CN111234730A - Phase-change powder secondary adsorption method based on metal oxide - Google Patents
Phase-change powder secondary adsorption method based on metal oxide Download PDFInfo
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- CN111234730A CN111234730A CN202010178436.5A CN202010178436A CN111234730A CN 111234730 A CN111234730 A CN 111234730A CN 202010178436 A CN202010178436 A CN 202010178436A CN 111234730 A CN111234730 A CN 111234730A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/066—Cooling mixtures; De-icing compositions
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
- C08L91/06—Waxes
Abstract
The secondary adsorption method of the phase-change powder based on the metal oxide comprises the following steps: heating a first phase change material to 80-100 ℃, and stirring, wherein the first phase change material is a first adsorption carrier after adsorbing phase change powder; adding a second adsorption carrier into the stirred first phase change material, wherein the second adsorption carrier is a metal oxide; heating the first phase change material added with the second adsorption carrier to more than 100 ℃, and stirring; and cooling the first phase change material which is uniformly stirred and added with the second adsorption carrier to the normal temperature to obtain a second phase change material. The filling and sealing material in the embodiment of the application effectively adsorbs the phase-change powder body overflowed by the phase-change substances again, and the flowability of the filling and sealing material is increased, so that the filling density of the filling and sealing material is improved when the filling and sealing material is used for filling corresponding containers.
Description
Technical Field
The invention relates to the technical field of encapsulating materials and preparation methods thereof, in particular to a secondary adsorption method of phase-change powder based on metal oxide.
Background
The electronic pouring sealant is liquid before being cured, has fluidity, and the viscosity of the glue solution is different according to the material, the performance and the production process of the product. The pouring sealant can realize the use value after being completely cured, and can play the roles of water resistance, moisture resistance, dust prevention, insulation, heat conduction, confidentiality, corrosion resistance, temperature resistance and shock resistance after being cured.
In order to improve the performance of the electronic pouring sealant, phase-change powder is added into the pouring material. In practical application, the phase-change material after first adsorbing the phase-change powder can overflow the phase-change powder, so that the oil leakage phenomenon of the encapsulating material is caused, and the quality of the encapsulating material is influenced; on the other hand, the overflow of the phase-change powder reduces the heat storage performance of the product.
Disclosure of Invention
One of the objectives of the present invention is to provide a secondary adsorption method for phase-change powder based on metal oxide, which is performed with a secondary adsorption treatment, so as to solve the problem of phase-change powder overflow of the electronic potting adhesive in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
the phase-change powder secondary adsorption method based on the metal oxide comprises the following steps:
s1, heating a first phase change material to 80-100 ℃, and stirring, wherein the first phase change material is a first adsorption carrier after adsorbing phase change powder, and the first adsorption carrier is graphite, aerogel or capsule;
s2, adding a second adsorption carrier into the stirred first phase change material, wherein the second adsorption carrier is a metal oxide;
s3, heating the first phase change material added with the second adsorption carrier to 70-120 ℃, and stirring;
the heating temperature of the phase change material needs to be 20-60 ℃ higher than the phase change temperature, so the temperature range is generally set to be 70-120 ℃.
And S4, cooling the first phase change material which is uniformly stirred and added with the second adsorption carrier to normal temperature to obtain a second phase change material.
In one embodiment, said obtaining of the second phase change material comprises:
s5, the second phase change material in the step S4 is pulverized.
In one embodiment, after the step of pulverizing the second phase change material in the step S4, the method includes:
s6, sieving the second phase change material processed in step S5 to obtain a second phase change material in powder form.
In one embodiment, the stirring in step S3 includes:
and (3) placing the first phase change material added with the second adsorption carrier into a planetary stirrer, and stirring at the speed of 30 revolutions per minute and under the condition that the vacuum degree is between-0.04 and-0.10 Mpa.
In one embodiment, the stirring in step S3 further includes: the stirring time is 30 to 60 minutes.
In one embodiment, the heating and stirring the first phase change material to 80 to 100 degrees celsius comprises:
and (3) placing the first phase change material in a reaction kettle, heating to 80-100 ℃, vacuumizing the reaction kettle, and stirring.
In one embodiment, the vacuum is between-0.04 and-0.10 MPa, the vacuum is applied for 5-40min, and the stirring is continued for 15-90 min.
In one embodiment, from 5 to 20 parts of the first adsorption carrier are present per 100 parts by weight of the first phase change material;
80 to 95 parts of the phase change powder exist in each 100 parts by weight of the first phase change material.
In one embodiment, from 1 to 10 parts of said second adsorbent carrier is present per 100 parts by weight of said second phase change material; from 90 to 99 parts of said first phase change material per 100 parts by weight of said second phase change material.
In one embodiment, the metal oxide comprises at least one of the following materials:
aluminum oxide, aluminum nitride, copper oxide, and silicon oxide.
Compared with the prior art, the phase-change powder secondary adsorption method based on the metal oxide has the following beneficial effects:
the encapsulating material treated by the phase-change powder secondary adsorption method based on the metal oxide in the embodiment of the application has excellent heat absorption and temperature control performance, can effectively control the electronic equipment in the electronic encapsulating glue within a proper temperature, and cannot be overheated; meanwhile, the encapsulating material in the embodiment of the invention also comprises metal oxide as a second adsorption carrier, so that the phase-change powder overflowing from the phase-change substance is effectively adsorbed again, and the fluidity of the encapsulating material is increased, so that the filling density of the encapsulating material is improved when the encapsulating material is filled into a corresponding container.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without inventive effort.
Fig. 1 is a schematic flow chart of a secondary adsorption method of phase-change powder based on metal oxide in the embodiment of the invention.
Detailed Description
The present invention will be further described with reference to the following examples, which are preferred embodiments of the present invention.
Referring to fig. 1, an embodiment of a method for secondarily adsorbing phase-change powder based on metal oxide in the embodiment of the present application includes:
101. heating the first phase change material to 80-100 ℃ and stirring;
heating a first phase change material to 80-100 ℃ and stirring, wherein the first phase change material is a first adsorption carrier after adsorbing phase change powder, and the first adsorption carrier is graphite, aerogel or a capsule.
Specifically, the first adsorption carrier and the phase-change powder are mixed to obtain a first phase-change substance (i.e., a substance obtained after the phase-change powder is adsorbed for the first time). In the embodiment of the present application, the first phase change material may be a finished product directly obtained, or may be a material prepared by a manufacturer, and is not limited specifically here.
For example, the phase-change powder in the embodiment of the present application is selected from at least one of the following materials: paraffin waxes, fatty acids, PE waxes and PP waxes; the alkane wax has an alkane carbon number between 10 and 60.
For example, the first phase change material may be placed in a reaction kettle and heated to 80 to 100 degrees celsius, and the reaction kettle may be evacuated and stirred. The vacuum degree is between-0.04 and-0.10 Mpa, the vacuumizing time lasts for 5-40min, and the stirring time lasts for 15-90 min.
102. Adding a second adsorption carrier into the stirred first phase change material;
and adding a second adsorption carrier into the stirred first phase change material, wherein the second adsorption carrier is a metal oxide.
103. Heating the first phase change material added with the second adsorption carrier to 70-120 ℃, and stirring;
the heating temperature of the phase change material needs to be 20-60 ℃ higher than the phase change temperature, so the temperature range is generally set to be 70-120 ℃.
For example, step 103 may be performed by heating and then stirring, or by heating and stirring simultaneously.
For example, the first phase change material added with the second adsorption carrier can be placed in a planetary stirrer, and stirred for 30 to 60 minutes under the conditions that the speed is 30 revolutions per minute and the vacuum degree is between-0.04 and-0.10 MPa.
104. And cooling the first phase change material which is uniformly stirred and added with the second adsorption carrier to the normal temperature to obtain a second phase change material.
Further, since the second phase change material cooled to room temperature may have powder lumps, the second phase change material in step 104 may be pulverized and sieved with a 10 to 100 mesh sieve to obtain a second phase change material in powder form.
Wherein 5 to 20 parts of the first adsorption carrier are present per 100 parts by weight of the first phase change material; wherein 80 to 95 parts of the phase change powder exist in each 100 parts by weight of the first phase change material.
The second adsorption carrier is mixed with the first phase change material to obtain the second phase change material; wherein from 1 to 10 parts by weight of said second adsorbent carrier is present per 100 parts by weight of said second phase change material; wherein 90 to 99 parts of the first phase change material is present per 100 parts by weight of the second phase change material.
The secondary adsorption method of the phase-change powder based on the metal oxide in the embodiment of the application is obtained by carrying out secondary adsorption treatment after the first adsorption carrier adsorbs the phase-change powder for the first time. The second adsorption treatment in the present embodiment may be understood as "re-adsorption treatment", and may be a second adsorption, or may be a third or fourth adsorption, and is not particularly limited herein.
The encapsulating material treated by the phase-change powder secondary adsorption method based on the metal oxide in the embodiment of the application has excellent heat absorption and temperature control performance, can effectively control the electronic equipment in the electronic encapsulating glue within a proper temperature, and cannot be overheated; meanwhile, the encapsulating material in the embodiment of the invention also comprises metal oxide as a second adsorption carrier, so that the phase-change powder overflowing from the phase-change substance is effectively adsorbed again, and the fluidity of the encapsulating material is increased, so that the filling density of the encapsulating material is improved when the encapsulating material is filled into a corresponding container.
The following describes the main concepts and functional scenarios adapted by different materials in the embodiments of the present application, including:
about an adsorption carrier
In actual use to the phase change powder, the phase change powder is likely to leak out in the potting material after changing from solid state to liquid, so, need adsorb the parcel through the adsorption carrier with the phase change powder, prevent overflowing of phase change powder.
In the present embodiment, at least two kinds of adsorption carriers, respectively, a first adsorption carrier and a second adsorption carrier, are used. Wherein, the first adsorption carrier is a substance with stronger powder adsorption capacity, such as vermicular expanded graphite, aerogel or capsule, used in the first adsorption. The second adsorption carrier is a substance having a relatively heavy mass per unit volume used in the second adsorption. Wherein the metal oxide may include at least one of the following materials: aluminum oxide, aluminum nitride, magnesium oxide, magnesium hydroxide, aluminum hydroxide, copper oxide, and silicon oxide.
With respect to the second adsorption carrier
In the embodiment of the present application, the second adsorption carrier is selected according to the weight of the second adsorption carrier, in addition to the adsorption capacity of the phase-change powder. In practical application, the filling material is filled in a specific container, and the first phase change material in the prior art not only has the problem of overflowing phase change powder, but also has the problem of low filling density per unit volume stored in the container, mainly because the first phase change material is a light fluid material (such as toothpaste), and when the container is filled and sealed, the container cannot be effectively filled with the thick and light characteristic, so that the enthalpy per unit volume in the container is not high.
In the embodiment of the application, the second adsorption carrier selects the metal oxide which is a substance with heavier mass, so that the flowability of the encapsulating material is increased, the inner space of the container can be filled as much as possible during encapsulating in the container, the density of the encapsulating material in the container is increased, and the enthalpy value of the unit volume in the container is increased.
The following illustrates the increase in enthalpy per unit volume in the container:
assuming that the first phase change material is 100 parts by mass, wherein the first adsorption carrier and the phase change powder are respectively 10 parts and 90 parts (the proportion of the phase change powder in the first phase change material is 0.9); when 5 parts by mass of the second adsorption carrier is added in the second adsorption, the proportion of the phase change powder in the second phase change material is about 0.857.
In practical applications, a container with a unit volume of 100 can be filled with less than 90 parts of the first phase change material, that is, the container with the unit volume of 100 contains 81 parts of the phase change powder. The phase-change material can be filled with a second phase-change material with a unit volume of at least 99, namely, a container with a unit volume of 100, and contains about 84.84 parts of phase-change powder. Therefore, the enthalpy value per unit volume in the container when the second phase change material is used is higher than the enthalpy value per unit volume in the container when the first phase change material is used.
With respect to the first adsorption carrier
In the embodiment of the application, vermicular expanded graphite can be used as a first adsorption carrier, and is a loose and porous vermicular substance obtained by intercalating, washing, drying and high-temperature expanding natural crystalline flake graphite, wherein the vermicular expanded graphite has the excellent performances of cold and heat resistance, corrosion resistance, self-lubrication, radiation resistance, conductivity and the like of the natural graphite, and also has the characteristics of softness, compression resilience, adsorbability, ecological environment harmony, biocompatibility, radiation resistance and the like which are not possessed by the natural graphite; the worm-shaped expanded graphite cannot be too much, so that the cost is increased and the enthalpy value of the product is reduced on the one hand, meanwhile, the phase change enthalpy of the graphite adsorption phase change energy storage powder is reduced, and the heat storage performance of the product is reduced, therefore, the weight ratio of the graphite adsorption phase change energy storage powder to different powder is optimal.
Illustratively, if the adsorbent support is graphite, the graphite is vermicular expanded graphite; 99 to 99.5 parts of the phase change powder exists in each 100 parts by weight of the second phase change material; from 0.5 to 1 part by weight of said vermicular expanded graphite per 100 parts by weight of said second phase change material; the expansion rate of the vermicular expanded graphite is 100-600ml/g, the granularity is 100-200 meshes, the expansion multiple is 200-600 times, and the bulk density is 0.2-0.5 g/cm3。
In the embodiment of the application, aerogel can also be selected as the first adsorption carrier, the aerogel has a low heat conductivity coefficient, a good heat insulation effect, stable physicochemical property, high-temperature non-combustibility, complete water resistance, no toxicity, environmental friendliness, a large specific surface area and very strong adsorption capacity to the phase-change powder, and the second phase-change substance can be adsorbed only by adopting a small amount of aerogel by weight, however, the aerogel cannot be too little and cannot be completely adsorbed; the aerogel also can not be too many, if too many increases the weight of cost and product on the one hand, simultaneously, has reduced the phase transition enthalpy that the aerogel adsorbs phase transition energy storage powder, has reduced the heat-retaining property of product, consequently, to different phase transition powder, the weight ratio that can adsorb phase transition powder completely just is the optimum.
Illustratively, if the adsorption carrier is aerogel, 50 to 90 parts by weight of the phase-change powder is present per 100 parts by weight of the second phase-change material; 10 to 50 parts of said aerogel per 100 parts by weight of said second phase change material; the aerogel has the specific surface area of 100 square meters per gram and the particle size of 5-60 nm.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A secondary adsorption method of phase-change powder based on metal oxide is characterized by comprising the following steps:
s1, heating a first phase change material to 80-100 ℃, and stirring, wherein the first phase change material is a first adsorption carrier after adsorbing phase change powder, and the first adsorption carrier is graphite, aerogel or capsule;
s2, adding a second adsorption carrier into the stirred first phase change material, wherein the second adsorption carrier is a metal oxide;
s3, heating the first phase change material added with the second adsorption carrier to 70-120 ℃, and stirring;
and S4, cooling the first phase change material which is uniformly stirred and added with the second adsorption carrier to normal temperature to obtain a second phase change material.
2. The secondary adsorption method of phase-change powder based on metal oxide as claimed in claim 1, wherein after obtaining the second phase-change material, the method comprises:
s5, the second phase change material in the step S4 is pulverized.
3. The method for secondarily adsorbing the phase-change powder based on the metal oxide as recited in claim 2, wherein after the step of pulverizing the second phase-change material in the step S4, the method comprises:
s6, sieving the second phase change material processed in step S5 to obtain a second phase change material in powder form.
4. The method for secondarily adsorbing the phase-change powder based on the metal oxide as recited in claim 1, wherein the stirring in the step S3 includes:
and (3) placing the first phase change material added with the second adsorption carrier into a planetary stirrer, and stirring at the speed of 30 revolutions per minute and under the condition that the vacuum degree is between-0.04 and-0.10 Mpa.
5. The method for secondarily adsorbing the phase-change powder based on the metal oxide as recited in claim 4, wherein the stirring in the step S3 further comprises: the stirring time is 30 to 60 minutes.
6. The secondary adsorption method of phase-change powder based on metal oxide as claimed in claim 1, wherein the heating and stirring of the first phase-change material to 80-100 ℃ comprises:
and (3) placing the first phase change material in a reaction kettle, heating to 80-100 ℃, vacuumizing the reaction kettle, and stirring.
7. The secondary adsorption method of phase-change powder based on metal oxide as claimed in claim 6, wherein the degree of vacuum is between-0.04 and-0.10 MPa, the duration of vacuum pumping is 5-40min, and the duration of stirring is 15-90 min.
8. The secondary adsorption method of phase-change powder based on metal oxide as claimed in claim 1,
from 5 to 20 parts of said first adsorption carrier per 100 parts by weight of said first phase change material;
80 to 95 parts of the phase change powder exist in each 100 parts by weight of the first phase change material.
9. The secondary adsorption method of phase-change powder based on metal oxide as claimed in claim 8,
from 1 to 10 parts by weight of said second adsorbent carrier per 100 parts by weight of said second phase change material; from 90 to 99 parts of said first phase change material per 100 parts by weight of said second phase change material.
10. The secondary adsorption method of phase-change powder based on metal oxide as claimed in claim 1, wherein the metal oxide comprises at least one of the following materials:
aluminum oxide, aluminum nitride, copper oxide, and silicon oxide.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20140032793A (en) * | 2012-09-07 | 2014-03-17 | 한국과학기술연구원 | Polymer composite material having high thermal conductivity and manufacturing method thereof |
| CN110317578A (en) * | 2019-07-03 | 2019-10-11 | 张立强 | Phase-change thermal storage silica gel, preparation method and applications |
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2020
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20140032793A (en) * | 2012-09-07 | 2014-03-17 | 한국과학기술연구원 | Polymer composite material having high thermal conductivity and manufacturing method thereof |
| CN110317578A (en) * | 2019-07-03 | 2019-10-11 | 张立强 | Phase-change thermal storage silica gel, preparation method and applications |
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| 仝仓等: "聚乙二醇/二氧化硅/膨胀石墨相变储能材料的制备与性能研究", 《区域供热》 * |
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