CN115305068B - Preparation method of long-acting heat dissipation liquid for automobile - Google Patents

Preparation method of long-acting heat dissipation liquid for automobile Download PDF

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CN115305068B
CN115305068B CN202211121019.2A CN202211121019A CN115305068B CN 115305068 B CN115305068 B CN 115305068B CN 202211121019 A CN202211121019 A CN 202211121019A CN 115305068 B CN115305068 B CN 115305068B
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CN115305068A (en
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刘雨修
王永刚
王丽丽
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Tapoa Technology Co ltd
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    • C09K5/00Heat-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
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Abstract

The invention discloses a preparation method of a long-acting heat dissipation liquid for an automobile, which belongs to the technical field of engine heat dissipation liquid. The heat dissipation liquid prepared by the invention has low freezing point and high boiling point, is suitable for being used in extreme environments, has the freezing point of-75 to-76 ℃ and the boiling point of 126 to 128 ℃, has stable heat conductivity coefficient at different temperatures, and can keep high heat conductivity coefficient at low temperature.

Description

Preparation method of long-acting heat dissipation liquid for automobile
Technical Field
The invention relates to a preparation method of a long-acting heat dissipation liquid for an automobile, and belongs to the technical field of engine heat dissipation liquids.
Background
The engine cooling liquid is a working medium of an engine cooling system, is mainly used for taking away heat generated in the working process of the engine, is a liquid for ensuring the normal operation of the engine, and has higher and higher performance requirements on the cooling liquid, low freezing point, high boiling point, good heat transfer performance, good corrosion resistance and environment-friendly long-acting high-performance cooling liquid along with the increase of the power density of the engine and the increase of the load of a heated part, the upgrading and heat exchange strength of the cooling system, and has wide market prospect, so that the research of the high-performance cooling liquid is developed, and the development of the market and the engine is very necessary.
In order to maintain the heat dissipation performance of the engine under the working conditions of high temperature and high strength, the heat dissipation liquid is required to have a high boiling point, the highest boiling point of the heat dissipation liquid consisting of glycol and water is increased to 107 ℃ at present, the increasingly strict engine requirements are difficult to meet, the nano fluid heat dissipation liquid is widely researched, nano fluid heat dissipation liquid is prepared by adding nano metal particles into a heat dissipation liquid component, the heat conduction efficiency can be improved, the boiling point of the heat dissipation liquid is improved, the heat dissipation liquid containing nano aluminum oxide and propylene glycol component can be higher than 120 ℃.
Researches show that when the addition amount of the nano aluminum oxide is 1-2wt%, the optimal performance of the heat dissipation liquid can be maintained, the heat transfer coefficient is highest, and if the content of the nano aluminum oxide is increased, the viscosity of the heat dissipation liquid is increased, so that the heat transfer coefficient is reduced, and the addition amount of 1-2wt% is ensured to be most proper.
The applicant also found that the heat dissipation liquid containing the nano aluminum oxide and the propylene glycol component has lower heat conductivity coefficient in the temperature range of 50-90 ℃ under the condition of lower temperature, which indicates that the physical property of the cooling liquid is greatly influenced by the temperature, and the heat conductivity coefficient can reach higher level when the temperature rises to more than 100 ℃, so that the heat dissipation liquid containing the nano aluminum oxide and the propylene glycol component can not ensure good heat dissipation effect when the temperature is lower.
In summary, in the prior art, the heat dissipation liquid containing nano aluminum oxide and propylene glycol components has a low thermal conductivity when the temperature is low.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and further prepares the heat dissipation liquid with the propylene glycol as the main component by performing a series of treatments on the nano aluminum oxide, so as to improve the heat conductivity coefficient of the heat dissipation liquid at a lower temperature.
In order to solve the technical problems, the invention adopts the following technical scheme:
the preparation method comprises the steps of preparing ferric oxide composite nano aluminum oxide, adhering silicon dioxide on the surface, calcining to prepare nano fluid medium and preparing the heat dissipation liquid.
The following is a further improvement of the above technical scheme:
mixing ferric trichloride solution and nano alumina, stirring for 13-17min, controlling the temperature to be 91-95 ℃ after stirring, drying until no water exists, obtaining mixed powder, controlling the temperature to be 355-385 ℃, performing high-temperature treatment under the protection of nitrogen for 185-215min, and cooling to obtain the ferric oxide composite nano alumina;
the mass ratio of the ferric trichloride solution to the nano-alumina is 14-16:4;
the mass concentration of the ferric trichloride solution is 8.2-8.7%;
the particle size of the nano alumina is 60-70nm;
mixing and stirring iron oxide composite nano alumina, deionized water and sodium polyacrylate to obtain uniformly dispersed dispersion liquid, adding tetramethoxysilane, stirring for 20-30min, adding ammonia water, continuously stirring for 140-160min, filtering and drying to obtain iron oxide composite nano alumina with surface adhered with silicon dioxide;
the mass ratio of the ferric oxide composite nano aluminum oxide to the deionized water to the sodium polyacrylate to the tetramethoxysilane to the ammonia water is 85-115:710-790:80-90:24-31:3.5-4.5;
the mass concentration of the ammonia water is 14-16%;
the method for preparing the nano fluid medium by calcining comprises the steps of controlling the temperature to 182-189 ℃, calcining the iron oxide composite nano alumina with silicon dioxide adhered on the surface under the protection of nitrogen for 87-95min, adjusting the temperature to 220-230 ℃, continuously calcining for 70-80min, and cooling to obtain the nano fluid medium.
The method for preparing the heat dissipation liquid comprises the steps of mixing half of propylene glycol, sebacic acid, succinic acid, sodium benzoate, sodium molybdate, benzotriazole and sodium petroleum sulfonate, stirring for 13-18min, adding the rest propylene glycol, adding deionized water, nano fluid medium and dimethyl silicone oil, stirring for 23-28min, carrying out ultrasonic treatment at 27-35kHz frequency for 6-12min after stirring, and standing after ultrasonic treatment to obtain the heat dissipation liquid;
the raw materials of the heat dissipation liquid comprise the following components in parts by mass: 60-70 parts of propylene glycol, 32-37 parts of deionized water, 1.8-2.2 parts of nano fluid medium, 0.5-0.7 part of sebacic acid, 0.15-0.25 part of succinic acid, 0.04-0.06 part of dimethyl silicone oil, 0.75-0.95 part of sodium benzoate, 0.32-0.37 part of sodium molybdate, 0.11-0.13 part of benzotriazole and 0.13-0.17 part of petroleum sodium sulfonate.
Compared with the prior art, the invention has the following beneficial effects:
the heat dissipation liquid prepared by the invention has low freezing point and high boiling point, is suitable for being used in a limiting environment, and has the freezing point of-75 to-76 ℃ and the boiling point of 126 to 128 ℃;
the heat dissipation liquid prepared by the invention has stable heat conduction coefficient at different temperatures, can keep high heat conduction coefficient at low temperature, has the heat conduction coefficient of 0.481-0.485W/(m.K) at 30 ℃, the heat conduction coefficient of 0.467-0.471W/(m.K) at 40 ℃, the heat conduction coefficient of 0.452-0.455W/(m.K) at 50 ℃, the heat conduction coefficient of 0.452-0.454W/(m.K) at 60 ℃, the heat conduction coefficient of 0.446-0.448W/(m.K) at 70 ℃, the heat conduction coefficient of 0.458-0.460W/(m.K) at 80 ℃, the heat conduction coefficient of 0.484-0.491W/(m.K) at 90 ℃, the heat conduction coefficient of 0.502-0.505W/(m.K) at 100 ℃, and the heat conduction coefficient of 0.515-0.519W/(m.K) at 120 ℃.
The prepared heat dissipation liquid has low corrosiveness, in a simulated corrosion test, the corrosiveness to red copper is +0.3- +0.5mg, the corrosiveness to brass is +0.4- +0.7mg, the corrosiveness to steel is-0.3-0.5 mg, the corrosiveness to cast iron is-0.8-0.9 mg, the corrosiveness to tin soldering is +1.4- +1.7mg, and the corrosiveness to cast aluminum is-1.2-1.5 mg;
the heat dissipation liquid prepared by the invention has good heat transfer corrosion resistance, and in the heat transfer corrosion test of the cast aluminum alloy, the heat transfer corrosion quality of the cast aluminum alloy is changed to-0.1 mg/cm 2
The heat dissipation liquid prepared by the invention has good cavitation corrosion resistance, and in the cavitation corrosion test of the aluminum pump, the corrosion resistance grade is 9-10.
Detailed Description
Example 1
(1) Preparation of iron oxide composite nano alumina
Mixing ferric trichloride solution and nano alumina, stirring for 15min, controlling the temperature to 92 ℃ after stirring, drying until no water exists, obtaining mixed powder, controlling the temperature to 375 ℃, performing high-temperature treatment under the protection of nitrogen for 195min, and cooling to obtain the iron oxide composite nano alumina;
the mass ratio of the ferric trichloride solution to the nano-alumina is 15:4;
the mass concentration of the ferric trichloride solution is 8.5%;
the particle size of the nano alumina is 65nm;
(2) Surface-adhered silica
Mixing and stirring iron oxide composite nano alumina, deionized water and sodium polyacrylate to obtain uniformly dispersed dispersion liquid, then adding tetramethoxysilane, stirring for 25min, then adding ammonia water, continuing stirring for 150min, filtering and drying to obtain iron oxide composite nano alumina with silica adhered on the surface;
the mass ratio of the ferric oxide composite nano aluminum oxide to the deionized water to the sodium polyacrylate to the tetramethoxysilane to the ammonia water is 100:750:85:27:4;
the mass concentration of the ammonia water is 15%.
(3) Calcination to prepare nanofluidic media
And (3) controlling the temperature to be 185 ℃, calcining the iron oxide composite nano alumina with the silicon dioxide adhered on the surface under the protection of nitrogen for 90min, then adjusting the temperature to be 225 ℃, continuously calcining for 75min, and cooling to obtain the nano fluid medium.
(4) Preparing a heat dissipation liquid
The raw materials of the heat dissipation liquid comprise the following components in parts by mass: 65 parts of propylene glycol, 35 parts of deionized water, 2 parts of nano fluid medium, 0.6 part of sebacic acid, 0.2 part of succinic acid, 0.05 part of simethicone, 0.85 part of sodium benzoate, 0.35 part of sodium molybdate, 0.12 part of benzotriazole and 0.15 part of petroleum sodium sulfonate;
and mixing half of the propylene glycol, sebacic acid, succinic acid, sodium benzoate, sodium molybdate, benzotriazole and sodium petroleum sulfonate, stirring for 15min, adding the rest propylene glycol, adding deionized water, a nanofluidic medium and dimethyl silicone oil, stirring for 25min, performing ultrasonic treatment at 30kHz frequency, performing ultrasonic treatment for 7min, and standing after ultrasonic treatment to obtain the heat dissipation liquid.
Example 2
(1) Preparation of iron oxide composite nano alumina
Mixing ferric trichloride solution and nano alumina, stirring for 13min, controlling the temperature to be 91 ℃ after stirring, drying until no water exists, obtaining mixed powder, controlling the temperature to be 355 ℃, performing high-temperature treatment under the protection of nitrogen for 215min, and cooling to obtain the iron oxide composite nano alumina;
the mass ratio of the ferric trichloride solution to the nano-alumina is 14:4;
the mass concentration of the ferric trichloride solution is 8.2%;
the particle size of the nano alumina is 60nm;
(2) Surface-adhered silica
Mixing and stirring iron oxide composite nano alumina, deionized water and sodium polyacrylate to obtain uniformly dispersed dispersion liquid, then adding tetramethoxysilane, stirring for 20min, then adding ammonia water, continuing stirring for 160min, filtering and drying to obtain iron oxide composite nano alumina with silica adhered on the surface;
the mass ratio of the ferric oxide composite nano aluminum oxide to the deionized water to the sodium polyacrylate to the tetramethoxysilane to the ammonia water is 85:710:80:24:3.5;
the mass concentration of the ammonia water is 14%.
(3) Calcination to prepare nanofluidic media
And (3) controlling the temperature to 182 ℃, calcining the iron oxide composite nano alumina with the silicon dioxide adhered on the surface under the protection of nitrogen for 95min, then adjusting the temperature to 220 ℃, continuously calcining for 80min, and cooling to obtain the nano fluid medium.
(4) Preparing a heat dissipation liquid
The raw materials of the heat dissipation liquid comprise the following components in parts by mass: 60 parts of propylene glycol, 32 parts of deionized water, 1.8 parts of nano fluid medium, 0.5 part of sebacic acid, 0.15 part of succinic acid, 0.04 part of simethicone, 0.75 part of sodium benzoate, 0.32 part of sodium molybdate, 0.11 part of benzotriazole and 0.13 part of sodium petroleum sulfonate;
and mixing half of the propylene glycol, sebacic acid, succinic acid, sodium benzoate, sodium molybdate, benzotriazole and sodium petroleum sulfonate, stirring for 13min, adding the rest propylene glycol, adding deionized water, a nanofluidic medium and dimethyl silicone oil, stirring for 28min, performing ultrasonic treatment at 27kHz frequency after stirring for 12min, and standing after ultrasonic treatment to obtain the heat dissipation liquid.
Example 3
(1) Preparation of iron oxide composite nano alumina
Mixing ferric trichloride solution and nano alumina, stirring for 17min, controlling the temperature to be 95 ℃ after stirring, drying until no water exists, obtaining mixed powder, controlling the temperature to be 385 ℃, performing high-temperature treatment under the protection of nitrogen for 185min, and cooling to obtain the iron oxide composite nano alumina;
the mass ratio of the ferric trichloride solution to the nano-alumina is 16:4;
the mass concentration of the ferric trichloride solution is 8.7%;
the particle size of the nano alumina is 70nm;
(2) Surface-adhered silica
Mixing and stirring iron oxide composite nano alumina, deionized water and sodium polyacrylate to obtain uniformly dispersed dispersion liquid, then adding tetramethoxysilane, stirring for 30min, then adding ammonia water, continuing stirring for 140min, filtering and drying to obtain iron oxide composite nano alumina with silica adhered on the surface;
the mass ratio of the ferric oxide composite nano aluminum oxide to the deionized water to the sodium polyacrylate to the tetramethoxysilane to the ammonia water is 115:790:90:31:4.5;
the mass concentration of the ammonia water is 16%.
(3) Calcination to prepare nanofluidic media
The temperature is controlled to be 189 ℃, under the protection of nitrogen, the iron oxide composite nano alumina with silicon dioxide adhered on the surface is calcined for 87min, then the temperature is adjusted to be 230 ℃, the calcination is continued for 70min, and the nano fluid medium is obtained after cooling.
(4) Preparing a heat dissipation liquid
The raw materials of the heat dissipation liquid comprise the following components in parts by mass: 70 parts of propylene glycol, 37 parts of deionized water, 2.2 parts of nano fluid medium, 0.7 part of sebacic acid, 0.25 part of succinic acid, 0.06 part of simethicone, 0.95 part of sodium benzoate, 0.37 part of sodium molybdate, 0.13 part of benzotriazole and 0.17 part of petroleum sodium sulfonate;
mixing half mass of propylene glycol, sebacic acid, succinic acid, sodium benzoate, sodium molybdate, benzotriazole and sodium petroleum sulfonate, stirring for 18min, adding the rest propylene glycol, adding deionized water, a nanofluidic medium and dimethyl silicone oil, stirring for 23min, performing ultrasonic treatment at 35kHz frequency, performing ultrasonic treatment for 6min, and standing after ultrasonic treatment to obtain the heat dissipation liquid.
Comparative example 1
On the basis of the embodiment 1, the step of preparing the ferric oxide composite nano aluminum oxide is omitted, the nano iron oxide and the nano aluminum oxide are mixed and then ground to obtain mixed powder, in the step of adhering silicon dioxide on the surface, the mixed powder is subjected to surface adhesion, and the rest steps are the same, so that the heat dissipation liquid is prepared;
the mass ratio of the nano iron oxide to the nano aluminum oxide is 1:5;
the particle size of the nano ferric oxide is 40nm;
the particle size of the nano alumina is 65nm.
Comparative example 2
On the basis of the embodiment 1, in the step of preparing the ferric oxide composite nano aluminum oxide, after mixed powder is obtained, the temperature is controlled to be 200 ℃, high-temperature treatment is carried out for 300min under the protection of nitrogen, then the ferric oxide composite nano aluminum oxide is obtained through cooling, and the rest steps are the same, so that the heat dissipation liquid is prepared.
Comparative example 3
On the basis of the embodiment 1, in the step of adhering silica on the surface, mixing and grinding the ferric oxide composite nano alumina and the nano silica to obtain the ferric oxide composite nano alumina with the silica adhered on the surface, and preparing a heat dissipation liquid in the same steps;
the mass ratio of the ferric oxide composite nano aluminum oxide to the nano silicon dioxide is 100:55;
the particle size of the nano silicon dioxide is 25nm.
Example 4 freezing point boiling Point test of Heat sink
The heat sinks prepared in examples 1 to 3 and comparative examples 1 to 3 were tested for freezing point and boiling point, respectively, and the results are shown in Table 1.
In the comparative example 1, nano iron oxide and nano aluminum oxide are mixed and then ground, instead of uniformly coating the nano iron oxide on the surface of the nano aluminum oxide, the finally prepared cooling liquid has a higher freezing point;
in comparative example 2, after the mixed powder is obtained, the temperature is controlled to be 200 ℃, high-temperature treatment is carried out under the protection of nitrogen, the treatment time is 300min, the treatment temperature is reduced, and the treatment time is increased, so that the combination of nano-iron oxide and nano-aluminum oxide is slightly influenced, but the influence on the freezing point boiling point is small;
in the step of adhering silica to the surface, comparative example 3, iron oxide composite nano alumina and nano silica were mixed and ground, and the combination of both was poor, so that the boiling point was reduced more.
Example 5 Heat conductivity coefficient test of Heat dissipating liquid at different temperatures
The engine radiator fluids prepared in examples 1 to 3 and comparative examples 1 to 3 were tested for thermal conductivity at 30℃C, 40℃C, 50℃C, 60℃C, 70℃C, 80℃C, 90℃C, 100℃C and 120℃C, respectively, using a thermal conductivity tester, and the results are shown in Table 2.
Comparative example 1 nano iron oxide and nano aluminum oxide are mixed and then ground, instead of uniformly coating the nano iron oxide on the surface of the nano aluminum oxide, the heat conductivity of the finally prepared heat dissipation liquid is seriously reduced at a low temperature, particularly in the range of 40-90 ℃, wherein the heat dissipation liquid is most seriously in the range of 60-80 ℃;
in comparative example 2, after the mixed powder is obtained, the temperature is controlled to be 200 ℃, high-temperature treatment is carried out under the protection of nitrogen, the treatment time is 300min, the treatment temperature is reduced, and the treatment time is increased, so that the combination of nano iron oxide and nano aluminum oxide is slightly influenced, but the influence on the heat conductivity is small, and the degree of the reduction of the heat conductivity at low temperature is small;
in the step of adhering silica to the surface, in comparative example 3, iron oxide composite nano alumina and nano silica are mixed and ground, the combination of the two is poor, the heat conductivity coefficient is affected to a certain extent, and the heat conductivity coefficient at low temperature is slightly reduced.
Example 6 other Performance test of Heat dissipating liquid
The engine cooling liquid prepared in the examples 1-3 and the comparative examples 1-3 is subjected to a simulated corrosion test according to the test method in GB 29743-2013 motor vehicle engine cooling liquid, the test temperature is 88 ℃, the test time is 1064h, and the results are shown in Table 3; carrying out heat transfer corrosion test on the cast aluminum alloy, wherein the test temperature is 135 ℃, and the test time is 168 hours, and the results are shown in Table 4; the aluminum pump cavitation corrosion test was conducted at 113℃for 100 hours and 103kPa for the results shown in Table 5.

Claims (1)

1. The preparation method of the long-acting heat dissipation liquid for the automobile is characterized by comprising the steps of preparing iron oxide composite nano aluminum oxide, adhering silicon dioxide on the surface, calcining to prepare nano fluid medium and preparing heat dissipation liquid;
mixing ferric trichloride solution and nano alumina, stirring for 13-17min, drying after stirring, wherein the drying temperature is 91-95 ℃, drying until no water exists to obtain mixed powder, controlling the temperature to 355-385 ℃, performing high-temperature treatment under the protection of nitrogen for 185-215min, and cooling to obtain the ferric oxide composite nano alumina;
the mass concentration of the ferric trichloride solution is 8.2-8.7%, and the particle size of the nano aluminum oxide is 60-70nm;
the mass ratio of the ferric trichloride solution to the nano-alumina is 14-16:4;
mixing and stirring iron oxide composite nano alumina, deionized water and sodium polyacrylate to obtain uniformly dispersed dispersion liquid, adding tetramethoxysilane, stirring for 20-30min, adding ammonia water, continuously stirring for 140-160min, filtering and drying to obtain iron oxide composite nano alumina with surface adhered with silicon dioxide;
the mass ratio of the ferric oxide composite nano aluminum oxide to the deionized water to the sodium polyacrylate to the tetramethoxysilane to the ammonia water is 85-115:710-790:80-90:24-31:3.5-4.5;
the mass concentration of the ammonia water is 14-16%;
the method for preparing the nano fluid medium by calcination comprises the steps of controlling the temperature to 182-189 ℃, calcining the iron oxide composite nano alumina with silicon dioxide adhered on the surface under the protection of nitrogen for 87-95min, adjusting the temperature to 220-230 ℃, continuously calcining for 70-80min, and cooling to obtain the nano fluid medium;
the method for preparing the heat dissipation liquid comprises the steps of mixing half mass of propylene glycol, sebacic acid, succinic acid, sodium benzoate, sodium molybdate, benzotriazole and sodium petroleum sulfonate, stirring, adding the rest propylene glycol, adding deionized water, nano fluid medium and dimethyl silicone oil, stirring, performing ultrasonic treatment after stirring, wherein the ultrasonic frequency is 27-35kHz, the ultrasonic time is 6-12min, and standing to obtain the heat dissipation liquid;
the raw materials of the heat dissipation liquid comprise the following components in parts by mass: 60-70 parts of propylene glycol, 32-37 parts of deionized water, 1.8-2.2 parts of nano fluid medium, 0.5-0.7 part of sebacic acid, 0.15-0.25 part of succinic acid, 0.04-0.06 part of dimethyl silicone oil, 0.75-0.95 part of sodium benzoate, 0.32-0.37 part of sodium molybdate, 0.11-0.13 part of benzotriazole and 0.13-0.17 part of petroleum sodium sulfonate.
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