CN115058129A - Preparation method and application of functional micro powder for engine coolant - Google Patents
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Abstract
The invention provides a preparation method and application of functional micro powder for engine coolant, wherein the preparation method of the functional micro powder for the engine coolant comprises the following steps: s1, degrading fiber, and sequentially carrying out acidolysis and alkaline hydrolysis on the dried and crushed plant raw materials to prepare oligosaccharide solution; s2, Al 2 O 3 Coating carbon, and coating oligosaccharide obtained in step S1 with aluminum oxide to obtain C-Al 2 O 3 Micro-powder; s3, C-Al 2 O 3 Nickel-clad, C-Al of step S2 2 O 3 The micro powder is modified by nickel salt to obtain C-Al 2 O 3 -Ni micropowder. The functional micropowder has larger specific surface area and void volume and higher thermal conductivity. The nanometer cooling liquid prepared by the functional micro powder is suitable for the operating condition of less than or equal to 120 DEG CThe limit working temperature of the engine nano cooling liquid is about 15 ℃ higher than that of the traditional antifreezing solution, and the problem of high-temperature overheating of the engine is solved.
Description
Technical Field
The invention relates to the technical field of cooling liquid, in particular to a preparation method and application of functional micro powder for engine cooling liquid.
Background
The traditional water-polyol or all-organic engine coolant has the overheating problem and cannot meet the rapid cooling requirement of high-power heat source bodies such as diesel engines, turbine engines and the like. Although the nano fluid coolant has more excellent heat exchange capacity, the nano particles can generate agglomeration and precipitation at high temperature and cannot be used for cooling an engine, so the nano fluid coolant can only be used as a heat exchanger of a medium-low temperature heat source, such as a Hydromx @ series nano fluid heat exchanger, and is often used as a cold storage coolant and a domestic heating agent. Therefore, it is necessary to develop a functional fine powder having high thermal dispersibility and thermal conductivity and suitable for a high-temperature engine coolant.
Disclosure of Invention
In view of the above, the invention provides a preparation method and application of a functional micro powder which has high heat dispersibility and heat conductivity and is suitable for a high-temperature engine coolant.
The technical scheme of the invention is realized as follows: the invention provides a preparation method of functional micro powder for engine coolant, which comprises the following steps:
s1, degrading the fiber, and sequentially carrying out acidolysis and alkaline hydrolysis on the dried and crushed plant raw material to prepare an oligosaccharide solution;
S2，Al 2 O 3 coating carbon, and coating oligosaccharide obtained in step S1 with aluminum oxide to obtain C-Al 2 O 3 Micro-powder;
S3，C-Al 2 O 3 nickel cladding, C-Al of step S2 2 O 3 The micro powder is modified by nickel salt to obtain C-Al 2 O 3 -Ni micropowder.
On the basis of the above technical solution, preferably, the acidolysis method of step S1 is: soaking the plant raw materials in 1% sulfuric acid solution for 0.5-1h for acidolysis for 15-30min, filtering, leaching the filtrate with tap water, transferring into 2.5% NaOH solution for alkaline hydrolysis for 15-30min, filtering again, leaching the filtrate with tap water, transferring into 80% phosphoric acid solution, ultrasonically oscillating, centrifuging, and removing residue to obtain oligosaccharide solution.
On the basis of the technical scheme, the preferable mass ratio of the plant raw materials to sulfuric acid to NaOH to phosphoric acid is (10-15): (20-31): (18-23).
On the basis of the technical scheme, preferably, the plant raw material is one of straw, corncob, corn stalk and wheat stalk.
Based on the above technical solution, the coating method in step S2 preferably includes: mixing the oligosaccharide solution obtained in the step S1 with Al 2 O 3 Mixing the powders, filtering, and calcining the filtrate at 450 + -5 deg.C for 3-4h to obtain C-Al 2 O 3 And (5) micro-powder.
On the basis of the above technical solution, preferably, the alumina powder: the mass ratio of the oligosaccharide solution is 1:4, and the particle size of the alumina powder is less than or equal to 100 nm.
Based on the above technical solution, the coating method in step S3 preferably includes: mixing nickel salt, citric acid and 50% phosphoric acid solution, and adding C-Al of step S2 2 O 3 Stirring the micro powder uniformly, heating to 60-70 ℃, and filtering; evaporating the filtrate to dry the surface of the material, and then roasting at 600 + -5 deg.C for 2-3h to obtain C-Al 2 O 3 -Ni micropowder.
On the basis of the technical scheme, preferably, the nickel salt is citric acid, phosphoric acid solution is C-Al 2 O 3 The mass ratio of the micro powder is (4-6): (0.5-1): (80-90): (9-12).
On the basis of the above technical scheme, preferably, the nickel salt is nickel sulfate or nickel nitrate.
The invention also provides application of the functional micro powder in preparing the nano cooling liquid or the nano fluid heat exchange agent, and the functional micro powder is prepared by the preparation method.
Compared with the prior art, the preparation method and the application of the functional micro powder for the engine coolant have the following beneficial effects:
the functional micropowder of the invention has larger specific surface area and void volume and higher thermal conductivity. The nano cooling liquid prepared from the functional micro powder is suitable for the engine nano cooling liquid with the operating condition of less than or equal to 120 ℃, the limit working temperature is about 15 ℃ higher than that of the traditional polyhydric alcohol antifreeze liquid, and the nano cooling liquid is suitable for power systems such as diesel engines, gasoline engines, gas turbines, turbine engines, generators, motors and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a nanostructure diagram of the functional fine powder of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example one
The preparation method of the functional micro powder comprises the following steps:
s1, degrading fibers, immersing 10 parts of dried and crushed straws in 20 parts of sulfuric acid solution with the volume fraction of 1% in a reactor for 0.5h, heating to boil, keeping the temperature for 15min, taking out and filtering; leaching the filtrate with tap water until the pH value is 7, transferring the filtrate into a reactor which is pre-filled with 20 parts of NaOH solution with the volume fraction of 2.5%, heating to boil, stirring at constant temperature for 15min at the rotating speed of 60 r/min, taking out and filtering; leaching the filtrate with tap water until the pH value is 7, transferring the filtrate into an ultrasonic reactor in which 18 parts of phosphoric acid solution with the volume fraction of 80% is pre-filled, setting the power to be 10KW, degrading the filtrate by ultrasonic oscillation for 2 hours, transferring the degraded filtrate into a centrifugal machine, centrifuging the degraded filtrate for 20 minutes at the speed of 3000 r/min, and removing residues to obtain the hydrolyzed sugar solution.
S2，Al 2 O 3 Coating carbon, mixing 20 parts of alumina powder (particle size is less than or equal to 100nm) and 80 parts of hydrolyzed sugar solution in a reactor, stirring at normal temperature for 20min at the rotating speed of 60 r/min, and takingFiltering and discarding the solution. The filtered substance is placed in a muffle furnace at the temperature of 450 +/-5 ℃ to be roasted for 3 hours to prepare the light C-Al 2 O 3 And (5) micro-powder.
S3，C-Al 2 O 3 Nickel coating, mixing 4 parts of nickel sulfate, 0.5 part of citric acid and 80 parts of phosphoric acid solution with volume fraction of 50% in a reaction kettle, stirring and dissolving at normal temperature till complete, and then adding 9 parts of C-Al 2 O 3 Stirring the micropowder uniformly, heating to 60 deg.C, holding the temperature for 30min, standing, cooling, filtering, and discarding the solution. Transferring the filtrate into a reduced pressure evaporator, evaporating at 60 + -2 deg.C under negative pressure until the surface of the material is dry, placing in a muffle furnace, and roasting at 600 + -5 deg.C for 2 hr to obtain C-Al 2 O 3 -Ni micropowder.
Example two
The preparation method of the functional micro powder comprises the following steps:
s1, degrading fibers, soaking 12 parts of dried and crushed plant raw material corn straws in 25 parts of sulfuric acid solution with the volume fraction of 1% in a reactor for 40min, heating to boil, keeping the temperature for 20min, taking out and filtering; leaching the filtrate with tap water until the pH value is 7, transferring the filtrate into a reactor which is pre-filled with 25 parts of NaOH solution with the volume fraction of 2.5%, heating to boil, stirring at constant temperature for 20min at the rotating speed of 70 r/min, taking out and filtering; leaching the filtrate with tap water until the pH value is 7, transferring the filtrate into an ultrasonic reactor in which 20 parts of phosphoric acid solution with the volume fraction of 80% is pre-filled, setting the power to be 10KW, degrading the filtrate by ultrasonic oscillation for 2 hours, transferring the degraded filtrate into a centrifugal machine, centrifuging the degraded filtrate for 20 minutes at the speed of 3000 r/min, and removing residues to obtain the hydrolyzed sugar solution.
S2，Al 2 O 3 Coating carbon, mixing 20 parts of alumina powder (the particle size is less than or equal to 100nm) and 80 parts of hydrolysis sugar solution in a reactor, stirring at normal temperature for 20min at the rotating speed of 70 r/min, taking out, filtering and discarding the solution. The filtrate is placed in a muffle furnace at the temperature of 450 +/-5 ℃ to be roasted for 3.5h, and the light C-Al is prepared 2 O 3 And (5) micro-pulverizing.
S3，C-Al 2 O 3 Nickel coating, mixing 5 parts of nickel nitrate, 0.7 part of citric acid and 85 parts of phosphoric acid solution with volume fraction of 50% in a reaction kettle, stirring and dissolving at normal temperature till completion, and then adding 10 parts of C-Al 2 O 3 Stirring the micropowder uniformly, heating to 35 deg.C, holding the temperature for 30min, standing, cooling, filtering, and discarding the liquid. Transferring the filtrate into a reduced pressure evaporator, evaporating at 60 + -2 deg.C under negative pressure until the surface of the material is dry, placing in a muffle furnace, and roasting at 600 + -5 deg.C for 2.5h to obtain C-Al 2 O 3 -Ni micropowder.
EXAMPLE III
The preparation method of the functional micro powder comprises the following steps:
s1, degrading fibers, soaking 15 parts of dried and crushed wheat straws in 31 parts of sulfuric acid solution with the volume fraction of 1% in a reactor for 1 hour, heating to boil, keeping the temperature for 30min, taking out and filtering; leaching the filtrate with tap water until the pH value is 7, transferring the filtrate into a reactor which is previously filled with 31 parts of NaOH solution with the volume fraction of 2.5%, heating the mixture to boiling, stirring the mixture at constant temperature for 30min at the rotating speed of 80 r/min, taking out the mixture and filtering the mixture; leaching the filtrate with tap water until the pH value is 7, transferring the filtrate into an ultrasonic reactor which is pre-filled with 23 parts of phosphoric acid solution with the volume fraction of 80%, setting the power to be 10KW, degrading the filtrate by ultrasonic oscillation for 2 hours, transferring the degraded filtrate into a centrifugal machine, centrifuging the degraded filtrate at a speed of 3000 r/min for 20min, and removing residues to obtain the hydrolyzed sugar solution.
S2，Al 2 O 3 Coating carbon, mixing 20 parts of alumina powder (the particle size is less than or equal to 100nm) and 80 parts of hydrolysis sugar solution in a reactor, stirring at normal temperature for 20min at the rotating speed of 80 r/min, taking out, filtering and discarding the solution. The filtered substance is placed in a muffle furnace at the temperature of 450 +/-5 ℃ to be roasted for 4 hours to prepare the light C-Al 2 O 3 And (5) micro-powder.
S3，C-Al 2 O 3 Nickel coating, mixing 6 parts of nickel sulfate, 1 part of citric acid and 90 parts of phosphoric acid solution with volume fraction of 50% in a reaction kettle, stirring and dissolving at normal temperature till completion, and then adding 12 parts of C-Al 2 O 3 Stirring the micropowder uniformly, heating to 70 deg.C, holding the temperature for 30min, standing, cooling, filtering, and discarding the solution. Transferring the filtrate into a reduced pressure evaporator, evaporating at 60 + -2 deg.C under negative pressure until the surface of the material is dry, placing in a muffle furnace, and roasting at 600 + -5 deg.C for 3 hr to obtain C-Al 2 O 3 -Ni micropowder.
C-Al prepared in examples 1 to 3 2 O 3 Fine powder of-Ni as shown in FIG. 1 for C-Al 2 O 3 The heat dissipation and thermal conductivity of the-Ni micropowder were measured and the results are shown in tables 1-2,
TABLE 1C-Al 2 O 3 Specific surface area of-Ni nanopowder
As can be seen from the data in table 1, after carbon coating treatment, nano-alumina has larger specific surface area agent void volume, i.e. has smaller density in fluid, larger suspension force and better heat dissipation.
TABLE 2C-Al 2 O 3 Thermal conductivity of Ni nanopowder
| Sample name | Coefficient of thermal conductivity (W/m. K) |
| Al 2 O 3 | 30 |
| Example C-Al 2 O 3 -Ni | 129 |
| Example II C-Al 2 O 3 -Ni | 132 |
| Example III C-Al 2 O 3 -Ni | 135 |
The data in table 2 show that the thermal conductivity of the carbon-coated and nickel-coated alumina is increased by more than 3 times, and the carbon-coated and nickel-coated alumina has good thermal dispersibility and thermal conductivity.
The performance of a cooling liquid prepared by adding polyol, a dispersing agent, a corrosion inhibitor and a defoaming agent according to a preparation technology combined with nanofluid is compared with that of a domestic antifreeze and a Hydromx @ series nanofluid heat exchanger produced by U.S. hydromx.inc. by taking the functional micropowder of the embodiment of the present invention as a base material, wherein a thermal conductivity detection method adopts a heat flow meter method ASTMC518(25 ℃), and the comparison results are shown in Table 3:
TABLE 3 Coolant comparison results
Table 3 shows that the cooling liquid prepared from the micro powder can be suitable for the engine nano cooling liquid with the operating condition of less than or equal to 120 ℃, the limit working boiling point temperature is higher than 15 ℃ of the domestic cooling liquid, the limit working freezing point temperature is lower than 20 ℃ of the Hydromx @ series nano fluid heat exchanger, the micro powder is suitable for regions and various engines in China, the thermal conductivity is higher than that of the domestic cooling liquid and the Hydromx @ series nano fluid heat exchanger, the application range is wide, and the practicability is higher.
The cooling liquid prepared from the 1-3 functional micro powder has no sediment and floccule when placed for 1 year, and the domestic antifreeze and Hydromx @ series nano fluid heat exchange agents have turbidity, sediment and a small amount of floccule, which shows that the cooling liquid has better stability.
FIG. 1 is an electron microscope image of the cooling liquid prepared by the present invention, and it can be seen from FIG. 1 that the particles are uniformly dispersed without agglomeration.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A preparation method of functional micro powder for engine coolant is characterized by comprising the following steps: the method comprises the following steps:
s1, degrading the fiber, and sequentially carrying out acidolysis and alkaline hydrolysis on the dried and crushed plant raw material to prepare an oligosaccharide solution;
S2，Al 2 O 3 coating carbon, and coating oligosaccharide obtained in step S1 with aluminum oxide to obtain C-Al 2 O 3 Micro-powder;
S3，C-Al 2 O 3 nickel cladding, C-Al of step S2 2 O 3 The micro powder is modified by nickel salt to obtain C-Al 2 O 3 -Ni micropowder.
2. The method for preparing a functional micropowder for engine coolant as claimed in claim 1, wherein: the acidolysis method of the step S1 comprises the following steps: soaking the plant raw materials in 1% sulfuric acid solution for 0.5-1h for acidolysis for 15-30min, filtering, leaching the filtrate with tap water, transferring into 2.5% NaOH solution for alkaline hydrolysis for 15-30min, filtering again, leaching the filtrate with tap water, transferring into 80% phosphoric acid solution, ultrasonically oscillating, centrifuging, and removing residue to obtain oligosaccharide solution.
3. The method for producing a functional micropowder for engine coolant according to claim 2, characterized by: the plant raw materials comprise sulfuric acid, NaOH and phosphoric acid according to the mass ratio of (10-15) to (20-31) to (18-23).
4. The method for producing a functional micropowder for engine coolant according to claim 2, characterized by: the plant material is one of rice straw, corncob, corn stalk and wheat stalk.
5. The method for preparing a functional micropowder for engine coolant as claimed in claim 1, wherein: the coating method of step S2 includes: mixing the oligosaccharide solution obtained in the step S1 with Al 2 O 3 Mixing the powders, filtering, and calcining the filtrate at 450 + -5 deg.C for 3-4h to obtain C-Al 2 O 3 And (5) micro-powder.
6. The method for producing a functional micropowder for engine coolant according to claim 5, characterized in that: the alumina powder: the mass ratio of the oligosaccharide solution is 1:4, and the particle size of the alumina powder is less than or equal to 100 nm.
7. The method for preparing a functional micropowder for engine coolant as claimed in claim 1, wherein: the coating method of step S3 includes: mixing nickel salt, citric acid and 50% phosphoric acid solution, and adding C-Al of step S2 2 O 3 Stirring the micro powder uniformly, heating to 60-70 ℃, and filtering; evaporating the filtrate to dry the surface of the material, and then roasting at 600 + -5 deg.C for 2-3h to obtain C-Al 2 O 3 -Ni micropowder.
8. The method for producing a functional micropowder for engine coolant according to claim 7, characterized by: the nickel salt is citric acid, phosphoric acid solution is C-Al 2 O 3 The mass ratio of the micro powder is (4-6): (0.5-1): (80-90): (9-12).
9. The method for producing a functional micropowder for engine coolant according to claim 7, characterized by: the nickel salt is nickel sulfate or nickel nitrate.
10. The application of the functional micro powder in preparing the nanometer cooling liquid or the nanometer fluid heat exchanger is characterized in that: the functional micropowder is prepared by the preparation method of claim 1.
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| CN115058129B (en) | 2023-09-12 |
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