CN110776877A - Water-based energy exchange medium containing hydroxylated graphene and preparation method thereof - Google Patents
Water-based energy exchange medium containing hydroxylated graphene and preparation method thereof Download PDFInfo
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- 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
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Abstract
The invention relates to a water-based energy exchange medium containing hydroxylated graphene and a preparation method thereof, belonging to the technical field of heat energy exchange liquid media. The energy exchange medium is prepared by mixing and compounding organic polyol, purified water, hydroxylated graphene, organic carboxylate composite corrosion inhibitor, silicon emulsion defoaming agent and warning color dye, wherein the surface of the added hydroxylated graphene has a large number of oxygen-containing groups such as hydroxyl groups, so that the added hydroxylated graphene has good solvent solubility, is easy to disperse in aqueous solution, and can remarkably improve the heat conductivity coefficient of the energy exchange medium. The freezing point specification of the energy exchange medium is determined according to the characteristics and requirements of a new energy application system and according to the historical lowest temperature data of the area where the system is located. The organic carboxylate compound corrosion inhibitor does not contain inorganic salt harmful to the environment or organisms, and is green, safe and nontoxic. The preparation method has the advantages of easily obtained raw materials, simple and convenient process operation and suitability for large-scale production, application and popularization.
Description
Technical Field
The invention relates to a water-based energy exchange medium and a preparation method thereof, in particular to a water-based energy exchange medium containing hydroxylated graphene and a preparation method thereof, and belongs to the technical field of heat energy exchange liquid media.
Background
Energy exchange relates to various fields of industrial application, including traditional fields of power, metallurgy, petrochemical industry, machinery, materials and the like and emerging technological and technical industries of electronics, nuclear energy, aviation and the like, and due to the needs of industrial production and scientific and technical development, the energy exchange technology has gained wide attention in recent decades. With the rapid development of scientific technology, energy revolution and energy substitution are actively carried out in China at present, and in the process, new energy sources such as solar energy, an air source heat pump, a central air conditioner, geothermal heat and the like are widely applied, play an important role in the fields of heating, heat supply, hot water engineering, cooling, refrigeration, centralized cooling and the like, and are also important modes and measures for protecting the blue sky, protecting the environment, saving energy and reducing emission in China. As "blood" in the operation of various systems-the energy exchange medium is a key factor affecting system safety and energy exchange efficiency.
With continuous practice and vigorous popularization of new energy, various energy exchange media are developed and applied, and meanwhile, the problems of the energy exchange media in the prior art are exposed, so that the defects of narrow application range of the freezing point, unstable antifreezing effect performance, poor corrosion and scale inhibition performance, unstable heat conducting performance, environmental protection and the like exist.
Firstly, the problem of freezing prevention is that water naturally existing in nature is a cheap and efficient energy exchange medium, but China has wide breadth and wide temperature difference. Because of the abnormal property of thermal shrinkage and cold expansion of water at about 0 ℃, except for a few provinces in the south, the problem of freezing prevention is not considered, and energy exchange media with different freezing points are selected according to local conditions in most regions in China. The method is to add glycol, propylene glycol or glycerol and other polyols as antifreeze agents into water to achieve the purpose of lowering the freezing point, and the heat conductivity coefficients of several polyols are smaller than that of water. Therefore, the high water ratio is kept to achieve higher heat exchange efficiency on the premise of ensuring that the system is not frozen, namely, a medium with a proper freezing point is selected according to the lowest temperature of the local history, rather than a freezing point specification is selected at intervals.
Second, the problem of metal corrosion inhibition, regardless of the form of new energy application, is that there are a variety of metal materials (e.g., copper, brass, stainless steel, carbon steel, cast iron, aluminum alloys, etc.) in the equipment, piping, and ends of the system that come into contact with the energy exchange medium. The corrosion inhibition, namely the pre-corrosion prevention, of various metals is required to be done, and due to the lack of unified technical standards, a few enterprises for professional development and production of the energy exchange medium are available on the market, and most of the new energy application systems are filled with common automobile antifreeze or the energy exchange medium based on the formula of the automobile antifreeze. Because the metal materials in the automobile cooling system and the new energy application system are different, the corrosion inhibition and the formula redesign are not targeted. The quality is uneven, and the product mainly contains inorganic salt formula of components harmful to the environment, such as phosphorus, boron, silicon, nitrite and the like. Particularly, even if a silicon stabilizer is added into a product containing silicate, colloid is easily formed after long-time use, so that the problems of blockage, corrosion inhibition capability reduction and the like are solved, and an environment-friendly energy exchange medium special for a new energy industry is developed and designed.
Thirdly, the heat exchange efficiency is problematic, water is a cheap medium with a relatively high thermal conductivity in a liquid substance, the thermal conductivity is 0.599 w/m.k at 20 ℃, the thermal conductivity is 0.253 w/m.k, 0.219 w/m.k and 0.276 w/m.k at 20 ℃ for three antifreeze agents, namely ethylene glycol, propylene glycol and glycerol, respectively, and the thermal conductivity is 0.415 w/m.k, 0.402 w/m.k and 0.45 w/m.k at 20 ℃ for three energy exchange media (ethylene glycol type, propylene glycol type and glycerol type in sequence) by taking the preparation of an aqueous solution with a mass ratio of 40% as an example; obviously, the thermal conductivity of various media is greatly reduced due to the addition of organic alcohol, and how to increase the thermal conductivity of the media so as to improve the heat exchange efficiency of the media also becomes an important subject.
Fourth, the problem of environmental protection and safety is that various additives need to be added into the energy exchange medium when the metal corrosion inhibition is solved, but phosphate which can easily enrich and oxidize the water environment, borate, silicate and nitrite which are harmful to the environment are added into the conventional formula at present, particularly nitrite is a highly toxic substance and is more easily harmful to various organisms and even human health, so that the development of the energy exchange medium which is environment-friendly, safe, easily degradable and nontoxic and has an environment-friendly formula is urgent.
Based on the problems, the development of the water-based energy exchange medium and the preparation method thereof have the advantages of stable performance, high heat conductivity coefficient, wide application range of freezing point, wide use environment, long-acting corrosion and scale inhibition performance, environmental protection and no toxic or side effect, and can greatly promote the replacement of energy.
Disclosure of Invention
Aiming at the defects of narrow application range of an ice point, unstable anti-freezing effect performance, poor corrosion and scale inhibition performance, unstable heat conduction performance, environmental protection and the like of the energy exchange medium in the prior art, the invention aims to improve the heat exchange efficiency of the medium by utilizing the high heat conduction performance of hydroxylated graphene, and provides the hydroxylated graphene-containing aqueous energy exchange medium which has stable anti-freezing performance, wide use environment, long-acting corrosion and scale inhibition performance, good heat conduction performance, environmental protection and no toxic or side effect, and the preparation method thereof.
The specific technical scheme of the invention is as follows:
the water-based energy exchange medium containing the hydroxylated graphene is prepared by mixing and compounding organic polyol, purified water, the hydroxylated graphene, a corrosion inhibitor, a silicon emulsion defoaming agent and a warning color dye, and is characterized in that the water-based energy exchange medium is prepared from the following raw materials in parts by mass:
15-65 parts of organic polyol;
35-85 parts of purified water;
0.05-5 parts of hydroxylated graphene;
0.5-5 parts of corrosion inhibitor;
0.01-0.05 part of silicon emulsion defoaming agent;
0.002-0.005 part of warning color dye.
Preferably, the organic polyol is one or a mixture of more than two of ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol and glycerol.
Preferably, wherein said purified water has an electrical conductivity of less than 15 μ s/cm.
Preferably, the purity of the hydroxylated graphene is more than or equal to 98%, the number of layers is less than or equal to 10, and the oxygen content is more than or equal to 10% by mass.
Preferably, the corrosion inhibitor is an organic carboxylate composite corrosion inhibitor, wherein the organic carboxylate composite corrosion inhibitor is obtained by dissolving sodium gluconate, composite organic carboxylic acid, azole compound, sodium molybdate, amino acid salt, pyrazine or piperazine compound in purified water and adding sodium hydroxide to adjust the pH value to 11-12, and is characterized in that the raw materials comprise the following components in parts by mass:
2-20 parts of sodium gluconate;
5-30 parts of composite organic carboxylic acid;
0.5-10 parts of azole compounds;
1-15 parts of sodium molybdate;
2-25 parts of amino acid salt;
1-10 parts of pyrazine or piperazine and derivatives thereof;
20-90 parts of purified water.
Preferably, the complex organic carboxylic acid is a mixed acid composed of any two or more of benzoic acid or a derivative thereof, isononanoic acid and sebacic acid.
Preferably, the azole compound is any one or a mixture of more than two of benzotriazole, methylbenzotriazole and 2-mercaptobenzothiazole.
Preferably, the amino acid salt is any one or a mixture of two or more of organic compounds such as serine sodium salt or potassium salt, cysteine sodium salt or potassium salt, glycine sodium salt or potassium salt, serine sodium salt or potassium salt, threonine sodium salt or potassium salt, phenylalanine sodium salt or potassium salt, tyrosine sodium salt or potassium salt, aspartic acid sodium salt or potassium salt, and glutamic acid sodium salt or potassium salt.
A method for preparing the hydroxylated graphene-containing aqueous energy exchange medium, comprising the following steps:
A. firstly, respectively weighing hydroxylated graphene and purified water according to formula requirements, adding the hydroxylated graphene into the purified water, and ultrasonically dispersing for 30 minutes by using an ultrasonic crusher to obtain a premix for later use;
B. uniformly stirring the hydroxylated graphene premix prepared in the above steps, then sequentially adding the organic carboxylate composite corrosion inhibitor, the polyol, the organic silicon emulsion defoamer and the warning color dye, stirring, and uniformly mixing to obtain a homogeneous clear and transparent finished product.
Preferably, the operating frequency of the ultrasonic crusher in the step A is 25 kHz.
The invention has the beneficial effects that:
(1) the hydroxylated graphene added in the invention has excellent heat conductivity and light transmittance, has good solvent solubility (including water) due to a large number of oxygen-containing groups such as hydroxyl groups on the surface, is easy to disperse in an aqueous solution, can obviously improve the heat conductivity coefficient of an energy exchange medium, and can improve the heat conductivity coefficient reduced by adding organic polyol to the heat conductivity coefficient equivalent to that of pure water by adding a proper proportion, so that the system has high energy exchange efficiency. The addition proportion of the hydroxylated graphene is within the range of 0.05-5% (mass percent), and the specific addition amount is determined according to the percentage of the organic polyol so as to achieve the thermal conductivity coefficient equivalent to or higher than that of water.
(2) Aiming at the characteristics and requirements of the ice point according to the new energy application system in the formula, and the freezing point specification of the energy exchange medium is determined according to the historical lowest temperature data of the area where the system is located, one or a mixture of two or more of ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol and glycerol can be selected as the antifreeze according to the actual conditions, can be prepared into energy exchange media with various freezing points with temperature difference steps of 5 ℃ between-5 ℃ and-50 ℃, for example, the freezing point of the water solution is-10 ℃ when the ethylene glycol is 24 percent (mass percent), the freezing point of the water solution is-25 ℃ when the 1, 2-propylene glycol is 43.5 percent (mass percent), and the freezing point of the water solution is-30 ℃ when the 1, 3-propylene glycol is 47 percent (mass percent). In the formula, the adding proportion of purified water is 35-85% (mass percent in aqueous solution), the adding proportion of organic polyol is 15-65% (mass percent in aqueous solution), and the respective proportion of purified water and organic polyol is generally determined according to the specific freezing point requirement. This makes it possible to increase the water content as much as possible in order to achieve a high heat exchange efficiency of the energy exchange medium, depending on the circumstances.
(3) The organic carboxylate compound corrosion inhibitor used in the invention does not contain inorganic salt harmful to the environment or organisms, is green, safe and nontoxic, is an organic environment-friendly formula, has an addition proportion of 0.5-5% in an energy exchange medium, and has excellent corrosion inhibition performance on various metal materials such as red copper, brass, carbon steel, cast iron, cast aluminum, soldering tin and the like possibly existing in a system, and all technical indexes of glassware corrosion tests are within a required range.
Detailed Description
In order to better understand the invention, the following examples further illustrate the content of the invention, but the content of the invention is not limited to the following examples, and the examples should not be construed as limiting the scope of the invention.
Example 1 hydroxylated graphene containing 1, 2-propanediol-type aqueous energy exchange media with freezing point-20 ℃ and preparation thereof
Respectively weighing 10 g of hydroxylated graphene and 290 g of purified water, adding the hydroxylated graphene into the purified water, and ultrasonically dispersing for 30 minutes by using an ultrasonic crusher with the working frequency of 25kHz to obtain a premix for later use. And weighing 5.5 kg of purified water, adding the hydroxylated graphene premix into the mixture, uniformly stirring the mixture, sequentially adding 300 g of the organic carboxylate composite corrosion inhibitor, 3.9 kg of 1, 2-propylene glycol, 5 g of the organosilicon emulsion defoamer and 0.5 g of the dye, stirring the mixture, and uniformly mixing the mixture to obtain a homogeneous clear and transparent finished product, wherein the pH value of the solution is 8.8.
The obtained product and a self-produced inorganic salt formula (indicating corrosion inhibitor type) propylene glycol type medium with the same freezing point are subjected to glassware corrosion comparative test detection according to NB/T34073 and 2018 propylene glycol type solar low-temperature heat utilization working medium, and the test results are as follows:
according to the test results, the quality change values of various metal test pieces of the organic carboxylate formula in glassware corrosion tests are smaller than those of various inorganic salt type metal test pieces of the energy exchange medium with the same type and the same freezing point, and the product meets the design requirements.
Example 2 hydroxylated graphene containing 1, 3-propanediol-type aqueous energy exchange media with freezing point of-30 ℃ and preparation thereof
13 g of hydroxylated graphene and 287 g of purified water are weighed respectively, the hydroxylated graphene is added into the purified water, and the purified water is subjected to ultrasonic dispersion for 30 minutes by using an ultrasonic crusher with the working frequency of 25kHz, so that a premix is obtained for later use. And weighing 4.58 kg of purified water, adding the hydroxylated graphene premix into the mixture, uniformly stirring the mixture, sequentially adding 320 g of organic carboxylate composite corrosion inhibitor, 4.8 kg of 1, 3-propylene glycol, 5 g of organosilicon emulsion defoamer and 0.5 g of dye, stirring the mixture, and uniformly mixing the mixture to obtain a homogeneous clear transparent finished product, wherein the pH value of the solution is 8.6.
And preparing the 1, 3-propanediol type aqueous energy exchange medium with the freezing point of-30 ℃ without the hydroxylated graphene in a comparative sample according to the proportion (the preparation step of the hydroxylated graphene premix is removed, and purified water is completely replaced).
When the thermal conductivity coefficients of the two samples at 20 ℃ are respectively detected to be 0.357 w/m.k (a comparison sample without hydroxylated graphene) and 0.586 w/m.k (an energy exchange medium containing hydroxylated graphene), the addition of the hydroxylated graphene can be seen to greatly improve the thermal conductivity coefficient of the solution.
Example 3 Glycerol-type aqueous energy exchange Medium containing hydroxylated graphene with freezing Point-15 deg.C and preparation thereof
Weighing 8.5 g of hydroxylated graphene and 291.5 g of purified water respectively, adding the hydroxylated graphene into the purified water, and ultrasonically dispersing for 30 minutes by using an ultrasonic crusher with the working frequency of 25kHz to obtain a premix for later use. And then 5.315 kg of purified water is weighed, the hydroxylated graphene premix is added and stirred uniformly, then 285 g of organic carboxylate composite corrosion inhibitor, 4.1 kg of glycerol, 5 g of organosilicon emulsion defoamer and 0.5 g of dye are added in sequence, the mixture is stirred and mixed uniformly, a homogeneous clear and transparent finished product is obtained, and the pH value of the solution is 8.7.
According to the proportion (the preparation step of the hydroxylated graphene premix is removed, and purified water is completely replaced), a glycerol type aqueous energy exchange medium with a freezing point of-15 ℃ and without hydroxylated graphene in a comparative sample is prepared.
When the thermal conductivity coefficients of the two samples at 20 ℃ are respectively detected to be 0.446 w/m.k (a comparison sample without hydroxylated graphene) and 0.607 w/m.k (an energy exchange medium containing hydroxylated graphene), the addition of the hydroxylated graphene can be seen to greatly improve the thermal conductivity coefficient of the solution.
Example 4 glycol-based aqueous energy exchange media with hydroxylated graphene at freezing point-25 deg.C and preparation thereof
Respectively weighing 12.8 g of hydroxylated graphene and 287.2 g of purified water, adding the hydroxylated graphene into the purified water, and ultrasonically dispersing for 30 minutes by using an ultrasonic crusher with the working frequency of 25kHz to obtain a premix for later use. And weighing 5.185 kg of purified water, adding the hydroxylated graphene premix into the mixture, uniformly stirring the mixture, sequentially adding 315 g of the organic carboxylate composite corrosion inhibitor, 4.2 kg of ethylene glycol, 5 g of the organic silicon emulsion defoamer and 0.5 g of the dye, stirring the mixture, and uniformly mixing the mixture to obtain a homogeneous clear and transparent finished product, wherein the pH value of the solution is 8.5.
According to the proportion (the preparation step of the hydroxylated graphene premix is removed, and purified water is completely replaced), a glycerol type aqueous energy exchange medium with a freezing point of-15 ℃ and without hydroxylated graphene in a comparative sample is prepared.
When the thermal conductivity coefficients of the two samples at 20 ℃ are respectively detected to be 0.394 w/m.k (a comparison sample without hydroxylated graphene) and 0.613 w/m.k (an energy exchange medium containing hydroxylated graphene), it can be seen that the addition of the hydroxylated graphene greatly improves the thermal conductivity coefficient of the solution.
Claims (10)
1. The water-based energy exchange medium containing the hydroxylated graphene is obtained by mixing and compounding organic polyol, purified water, the hydroxylated graphene, a corrosion inhibitor, a silicon emulsion defoaming agent and a warning color dye, and is characterized in that the water-based energy exchange medium is prepared from the following raw materials in parts by mass:
15-65 parts of organic polyol;
35-85 parts of purified water;
0.05-5 parts of hydroxylated graphene;
0.5-5 parts of corrosion inhibitor;
0.01-0.05 part of silicon emulsion defoaming agent;
0.002-0.005 part of warning color dye.
2. The hydroxylated graphene-containing aqueous energy exchange medium of claim 1, wherein: wherein the organic polyol is one or a mixture of two or more of ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol and glycerol.
3. The hydroxylated graphene-containing aqueous energy exchange medium of claim 1, wherein: wherein the corrosion inhibitor is an organic carboxylate composite corrosion inhibitor, and the electric conductivity of the purified water is lower than 15 mu s/cm.
4. The hydroxylated graphene-containing aqueous energy exchange medium of claim 1, wherein: the purity of the hydroxylated graphene is more than or equal to 98%, the number of layers is less than or equal to 10, and the oxygen content is more than or equal to 10% by mass.
5. The aqueous energy exchange medium containing hydroxylated graphene according to claim 3, characterized in that the organic carboxylate compound corrosion inhibitor is obtained by dissolving sodium gluconate, compound organic carboxylic acid, azole compound, sodium molybdate, amino acid salt, pyrazine or piperazine compound in purified water and adding sodium hydroxide to adjust the pH value to 11-12, wherein the raw materials comprise, by mass:
2-20 parts of sodium gluconate;
5-30 parts of composite organic carboxylic acid;
0.5-10 parts of azole compounds;
1-15 parts of sodium molybdate;
2-25 parts of amino acid salt;
1-10 parts of pyrazine or piperazine and derivatives thereof;
20-90 parts of purified water.
6. The hydroxylated graphene-containing aqueous energy exchange medium of claim 5, wherein: wherein the compound organic carboxylic acid is a mixed acid consisting of any two or more of benzoic acid or derivatives thereof, isononanoic acid and sebacic acid.
7. The hydroxylated graphene-containing aqueous energy exchange medium of claim 5, wherein: wherein the azole compound is any one or a mixture of more than two of benzotriazole, methylbenzotriazole and 2-mercaptobenzothiazole.
8. The hydroxylated graphene-containing aqueous energy exchange medium of claim 5, wherein: the amino acid salt is any one or a mixture of more than two of organic compounds such as serine sodium salt or potassium salt, cysteine sodium salt or potassium salt, glycine sodium salt or potassium salt, serine sodium salt or potassium salt, threonine sodium salt or potassium salt, phenylalanine sodium salt or potassium salt, tyrosine sodium salt or potassium salt, aspartic acid sodium salt or potassium salt, glutamic acid sodium salt or potassium salt and the like.
9. A method of preparing the hydroxylated graphene-containing aqueous energy exchange medium of claim 1, comprising the steps of:
A. firstly, respectively weighing hydroxylated graphene and purified water according to the formula requirements, adding the hydroxylated graphene into the purified water, and ultrasonically dispersing for 30 minutes by using an ultrasonic crusher with the working frequency of 25kHz to obtain a premix for later use;
B. uniformly stirring the hydroxylated graphene premix prepared in the above steps, then sequentially adding the organic carboxylate composite corrosion inhibitor, the polyol, the organic silicon emulsion defoamer and the warning color dye, stirring, and uniformly mixing to obtain a homogeneous clear and transparent water-based energy exchange medium containing the hydroxylated graphene.
10. The method of claim 9, wherein the method comprises the steps of: the working frequency of the ultrasonic crusher in the step A is 25 kHz.
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| CN113351093A (en) * | 2021-06-07 | 2021-09-07 | 山东铂润新能源科技有限公司 | Water-soluble heat-conducting liquid preparation device |
| CN113351093B (en) * | 2021-06-07 | 2022-07-22 | 山东铂润新能源科技有限公司 | Water-soluble heat-conducting liquid preparation device |
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