 2019-05-27 | 2019-05-27 | A kind of preparation method of fusing point adjustable high-efficiency sealant |
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| CN110373113A true CN110373113A (en) | 2019-10-25 |
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| CN201910443443.0A Pending CN110373113A (en) | 2019-05-27 | 2019-05-27 | A kind of preparation method of fusing point adjustable high-efficiency sealant |
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| WO (1) | WO2020239136A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2020239136A1 (en) * | 2019-05-27 | 2020-12-03 | 苏州潜寻新能源科技有限公司 | Preparation method for high-efficiency sealant having adjustable melting point |
| CN113506924A (en) * | 2021-06-17 | 2021-10-15 | 重庆金康动力新能源有限公司 | Thermal runaway early warning method and system for battery pack |
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| WO2020239136A1 (en) * | 2019-05-27 | 2020-12-03 | 苏州潜寻新能源科技有限公司 | Preparation method for high-efficiency sealant having adjustable melting point |
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| WO2020239136A1 (en) | 2020-12-03 |
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