WO2024099277A1 - 介电冷却液及其制备方法与应用 - Google Patents

介电冷却液及其制备方法与应用 Download PDF

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WO2024099277A1
WO2024099277A1 PCT/CN2023/129991 CN2023129991W WO2024099277A1 WO 2024099277 A1 WO2024099277 A1 WO 2024099277A1 CN 2023129991 W CN2023129991 W CN 2023129991W WO 2024099277 A1 WO2024099277 A1 WO 2024099277A1
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base oil
oil
cycloalkyl
dielectric coolant
content
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English (en)
French (fr)
Inventor
张美琼
张静
罗来龙
何军
马蕊燕
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Petrochina Co Ltd
Petrochina Karamay Petrochemical Co
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Petrochina Co Ltd
Petrochina Karamay Petrochemical Co
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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
    • C09K5/20—Antifreeze additives therefor, e.g. for radiator liquids
    • 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
    • C09K5/08—Materials not undergoing a change of physical state when used
    • C09K5/10—Liquid materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/60—Heating or cooling; Temperature control
    • H01M10/61—Types of temperature control
    • H01M10/613—Cooling or keeping cold
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/60—Heating or cooling; Temperature control
    • H01M10/65—Means for temperature control structurally associated with the cells
    • H01M10/656—Means for temperature control structurally associated with the cells characterised by the type of heat-exchange fluid
    • H01M10/6567—Liquids

Definitions

  • the invention belongs to the technical field of liquid cooling of electronic devices, and in particular to a dielectric cooling liquid, a preparation method and application thereof.
  • liquid cooling In simple terms, the principle of liquid cooling is to use heat convection or heat conduction to The heat dissipated by the server is taken away by the liquid or flowing.
  • the liquid cooling methods of the server mainly include cold plate liquid cooling, immersion liquid cooling and spray liquid cooling.
  • the coolants used in liquid cooling technology mainly include water and fluorinated liquid.
  • water is a non-insulator and can only be used in non-direct contact cold plate liquid cooling technology. Once a leak occurs, it will cause fatal damage to IT equipment; fluorinated liquid is the most widely used direct contact coolant for immersion, but it is expensive, volatile, has high cost of use, high density, and high load-bearing requirements for buildings.
  • fluorinated liquid have the above disadvantages as coolants, the relevant industry actively studies and explores the use of oil coolants in direct contact liquid cooling, most of which are studies on synthetic oil and silicone oil coolants.
  • CN 110862806 A discloses a method for preparing a coolant for electronic devices using dimethyl silicone oil, natural ester oil or synthetic ester oil as a base oil and adding an antioxidant and a dispersant.
  • CN 113861948 A discloses an immersion liquid cooling coolant prepared from defoaming agent, oily epoxy resin, dispersant, siloxane, flash point enhancer, and terminal hydroxyl polybutadiene.
  • synthetic oil or silicone oil is cheaper than fluorinated liquid, their prices are still relatively expensive.
  • natural petroleum distillate oil is cheap and has a good application prospect as an IT equipment coolant.
  • CN 107502309B discloses a coolant and a preparation method thereof, which is prepared by adding a trace amount of antioxidant, defoamer and dispersant to a traditional mineral base oil, and is suitable for immersion direct cooling of IT equipment in an open environment.
  • the coolant has poor environmental performance, a breakdown voltage of only 30kV (poor insulation performance), poor flame retardancy, and after the cables of IT equipment are immersed in the coolant for a long time, the plasticizer is easily precipitated, causing the cables to harden.
  • the coolant in the prior art has the problems of high price, poor environmental performance, poor insulation performance, poor flame retardancy or easy precipitation of plasticizer.
  • the present invention provides a dielectric coolant, a preparation method and its application.
  • the raw materials of the coolant are easily available, the preparation process is simple and the cost is low, the coolant is colorless and transparent, has good flowability, fire safety performance, thermal conductivity, insulation performance and oxidation stability, is non-toxic, environmentally friendly, non-corrosive, has good compatibility with IT equipment liquid cooling system materials, has good stability during use, and can be applied to direct contact cooling such as immersion or spraying of IT equipment.
  • the present invention provides a dielectric coolant in a first aspect, wherein the dielectric coolant comprises a base oil and an additive;
  • the mass ratio of the base oil to the additive is 100:2-12;
  • the additive includes an antioxidant, a cable extender and a modified nanomaterial;
  • the base oil includes a cycloalkyl base oil and a paraffin base oil, wherein the content of the cycloalkyl base oil is not less than 60wt%, the content of the paraffin base oil is not less than 20wt%, and the total amount of the cycloalkyl base oil and the paraffin base oil is 100wt%;
  • the modified nano material is at least one of modified nano magnesium hydroxide and modified nano aluminum hydroxide, and the modified nano material accounts for 1-5wt% of the base oil mass.
  • a second aspect of the present invention provides a method for preparing a dielectric coolant, wherein the method comprises the following steps:
  • the base oil of the dielectric coolant is obtained by fully mixing a cycloalkane base oil having a content of not less than 60 wt % and a paraffin base oil having a content of not less than 20 wt % at 50-60° C.;
  • An antioxidant, a cable extender and a modified nanomaterial are sequentially added to the base oil, and then heated at 50-60° C. and stirred until the base oil becomes clear and transparent. After cooling to room temperature, the base oil is filtered to obtain a dielectric coolant.
  • a third aspect of the present invention provides an application of a dielectric coolant, wherein the dielectric coolant is applied in the field of IT equipment or battery cooling.
  • the present invention has the following beneficial technical effects:
  • the invention prepares a dielectric coolant by adding an antioxidant, a cable extender and a modified nano material to a base oil obtained by blending a cycloalkyl base oil and a paraffin base oil, wherein the content of heteroatoms such as sulfur and nitrogen in the cycloalkyl base oil and the paraffin base oil is 0, the base oil is non-toxic, environmentally friendly, has good solubility for additives and oxides that may be generated after use, and has good stability and stability; the antioxidant improves the oxidation stability of the dielectric coolant; the cable extender improves the compatibility of the dielectric coolant and the cable, so that after the cable is immersed in the dielectric coolant for a long time, the plasticizer of the cable will not precipitate and the cable will not harden; the nano material improves the flame retardant property, thermal conductivity and insulation property of the dielectric coolant.
  • the dielectric coolant developed by the present invention is colorless and transparent, has a kinematic viscosity of 4-15 mm 2 /s at 40°C, a pour point of ⁇ -60°C, good fluidity at 40°C and low temperatures, good fire safety performance, thermal conductivity, insulation performance, oxidation stability and environmental friendliness, is non-corrosive, has good compatibility with IT equipment liquid cooling system materials, has good stability during use, and can be applied to direct contact cooling of IT equipment such as immersion or spraying.
  • the dielectric coolant uses the product of deep hydrogenation of natural petroleum distillate as the base oil, and the process involved is simple, environmentally friendly, high in yield and low in cost.
  • the composition can achieve the same performance as other similar synthetic dielectric coolants, and is easier to prepare and has higher economic value than synthetic oil or silicone oil coolants, and is easy to realize industrial-scale production.
  • the endpoints of the ranges and any values disclosed herein are not limited to the exact ranges or values, and these ranges or values should be understood to include values close to these ranges or values.
  • the endpoint values, the endpoint values of each range and the individual point values, and the individual point values can be combined with each other to obtain one or more new numerical ranges, which should be considered to be specifically disclosed herein.
  • the first aspect of the present invention provides a dielectric coolant, wherein the dielectric coolant comprises a base oil and an additive; wherein the mass ratio of the base oil to the additive is 100:2-12; the additive comprises an antioxidant, a cable extender and a modified nanomaterial; the base oil comprises a cycloalkyl base oil and a paraffin base oil, in which the content of the cycloalkyl base oil is not less than 60wt%, the content of the paraffin base oil is not less than 20wt%, and the total amount of the cycloalkyl base oil and the paraffin base oil is 100wt%; the modified nanomaterial is at least one of modified nano magnesium hydroxide and modified nano aluminum hydroxide, and the modified nanomaterial is 1-5wt% of the mass of the base oil.
  • the base oil is obtained by further processing from natural petroleum belonging to mineral oil (specifically, it can be from naphthenic crude oil and paraffinic crude oil), and still belongs to mineral oil.
  • the distillate oil from naphthenic crude oil and the distillate oil from paraffinic crude oil are respectively subjected to high pressure hydrogenation (or deep hydrogenation) to obtain the naphthenic base oil and paraffinic base oil in the present invention respectively.
  • cycloalkyl crude oil is first subjected to atmospheric and vacuum distillation to obtain cycloalkyl crude oil fraction oil with a distillation range of 260-450° C., and then further subjected to hydrogenation treatment, isomerization decondensation, and hydrogenation supplementary refining in sequence under a hydrogen partial pressure of 14-18 MPa. Finally, the product obtained by hydrogenation supplementary refining is subjected to atmospheric and vacuum distillation, and the fraction oil with a temperature of 270-410° C. is taken as the cycloalkyl base oil in the dielectric coolant of the present invention.
  • paraffin-based crude oil is first subjected to atmospheric and vacuum distillation to obtain a paraffin-based crude oil fraction with a distillation range of 260-480°C, and then further subjected to hydrogenation treatment, isomerization decondensation, hydrogenation refining in sequence under a hydrogen partial pressure of 14-18 MPa, and finally the product obtained by hydrogenation refining is subjected to atmospheric and vacuum distillation to obtain a paraffin-based crude oil fraction with a distillation range of 270-410°C.
  • the distillate oil is used as the paraffin-based base oil in the dielectric coolant of the present invention.
  • the cycloalkyl crude oil or the paraffinic crude oil is subjected to atmospheric and vacuum distillation (concurrently subjected to atmospheric distillation and vacuum distillation), and the conditions may include: the atmospheric distillation temperature is 350-390°C and the pressure is 0.1-0.2MPa; the vacuum distillation temperature is 350-420°C and the pressure is ⁇ 11kPa; the corresponding cycloalkyl crude oil fraction or the paraffinic crude oil fraction is recorded as raw material oil I.
  • the conditions for the hydrogenation treatment of the cycloalkyl base oil or the paraffinic base oil include: the hydrogenation temperature is 300-400°C, the weight hourly space velocity of the raw material oil I is 0.7-1.4h -1 , the volume ratio of hydrogen to oil (hydrogen to raw material oil I) is 900-2800:1, wherein the catalyst is alumina as a carrier, Ni and/or Mo are active components, and the active component content is 0.2-1.5wt%.
  • the cycloalkyl hydrotreated oil or the paraffinic hydrotreated oil is obtained, which is recorded as raw material oil II.
  • the conditions for isomerization decondensation include: isomerization decondensation temperature of 310-390°C, weight hourly space velocity of feedstock oil II of 0.2-0.9h -1 , volume ratio of hydrogen to oil (hydrogen to feedstock oil II) of 900-2200:1, wherein the catalyst is supported by zirconium oxide and loaded with 0.2-1.2 wt % of Group VIII noble metal (as active component, such as loaded rhodium and/or iridium), and cycloalkyl decondensation oil or paraffin decondensation oil is obtained, which is recorded as feedstock oil III.
  • Group VIII noble metal as active component, such as loaded rhodium and/or iridium
  • the conditions for hydrogenation supplementary refining include: refining temperature of 200-340°C, weight hourly space velocity of feed oil III of 1.6-2.8h -1 , volume ratio of hydrogen to oil (hydrogen to feed oil III) of 900-2200:1, wherein the catalyst is supported by silicate and loaded with Group VIII noble metals (as active components) rhodium and/or iridium 0.4-1.5wt%. To obtain cycloalkyl base oil or paraffin base oil respectively.
  • the content of the cycloalkane base oil can generally be 60-80wt%, and the content of the paraffin base oil can be 20-40wt%.
  • the cycloalkyl base oil includes a first cycloalkyl oil and a second cycloalkyl oil, wherein, based on the total amount of the base oil, the content of the first cycloalkyl oil in the base oil is 0-60wt%, and the content of the second cycloalkyl oil in the base oil is 20-60wt%.
  • the total amount of oil is equal to the content of the naphthenic base oil in the base oil.
  • the first cycloalkyl oil is obtained by the following method:
  • the cycloalkyl crude oil is subjected to atmospheric and vacuum distillation to obtain a cycloalkyl fraction oil with a distillation range of 290-410° C., and then the cycloalkyl fraction oil is subjected to hydrogenation treatment, isomerization decondensation, and hydrogenation supplementary refining in sequence under a hydrogen partial pressure of 14-18 MPa, and the product obtained by hydrogenation supplementary refining is subjected to atmospheric and vacuum distillation to obtain a fraction of 270-410° C. as the first cycloalkyl oil;
  • the conditions of the hydrotreatment include: a hydrogenation temperature of 300-360°C, a weight hourly space velocity of 0.7-1.4h -1 , and a hydrogen to oil volume ratio of 900-2800:1;
  • the conditions for isomerization decondensation include: isomerization decondensation temperature of 310-360°C, weight hourly space velocity of 0.2-0.9h -1 , hydrogen to oil volume ratio of 900-2200:1;
  • the conditions for hydrogenation supplementary refining include: refining temperature of 200-340°C, weight hourly space velocity of 1.6-2.8h -1 , hydrogen-to-oil volume ratio of 900-2200:1.
  • the second cycloalkyl oil is obtained by the following method:
  • the cycloalkyl crude oil is subjected to atmospheric and vacuum distillation to obtain a cycloalkyl fraction oil with a distillation range of 280-400°C, and then subjected to hydrogenation treatment, isomerization decondensation, and hydrogenation supplementary refining at a hydrogen partial pressure of 14-18 MPa in sequence, and the product obtained by hydrogenation supplementary refining is then subjected to atmospheric and vacuum distillation to obtain a fraction of 270-410°C as the second cycloalkyl oil;
  • the conditions of the hydrotreatment include: a hydrogenation temperature of 330-400°C, a weight hourly space velocity of 0.7-1.4h -1 , and a hydrogen to oil volume ratio of 900-2800:1;
  • the conditions for isomerization decondensation include: isomerization decondensation temperature of 330-390°C, weight hourly space velocity of 0.2-0.9h -1 , hydrogen to oil volume ratio of 900-2200:1;
  • the conditions for hydrogenation supplementary refining include: refining temperature of 200-340°C, weight hourly space velocity of 1.6-2.8h -1 , hydrogen-to-oil volume ratio of 900-2200:1.
  • first cycloalkane oil hereinafter referred to as base oil A
  • second cycloalkane oil hereinafter referred to as base oil B
  • paraffin-based base oil hereinafter referred to as base oil C
  • the content of heteroatoms such as sulfur and nitrogen in base oil A is 0, the number of aromatic rings contained is at most one ring, it is non-toxic, environmentally friendly, the distillation range is 270-410°C, and the pour point is -50°C to -40°C
  • the content of heteroatoms such as sulfur and nitrogen in base oil B is 0, there is no aromatic hydrocarbon, it is non-toxic, environmentally friendly, the distillation range is 270-410°C, and the pour point is -70°C to -60°C
  • the content of heteroatoms such as sulfur and nitrogen in base oil C is 0, there is no aromatic hydrocarbon, it is non-toxic, environmentally friendly, the distillation range is 270-410°C, and the pour point is -70°C to -60°C.
  • High-pressure hydrogenation can remove heteroatoms such as sulfur, nitrogen, and oxygen from crude oil fractions, hydrogenate unsaturated hydrocarbons (especially condensed-ring aromatic hydrocarbons), and generate stable heteroatom-free alkanes and cycloalkanes (cycloalkanes have good solubility for additives and oxides that may be produced during use), further improving the stability and environmental friendliness of the coolant base oil, while retaining an appropriate content of monocyclic aromatic hydrocarbons in the first cycloalkane base oil to further improve the solubility of the coolant base oil, and the monocyclic aromatic hydrocarbons do not affect the environmental friendliness.
  • the isomerization depressant in high-pressure hydrogenation converts straight-linked alkanes into isomerized alkanes, improving the low-temperature properties of the coolant such as the pour point.
  • the invention adopts distillate oil of atmospheric and vacuum suitable fraction section of paraffin-based crude oil and distillate oil of atmospheric and vacuum suitable fraction section of naphthenic crude oil as raw materials, respectively undergoes three-stage high-pressure hydrogenation treatment of hydrogenation treatment, isomerization decondensation and hydrogenation supplementary refining under reasonable process conditions, and then blends the prepared naphthenic base oil of suitable fraction and paraffin-based base oil in a suitable proportion as dielectric coolant base oil, so as to adjust the carbon structure of the coolant base oil and improve the flowability, stability and environmental friendliness of the coolant at a working temperature of 40°C and low temperature.
  • the dielectric coolant further includes an additive, and the mass ratio of the base oil to the additive is 100:2-12.
  • the additives include antioxidants, cable extenders and modified nanomaterials.
  • Antioxidants can improve the oxidation stability of dielectric coolants. Due to factors such as cost, the amount of antioxidant used can generally be 0.2-0.6wt% of the base oil.
  • the antioxidant is at least one of 2,6-di-tert-butyl-p-cresol, 2,6-di-tert-butylphenol and alkyl diphenylamine.
  • Cable extenders can improve the compatibility of cables such as electrical wires and network cables in dielectric coolants, so that after the cables are immersed in 40-60°C dielectric coolants for a long time, the plasticizers in the cables will not precipitate and the cables will not harden.
  • the cable compatibilizer includes an oily epoxy resin and a dispersant, and the oily epoxy resin and the dispersant interact with each other to improve the compatibility of the cable in the dielectric coolant.
  • the amount of the oily epoxy resin is 1-5wt% of the base oil, and the amount of the dispersant is 0.03-0.1wt% of the base oil.
  • the oily epoxy resin can be commercially available epoxy resin E-44.
  • the dispersant is at least one of BYK-2152 dispersant and BYK-R605 dispersant, which are commercially available from Vibos New Materials Company.
  • Nanomaterials can improve the flame retardancy, thermal conductivity and electrical properties of dielectric coolants. Compared with ordinary nanomaterials, modified nanomaterials have the above advantages and a more prominent advantage of good dispersibility in dielectric coolants.
  • the modified nanomaterials used in the present invention are commercially available products, and the amount of the modified nanomaterials can generally be 1-5wt% of the mass of the base oil.
  • the modified nanomaterials can be nanomaterials modified with surfactants, and the surfactants can be, for example, phosphate surfactants. In the modified nanomaterials, the content of the surfactant is 1-10wt%.
  • the modified nano material is at least one of modified nano magnesium hydroxide and modified nano aluminum hydroxide.
  • the modified nano magnesium hydroxide and modified nano aluminum hydroxide are spherical in shape, with an average particle size of 10-50nm, a specific surface area of 30-50m2 /g, good dispersion stability in the coolant, and non-volatile.
  • the dielectric coolant has a kinematic viscosity of 40°C of 4-15 mm 2 /s and a pour point of ⁇ -60°C, so it has good flow properties at 40°C and low temperatures.
  • the second aspect of the present invention provides a method for preparing the above-mentioned dielectric coolant, wherein the method comprises the following steps: fully mixing a cycloalkane base oil with a content of not less than 60wt% and a paraffin base oil with a content of not less than 20wt% at 50-60°C to obtain a base oil for the dielectric coolant; adding an antioxidant, an oily epoxy resin, a dispersant and a modified nanomaterial to the base oil in sequence, heating and stirring at 50-60°C until clear and transparent, cooling to room temperature, and filtering to obtain the dielectric coolant.
  • the dielectric coolant of the present invention comprises a base oil in which the total amount of the cycloalkyl base oil and the paraffin base oil is 100wt%.
  • the dielectric coolant is prepared by adding an antioxidant, a cable extender and a modified nano material to a base oil prepared by blending the cycloalkyl base oil and the paraffin base oil, wherein the cycloalkyl base oil and the paraffin base oil have a heteroatom content of 0 such as sulfur and nitrogen, are non-toxic, environmentally friendly, have good solubility for additives and oxides that may be generated after use, and have good stability and stability;
  • the antioxidant improves the oxidation stability of the dielectric coolant;
  • the cable extender improves the compatibility of the dielectric coolant with the cable; and the nano material improves the flame retardant performance, thermal conductivity and electrical performance of the dielectric coolant.
  • the dielectric coolant developed by the present invention is colorless and transparent, has a kinematic viscosity of 4-15 mm2 /s at 40°C, a pour point of ⁇ -60°C, and has good flow properties at 40°C and low temperatures, good fire safety performance, thermal conductivity, insulation performance, oxidation stability and environmental friendliness, is non-corrosive, has good compatibility with IT equipment liquid cooling system materials, has good stability during use, and can be applied to direct contact cooling such as immersion or spraying of IT equipment.
  • the dielectric coolant provided by the present invention uses the product of deep hydrogenation of natural petroleum distillate oil as the base oil, and the process involved is simple, environmentally friendly, high in yield and low in cost.
  • the composition can achieve the same performance as other similar synthetic dielectric coolants, and is easier to prepare and has higher economic value than synthetic oil or silicone oil coolants, and is easy to achieve industrial scale production.
  • the preparation of the cycloalkyl base oil and the paraffin base oil is as described above, and no further description is given.
  • the base oil is obtained by blending the first cycloalkyl oil and the second cycloalkyl oil with a paraffinic base oil.
  • the first cycloalkyl oil and the second cycloalkyl oil are charged to meet the requirement that, based on the total amount of the base oil, the content of the first cycloalkyl oil in the base oil is 0-60wt%, and the content of the second cycloalkyl oil in the base oil is 20-60wt%.
  • the total amount of the first cycloalkyl oil and the second cycloalkyl oil is equal to the content of the cycloalkyl base oil in the base oil.
  • the amount of the paraffinic base oil is satisfied that, based on the total amount of the base oil, in the base oil, the content of the cycloalkyl base oil is not less than 60wt%, the content of the paraffinic base oil is not less than 20wt%, and the total amount of the cycloalkyl base oil and the paraffinic base oil is 100wt%.
  • a third aspect of the present invention provides an application of a dielectric coolant, wherein the dielectric coolant is applied in the field of IT equipment or battery cooling.
  • the naphthenic crude oil is subjected to atmospheric and vacuum distillation to obtain a distillate oil with a distillation range of 290-410°C, which is then subjected to hydrogenation treatment, isomerization decondensation, and hydrogenation supplementary refining in sequence under the following conditions:
  • Hydrogenation treatment The catalyst is supported by alumina and loaded with 0.5 wt% nickel.
  • the conditions include: pressure of 15.0 ⁇ 0.5 MPa, temperature of 320 ⁇ 5°C, space velocity of 1.0 ⁇ 0.1 h -1 , and hydrogen-to-oil volume ratio of 1000:1.
  • Heterogeneous decondensation The catalyst is supported by zirconium oxide and loaded with 0.4 wt% iridium; the conditions include: pressure of 15.0 ⁇ 0.5 MPa, temperature of 320 ⁇ 5°C, space velocity of 0.8 ⁇ 0.1h -1 , and hydrogen-oil volume ratio of 1000:1.
  • Hydrogenation supplementary refining The catalyst is supported by silicate and loaded with 0.6 wt% rhodium; the conditions include: pressure of 15.0 ⁇ 0.5 MPa, temperature of 310 ⁇ 5°C, space velocity of 2.0 ⁇ 0.1h -1 , and hydrogen-to-oil volume ratio of 1000:1.
  • the product obtained by hydrogenation refining is subjected to atmospheric and vacuum distillation, and the 290-370°C fraction is taken as the base oil A.
  • the naphthenic crude oil is subjected to atmospheric and vacuum distillation to obtain a distillate oil with a distillation range of 280-400°C, which is then subjected to hydrogenation treatment, isomerization decondensation, and hydrogenation supplementary refining in sequence under the following conditions:
  • Hydrogenation treatment The catalyst is supported by alumina and loaded with 0.5 wt% nickel.
  • the conditions include: pressure of 17.0 ⁇ 0.5 MPa, temperature of 340 ⁇ 5°C, space velocity of 1.0 ⁇ 0.1 h -1 , and hydrogen-to-oil volume ratio of 1000:1.
  • Heterogeneous decondensation The catalyst is supported by zirconium oxide and loaded with 0.4 wt% iridium.
  • the conditions include: pressure of 17.0 ⁇ 0.5 MPa, temperature of 340 ⁇ 5°C, space velocity of 0.8 ⁇ 0.1 h -1 , and hydrogen-to-oil volume ratio of 1000:1.
  • Hydrogenation supplementary refining The catalyst is supported by silicate and loaded with 0.6 wt% rhodium.
  • the conditions include: pressure of 17.0 ⁇ 0.5 MPa, temperature of 310 ⁇ 5°C, space velocity of 2.0 ⁇ 0.1 h -1 , and hydrogen-to-oil volume ratio of 1000:1.
  • the product obtained by hydrogenation refining is subjected to atmospheric and vacuum distillation, and the fraction at 280-350°C is taken as base oil B.
  • paraffin-based crude oil is subjected to atmospheric and vacuum distillation to obtain a distillate oil with a distillation range of 300-420°C, which is then subjected to hydrogenation treatment, isomerization decondensation, and hydrogenation supplementary refining in sequence under the following conditions:
  • Hydrogenation treatment The catalyst is supported by alumina and loaded with 0.5 wt% nickel.
  • the conditions include: pressure of 17.0 ⁇ 0.5 MPa, temperature of 340 ⁇ 5°C, space velocity of 1.0 ⁇ 0.1 h -1 , and hydrogen-to-oil volume ratio of 1000:1.
  • Heterogeneous decondensation The catalyst is supported by zirconium oxide and loaded with 0.4wt% iridium.
  • the conditions include: pressure 17.0 ⁇ 0.5MPa, temperature 320 ⁇ 5°C, space velocity 0.8 ⁇ 0.1h -1 , hydrogen to oil volume ratio 1000:1.
  • Hydrogenation supplementary refining The catalyst is supported by silicate and loaded with 0.6 wt% rhodium.
  • the conditions include: pressure of 17.0 ⁇ 0.5 MPa, temperature of 310 ⁇ 5°C, space velocity of 2.0 ⁇ 0.1 h -1 , and hydrogen-to-oil volume ratio of 1000:1.
  • the product obtained by hydrogenation refining is subjected to atmospheric and vacuum distillation, and the fraction at 290-350°C is taken as base oil C.
  • base oil A The properties of base oil A, base oil B and base oil C are shown in Table 1.
  • the aromatic hydrocarbons with a CA value produced by base oil A are monocyclic aromatic hydrocarbons.
  • Comparative Example a Naphthenic crude oil is subjected to regular vacuum distillation (the conditions are the same as above) to obtain a naphthenic distillate oil with a distillation range of 260-450°C, which is then subjected to a solvent refining combined process of "hydrogenation pre-refining-furfural refining-white clay supplementary refining" to obtain a distillate oil with a temperature of 270-410°C.
  • Comparative Example b The cycloalkyl crude oil was subjected to atmospheric and vacuum distillation (the conditions were the same as those described above) to obtain a cycloalkyl distillate oil having a distillation range of 290-410°C, which was then subjected to hydrogenation treatment, isomerization decondensation, and hydrogenation supplementary refining in sequence under a hydrogen partial pressure of 6 MPa (the temperature, hydrogen-to-oil ratio, space velocity, and catalyst of the three stages were the same as those of the production conditions of base oil A), and the product obtained by hydrogenation supplementary refining was subjected to atmospheric and vacuum distillation to obtain a distillate oil having a distillation range of 270-410°C.
  • the base oils A, B and C provided by the present invention are obtained according to the specific method of the present invention, and have different properties from the products obtained by the prior art (Comparative Examples a and b), are more environmentally friendly, have lower pour points, and have less impurities such as sulfur and nitrogen.
  • the atomic content is 0.
  • the first cycloalkyl oil (base oil A), the second cycloalkyl oil (base oil B) and the paraffin base oil (base oil C) are blended according to the formula and amount in Table 2, the blending temperature is 50-60° C., and after being fully mixed, a base oil is obtained;
  • the coolants prepared in Examples 1 to 4 are all colorless and transparent in appearance, have good fluidity at 40°C and low temperatures, have excellent fire safety, thermal conductivity, insulation performance (the breakdown voltage at low temperatures is not weakened), oxidation stability, are non-corrosive, and have a low dielectric constant, and do not interfere with the signals of IT equipment immersed therein.
  • the server power cables, data cables, network cables and other cables as well as various accessories of the liquid cooling pipeline were immersed in the coolants prepared in Examples 1 to 4 to examine the compatibility of the materials and the coolants.
  • the test temperature The temperature was 60°C, the test time was 6 months, and the material condition was checked every week. The test results after 6 months of immersion are shown in Table 5.
  • the coolants prepared in Examples 1 to 4 were poured into the server respectively, and the server CPU load was 100% immersed in the coolant to test the overall compatibility of the coolant with the server.
  • the test time was 16 months, and the server parameters were monitored regularly every week. The test results are shown in Table 6.
  • the coolant prepared in Example 1 to Example 4 has low volatility, with an annual volatility loss of about 2wt%, which does not affect the operation and maintenance of the server; the coolant is not easy to absorb water, and the water content has no obvious change during the 16-month operation process, and it is safe to use; it is compatible with the liquid cooling system materials and meets the long-term use requirements of the equipment; the server is in good operating condition, and all parameters are normal, indicating that the coolant has good thermal conductivity and high heat dissipation efficiency.
  • any factor of physical evaporation (temperature increase causes liquid to gasify) and chemical evaporation (oxidation reaction causes light component gas to be generated) will increase the evaporation loss of the dielectric coolant.
  • the annual volatilization loss of the coolant of the present invention is small, indicating that its physical evaporation and chemical evaporation are both very small, further indicating that its antioxidant formula is suitable for making the coolant have good oxidation stability.
  • Example 2 The method of Example 2 is followed, except that modified nano magnesium hydroxide is not added.
  • the autoignition point is an important indicator for characterizing the flame retardant properties of the coolant
  • the breakdown voltage is an important indicator for characterizing the electrical properties (insulation properties) of the coolant.
  • the autoignition point and the breakdown voltage at room temperature and low temperature of Example 2 are much higher than those of Comparative Example 1 without modified nano-magnesium hydroxide, indicating that the modified nano-magnesium hydroxide of the present invention has greatly improved the flame retardant properties and electrical properties of the coolant.
  • the dielectric coolant of the present invention can be applied in the field of battery cooling, and the batteries include energy storage batteries, new energy vehicle batteries and other batteries that can be cooled by liquid.
  • the dielectric coolant of the present invention When used as a battery coolant, it has good oxidation stability, is non-corrosive, avoids the reaction between the coolant and the battery shell, and has good fire safety performance, thermal conductivity and insulation performance.

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Abstract

本发明公开了一种介电冷却液及其制备方法与应用。该介电冷却液包括基础油和添加剂；基础油与添加剂的质量比为100:2-12；添加剂包括抗氧剂、线缆增容剂和改性纳米材料；基础油包括环烷基油和石蜡基油，环烷基基础油的含量不低于60wt％，石蜡基基础油的含量不低于20wt％，环烷基基础油和石蜡基基础油的总量为100wt％；改性纳米材料为改性纳米氢氧化镁和改性纳米氢氧化铝中的至少一种，改性纳米材料为基础油质量的1-5wt％。该冷却液无色透明，具有良好的流动性能、防火安全性能、导热性能、绝缘性能、氧化安定性能和环保友好性，无腐蚀性，与IT设备液冷系统材料的兼容性良好，使用过程中稳定性好，能够应用于IT设备的浸没式或喷淋式等直接接触式冷却中。

Description

介电冷却液及其制备方法与应用
相关申请的交叉引用
本申请要求2022年11月07日提交的中国专利申请202211386652.4的权益，该申请的内容通过引用被合并于本文。
技术领域
本发明属于电子器件液冷技术领域，具体属于一种介电冷却液、制备方法及其应用。
背景技术
人工智能、云计算、大数据和区块链等技术的创新发展，以及5G通信时代的到来，使得计算机技术飞速发展。为了应对网络处理性能的挑战，IT设备不断提升自身处理能力和集成度，带来了功率密度的节节攀升，这些变化除了带来巨额能耗问题以外，高热密度也给制冷设备和技术提出了更高要求。
传统风冷技术面对高热密度场景呈现瓶颈，散热效率已经跟不上计算效率。尽管业界不停地创新风冷系统，但是空气的载热能力远远低于液体，液体的冷却能力是空气的1000-3000倍。液冷技术具有高效、能量损耗低、部署对建筑物依赖度低以及静音安全等特点，相对于风冷技术具有无法比拟的技术优势，是一种可以适用于需要大幅度提高计算能力、能源效率和部署密度等场景的优秀散热解决方案，可满足场地电力容量不足条件下部署更高的密度。因此，当风冷面对高热已经力不从心时，液冷技术逐渐从幕后走向前台，引起行业的普遍关注。
简单来说，液冷散热的原理就是采用热对流或热传导的方式，通过液体的浸 没或流动将服务器散出的热量带走。服务器的液冷方式主要有冷板式液冷、浸没式液冷和喷淋式液冷。
目前，液冷技术采用的冷却液主要有水和氟化液，其中：水是非绝缘体，只能应用于非直接接触型冷板式液冷技术中，一旦发生泄漏，会对IT设备造成致命损害；氟化液是目前浸没式应用最广泛的直接接触型冷却液，但价格昂贵，而且易挥发，使用成本高，密度大，对建筑物承重要求高。因为水和氟化液作为冷却液有上述缺点，所以相关行业积极研究和探索油类冷却液在直接接触型液冷中的使用，其中大多是关于合成油型和硅油型冷却液的研究。
CN 110862806 A公开了以二甲基硅油、天然酯类油或合成酯类油为基础油并加入抗氧剂、分散剂制备电子器件冷却液。
CN 113861948 A公开了以消泡剂、油性环氧树脂、分散剂、硅氧烷、闪点提高剂、端羟基聚丁二烯为原料制备的一种浸没式液冷冷却液。虽然合成油或硅油比氟化液成本低，但它们的价格仍然较贵，相比之下，天然石油的馏分油价格低廉，作为IT设备冷却液使用有很好的应用前景。
现有的IT设备冷却液的技术中，CN 107502309B公开了一种冷却液及其制备方法，其通过在传统的矿物型基础油中添加微量的抗氧剂、消泡剂和分散剂制备得到冷却液，能够适用于IT设备在开放式环境中的浸没式直接冷却。但是，该冷却液环保性能差、击穿电压仅为30kV(绝缘性能差)、阻燃性能差，且IT设备的线缆在冷却液中长期浸泡后，增塑剂易析出而导致线缆变硬。
综上所述，现有技术中的冷却液存在价格昂贵、环保性能差、绝缘性能差、阻燃性能差或增塑剂易析出的问题。
发明内容
为了解决现有技术的电子设备冷却液存在绝缘性能差、阻燃性能差或增塑剂易析出的问题，本发明提供一种介电冷却液、制备方法及其应用。该冷却液的原料易得且制备工艺简单成本低，冷却液为无色透明，具有良好的流动性能、防火安全性能、导热性能、绝缘性能和氧化安定性能，无毒、环保友好，无腐蚀性，与IT设备液冷系统材料的兼容性良好，使用过程中稳定性好，能够应用于IT设备的浸没式或喷淋式等直接接触式冷却中。
为实现上述目的，本发明第一方面提供一种介电冷却液，其中，该介电冷却液包括基础油和添加剂；
其中，所述基础油与添加剂的质量比为100:2-12；所述添加剂包括抗氧剂、线缆增容剂和改性纳米材料；
所述基础油包括环烷基基础油和石蜡基基础油，所述环烷基基础油的含量不低于60wt％，所述石蜡基基础油的含量不低于20wt％，环烷基基础油和石蜡基基础油的总量为100wt％；
所述改性纳米材料为改性纳米氢氧化镁和改性纳米氢氧化铝中的至少一种，所述改性纳米材料为基础油质量的1-5wt％。
本发明第二方面提供一种介电冷却液的制备方法，其中，所述方法包括以下过程，
将含量不低于60wt％的环烷基基础油和含量不低于20wt％的石蜡基基础油在50-60℃下充分调匀后得到介电冷却液的基础油；
向所述基础油中依次加入抗氧剂、线缆增容剂和改性纳米材料，再在50-60℃下加热并搅拌至澄清透明，冷却至室温后，过滤得到介电冷却液。
本发明第三方面提供一种介电冷却液的应用，所述介电冷却液应用于IT设备或电池冷却领域。
通过上述技术方案，与现有技术相比，本发明具有以下有益的技术效果：
本发明通过向由环烷基基础油和石蜡基基础油经调合而得的基础油中添加抗氧剂、线缆增容剂和改性纳米材料制备得到介电冷却液，其中：环烷基基础油和石蜡基基础油中的硫、氮等杂原子含量为0，无毒，环保友好，对添加剂和使用后可能产生的氧化物溶解性好，稳定性和安定性好；抗氧剂提高了介电冷却液的氧化安定性能；线缆增容剂提高了介电冷却液与线缆的兼容性，使线缆在介电冷却液中长期浸泡之后，线缆的增塑剂不会析出，线缆不会变硬；纳米材料改善了介电冷却液的阻燃性能、导热性能和绝缘性能。本发明研制的介电冷却液为无色透明，40℃运动粘度为4-15mm2/s，倾点≤-60℃，在40℃和低温下的流动性能均很好，具有良好的防火安全性能、导热性能、绝缘性能、氧化安定性能和环保友好性，无腐蚀性，与IT设备液冷系统材料的兼容性良好，使用过程中稳定性好，能够应用于IT设备的浸没式或喷淋式等直接接触式冷却中。
本发明提供的介电冷却液的制备方法中，介电冷却液以天然石油的馏分油经深度加氢后的产物为基础油，所涉及的工艺过程简单、环保、收率高、成本低，所述组合物可以达到与其它同类合成型介电冷却液相同的性能，且比合成油型或硅油型冷却液更易制取、经济价值更高，易实现工业化规模生产。
具体实施方式
在本文中所披露的范围的端点和任何值都不限于该精确的范围或值，这些范围或值应当理解为包含接近这些范围或值的值。对于数值范围来说，各个范围的 端点值之间、各个范围的端点值和单独的点值之间，以及单独的点值之间可以彼此组合而得到一个或多个新的数值范围，这些数值范围应被视为在本文中具体公开。
本发明第一方面提供一种介电冷却液，其中，所述介电冷却液包括基础油和添加剂；其中，所述基础油与添加剂的质量比为100:2-12；所述添加剂包括抗氧剂、线缆增容剂和改性纳米材料；所述基础油包括环烷基基础油和石蜡基基础油，所述基础油中，所述环烷基基础油的含量不低于60wt％，所述石蜡基基础油的含量不低于20wt％，环烷基基础油和石蜡基基础油的总量为100wt％；所述改性纳米材料为改性纳米氢氧化镁和改性纳米氢氧化铝中的至少一种，所述改性纳米材料为基础油质量的1-5wt％。
本发明中，所述基础油是以属于矿物油的天然石油为原料(具体可以来自环烷基原油和石蜡基原油)，经进一步加工处理而得，仍属于矿物油。
本发明中，将来自环烷基原油的馏分油和来自石蜡基原油的馏分油各自进行高压加氢(或深度加氢)，相应分别得到本发明中的环烷基基础油和石蜡基基础油。
本发明中，先将环烷基原油经常减压蒸馏，得到馏程为260-450℃的环烷基原油馏分油，然后进一步在14-18MPa的氢分压下依次经过加氢处理、异构降凝、加氢补充精制，最后再将加氢补充精制而得的产物进行常减压蒸馏，取270-410℃的馏分油作为本发明的所述介电冷却液中的环烷基基础油。
本发明中，先将石蜡基原油经常减压蒸馏，得到馏程为260-480℃的石蜡基原油馏分油，然后进一步在14-18MPa的氢分压下依次经过加氢处理、异构降凝、加氢补充精，最后再将加氢补充精制而得的产物进行常减压蒸馏，取270-410℃ 的馏分油作为本发明的所述介电冷却液中的石蜡基基础油。
本发明中，将环烷基原油或石蜡基原油分别进行常减压蒸馏(依次进行常压蒸馏和减压蒸馏)，条件可以包括：常压蒸馏温度为350-390℃，压力为0.1-0.2MPa；减压蒸馏温度为350-420℃，压力<11kPa；分别相应得到环烷基原油馏分油或石蜡基原油馏分油记为原料油I。制备所述环烷基基础油或石蜡基基础油的加氢处理的条件包括：加氢温度为300-400℃、原料油I的重时空速为0.7-1.4h-1、氢油(氢气与原料油I)的体积比为900-2800:1，其中，催化剂为氧化铝为载体，Ni和/或Mo为活性组分，活性组分含量为0.2-1.5wt％。分别得到环烷基的加氢处理油或石蜡基的加氢处理油，记为原料油II。
本发明中，异构降凝的条件包括：异构降凝温度为310-390℃、原料油II的重时空速为0.2-0.9h-1、氢油(氢气与原料油II)的体积比为900-2200:1，其中，催化剂以氧化锆为载体，负载VIII族贵金属(作为活性组分，如负载铑和/或铱)0.2-1.2wt％。分别得到环烷基的降凝油或石蜡基的降凝油，记为原料油III。
本发明中，加氢补充精制的条件包括：精制温度为200-340℃、原料油III的重时空速为1.6-2.8h-1、氢油(氢气与原料油III)的体积比为900-2200:1，其中，催化剂以硅酸盐为载体，负载VIII族贵金属(作为活性组分)铑和/或铱0.4-1.5wt％。分别得到环烷基基础油或石蜡基基础油。
根据本发明的研究，所述基础油中，所述环烷基基础油的含量一般可以为60-80wt％，所述石蜡基基础油的含量可以为20-40wt％。
进一步地，本发明中，所述环烷基基础油包括第一环烷基油和第二环烷基油，其中，基于所述基础油的总量，所述第一环烷基油在基础油中的含量为0-60wt％，所述第二环烷基油在基础油中的含量为20-60wt％。第一环烷基油和第二环烷基 油的总量等于所述环烷基基础油在所述基础油中的含量。
本发明中，所述第一环烷基油通过以下方法获得：
将环烷基原油经常减压蒸馏，得到馏程为290-410℃的环烷基馏分油，然后在14-18MPa的氢分压下，依次经过加氢处理、异构降凝、加氢补充精制，再将加氢补充精制而得的产物进行常减压蒸馏，取270-410℃馏分作为所述第一环烷基油；其中，
加氢处理的条件包括：加氢温度为300-360℃、重时空速为0.7-1.4h-1、氢油体积比为900-2800:1；
异构降凝的条件包括：异构降凝温度为310-360℃、重时空速为0.2-0.9h-1、氢油体积比为900-2200:1；
加氢补充精制的条件包括：精制温度为200-340℃、重时空速为1.6-2.8h-1、氢油体积比为900-2200:1。
本发明中，所述第二环烷基油通过以下方法获得：
将环烷基原油经常减压蒸馏，得到馏程为280-400℃的环烷基馏分油，然后在14-18MPa的氢分压下，依次经过加氢处理、异构降凝、加氢补充精制，再将加氢补充精制而得的产物进行常减压蒸馏，取270-410℃馏分作为所述第二环烷基油；其中，
加氢处理的条件包括：加氢温度为330-400℃、重时空速为0.7-1.4h-1、氢油体积比为900-2800:1；
异构降凝的条件包括：异构降凝温度为330-390℃、重时空速为0.2-0.9h-1、氢油体积比为900-2200:1；
加氢补充精制的条件包括：精制温度为200-340℃、重时空速为1.6-2.8h-1、氢油体积比为900-2200:1。
上述第一环烷基油(以下记为基础油A)、第二环烷基油(以下记为基础油B)和石蜡基基础油(以下记为基础油C)中，基础油A中硫、氮等杂原子含量为0，含有的芳烃环数最多为一环，无毒，环保友好，馏程为270-410℃，倾点为-50℃至-40℃；基础油B中硫、氮等杂原子含量为0，无芳烃，无毒，环保友好，馏程为270-410℃，倾点为-70℃至-60℃；基础油C中硫、氮等杂原子含量为0，无芳烃，无毒，环保友好，馏程为270-410℃，倾点为-70℃至-60℃。
高压加氢可以脱除原油馏分油中的硫、氮、氧等杂原子，对不饱和烃(尤其是稠环芳烃)加氢，生成稳定性好的不含杂原子的烷烃和环烷烃(环烷烃对添加剂和使用过程中可能产生的氧化物溶解性好)，进一步改善冷却液基础油的安定性和环保友好性能，同时保留第一环烷基基础油适宜含量的一环芳烃，以进一步提高冷却液基础油的溶解性，且一环芳烃不影响环保友好性，高压加氢中的异构降凝将直连烷烃变为异构烷烃，改善了冷却液的倾点等低温性能。
本发明采用石蜡基原油的常减压适宜馏分段的馏分油和环烷基原油的常减压适宜馏分段的馏分油作为原料，分别经过合理工艺条件下的加氢处理、异构降凝、加氢补充精制三段高压加氢处理，然后将制备的适宜馏分的环烷基基础油和石蜡基基础油以合适比例调合作为介电冷却液基础油，以调整冷却液基础油的碳型结构，改善冷却液的工况温度40℃和低温下的流动性能、稳定性能和环保友好性能。
为了进一步提高本发明的介电冷却液的使用性能，在本发明的具体实施过程中，上述介电冷却液还包括添加剂，基础油与添加剂的质量比为100:2-12。
具体地，添加剂包括抗氧剂、线缆增容剂和改性纳米材料。
抗氧剂可以改善介电冷却液的氧化安定性能，综合考虑介电冷却液的性能以 及成本等因素，抗氧剂的用量一般可以为基础油质量的0.2-0.6wt％。
具体地，抗氧剂为2,6-二叔丁基对甲酚、2,6-二叔丁基酚和烷基二苯胺中的至少一种。
线缆增容剂可以提高电线网线等线缆在介电冷却液中的兼容性，使线缆在40-60℃介电冷却液中长期浸泡之后，线缆的增塑剂不会析出，线缆不会变硬。
具体地，线缆增容剂包括油性环氧树脂和分散剂，油性环氧树脂和分散剂相互作用，共同提高线缆在介电冷却液中的兼容性。具体实施时，油性环氧树脂用量为基础油质量的1-5wt％，分散剂的用量为基础油质量的0.03-0.1wt％。油性环氧树脂可以为商购的环氧树脂E-44。
具体地，分散剂为毕克BYK-2152分散剂和毕克BYK-R605分散剂中的至少一种，商购自维波斯新材料公司。
纳米材料可以改善介电冷却液的阻燃性能、导热性能和电性能，跟普通纳米材料相比，改性纳米材料除了具有以上优点外，更为突出的优点是在介电冷却液中分散性很好。本发明所采用的改性纳米材料为市售商品，改性纳米材料的用量一般可以为基础油质量的1-5wt％。所述改性纳米材料可以是以表面活性剂改性的纳米材料，表面活性剂可以例如是磷酸酯类表面活性剂。所述改性纳米材料中，所述表面活性剂的含量为1-10wt％。
具体地，改性纳米材料为改性纳米氢氧化镁和改性纳米氢氧化铝中的至少一种。改性纳米氢氧化镁和改性纳米氢氧化铝的形状为球形，平均粒径为10-50nm，比表面积为30-50m2/g，在冷却液中的分散稳定性好，不挥发。
本发明中，介电冷却液的40℃运动粘度为4-15mm2/s，倾点≤-60℃，因此，在40℃和低温下的流动性能均很好。
本发明第二方面提供一种上述介电冷却液的制备方法，其中，所述方法包括以下过程：将含量不低于60wt％的环烷基基础油和含量不低于20wt％的石蜡基基础油在50-60℃下充分调匀后得到介电冷却液的基础油；向所述基础油中依次加入抗氧剂、油性环氧树脂、分散剂和改性纳米材料，再在50-60℃下加热并搅拌至澄清透明，冷却至室温后，过滤得到介电冷却液。
本发明的介电冷却液，所述基础油中，所述环烷基基础油和石蜡基基础油的总量为100wt％。本发明通过向由环烷基基础油和石蜡基基础油调合的基础油中添加抗氧剂、线缆增容剂和改性纳米材料制备得到介电冷却液，其中：环烷基基础油和石蜡基基础油的硫、氮等杂原子含量为0，无毒，环保友好，对添加剂和使用后可能产生的氧化物溶解性好，稳定性和安定性好；抗氧剂提高了介电冷却液的氧化安定性能；线缆增容剂提高了介电冷却液与线缆的兼容性；纳米材料改善了介电冷却液的阻燃性能、导热性能和电性能。本发明研制的介电冷却液无色透明，40℃运动粘度为4-15mm2/s，倾点≤-60℃，在40℃和低温下的流动性能均很好，具有良好的防火安全性能、导热性能、绝缘性能、氧化安定性能和环保友好性，无腐蚀性，与IT设备液冷系统材料的兼容性良好，使用过程中稳定性好，能够应用于IT设备的浸没式或喷淋式等直接接触式冷却中。本发明提供的介电冷却液以天然石油馏分油深度加氢后的产物为基础油，所涉及的工艺过程简单、环保、收率高、成本低，所述组合物可以达到与其它同类合成型介电冷却液相同的性能，且比合成油型或硅油型冷却液更易制取、经济价值更高，易实现工业化规模生产。
本发明中，所述环烷基基础油和石蜡基基础油的制得如前所述，不再赘述。其中，如前述制备所述第一环烷基油和第二环烷基油，调合获得所述环烷基基础 油，再与石蜡基基础油调合得到所述基础油。所述第一环烷基油和第二环烷基油的投料满足基于所述基础油的总量，所述第一环烷基油在基础油中的含量为0-60wt％，所述第二环烷基油在基础油中的含量为20-60wt％。且第一环烷基油和第二环烷基油的总量等于所述环烷基基础油在所述基础油中的含量。所述石蜡基基础油的用量满足，基于所述基础油的总量，所述基础油中，所述环烷基基础油的含量不低于60wt％，所述石蜡基基础油的含量不低于20wt％，环烷基基础油和石蜡基基础油的总量为100wt％
本发明第三方面提供一种介电冷却液的应用，所述介电冷却液应用于IT设备或电池冷却领域。
为了进一步说明本发明，下面通过以下实施例进行详细说明。
制备例1
用于说明第一环烷基油的制备。
将环烷基原油进行常减压蒸馏，得到馏程为290-410℃的馏分油依次进行加氢处理、异构降凝、加氢补充精制，条件如下：
加氢处理：催化剂以氧化铝为载体，负载镍0.5wt％，条件包括：压力为15.0±0.5MPa，温度为320±5℃，空速为1.0±0.1h-1，氢油体积比1000:1。
异构降凝：催化剂以氧化锆为载体，负载铱0.4wt％；条件包括：压力为15.0±0.5MPa，温度为320±5℃，空速为0.8±0.1h-1，氢油体积比1000:1。
加氢补充精制：催化剂以硅酸盐为载体，负载铑0.6wt％；条件包括：压力为15.0±0.5MPa，温度为310±5℃，空速为2.0±0.1h-1，氢油体积比1000:1。
对加氢补充精制而得的产物进行常减压蒸馏，取290-370℃馏分作为基础油 A。
制备例2
用于说明第二环烷基油的制备。
将环烷基原油进行常减压蒸馏，得到馏程为280-400℃的馏分油依次进行加氢处理、异构降凝、加氢补充精制，条件如下：
加氢处理：催化剂以氧化铝为载体，负载镍0.5wt％，条件包括：压力为17.0±0.5MPa，温度为340±5℃，空速为1.0±0.1h-1，氢油体积比1000:1。
异构降凝：催化剂以氧化锆为载体，负载铱0.4wt％，条件包括：压力为17.0±0.5MPa，温度为340±5℃，空速为0.8±0.1h-1，氢油体积比1000:1。
加氢补充精制：催化剂以硅酸盐为载体，负载铑0.6wt％，条件包括：压力为17.0±0.5MPa，温度为310±5℃，空速为2.0±0.1h-1，氢油体积比1000:1。
对加氢补充精制而得的产物进行常减压蒸馏，取280-350℃馏分作为基础油B。
制备例3
用于说明石蜡基基础油的制备。
将石蜡基原油进行常减压蒸馏，得到馏程为300-420℃的馏分油依次进行加氢处理、异构降凝、加氢补充精制，条件如下：
加氢处理：催化剂以氧化铝为载体，负载镍0.5wt％，条件包括：压力为17.0±0.5MPa，温度为340±5℃，空速为1.0±0.1h-1，氢油体积比1000:1。
异构降凝：催化剂以氧化锆为载体，负载铱0.4wt％，条件包括：压力为 17.0±0.5MPa，温度为320±5℃，空速为0.8±0.1h-1，氢油体积比1000:1。
加氢补充精制：催化剂以硅酸盐为载体，负载铑0.6wt％，条件包括：压力为17.0±0.5MPa，温度为310±5℃，空速为2.0±0.1h-1，氢油体积比1000:1。
对加氢补充精制而得的产物进行常减压蒸馏，取290-350℃馏分作为基础油C。
基础油A、基础油B和基础油C的性质如表1所示。
表1
其中，基础油A产生CA值的芳烃为一环芳烃。
对比例a：环烷基原油经常减压蒸馏(条件与前述相同)，得到馏程为260-450℃的环烷基馏分油，然后经过溶剂精制组合工艺“加氢预精制-糠醛精制-白土补充精制”后，取270-410℃的馏分油。
对比例b：环烷基原油经常减压蒸馏(条件与前述相同)，得到的馏程为290-410℃的环烷基馏分油，然后在6MPa的氢分压下，依次经过加氢处理、异构降凝、加氢补充精制(该三段的温度、氢油比、空速、催化剂同基础油A的生产条件)，将加氢补充精制而得的产物进行常减压蒸馏，取270-410℃馏分油。
可见，本发明提供的基础油A、B和C，按照本发明的特定方法获得，性质与现有技术得到的产物(对比例a和b)不同，更环保，倾点更低，硫、氮等杂 原子含量为0。
以下实施例和对比例中，在没有特别说明的情况下，所有原料均为市售品。
实施例1-4
将第一环烷基油(基础油A)、第二环烷基油(基础油B)和石蜡基基础油(基础油C)按照表2中配方及用量进行调合，调合温度为50-60℃，充分调匀后，得到基础油；
向该基础油中依次加入抗氧剂、油性环氧树脂、分散剂和改性纳米材料，再在50-60℃下加热并搅拌至澄清透明，冷却至室温，过滤即得介电冷却液。
表2实施例1-实施例4的配方(添加剂为外加法)
对实施例1-实施例4各自制得的介电冷却液进行性质测试，测试方法见表3，测试结果见表4。
表3介电冷却液的性质测试方法

表4实施例1-实施例4冷却液的性质分析结果
从表4可以看出：实施例1-实施例4制得的冷却液的外观均为无色透明，在40℃和低温下的流动性能较好，具有优异的防火安全性、导热性能、绝缘性能(低温下的击穿电压没有减弱)、氧化安定性能，无腐蚀性，且介电常数较低，对浸泡在其中的IT设备信号无干扰。
将服务器电源线、数据线和网线等各种线缆以及液冷管路各种配件分别置于实施例1-实施例4制得的冷却液中浸泡，考察材料和冷却液的兼容性，试验温度 为60℃，试验时间6个月，每周检查材料情况。浸泡6个月后的试验结果如表5所示。
表5实施例1-实施例4制得的冷却液与各材料兼容性情况
从表5可以看出：实施例1-实施例4制得的冷却液与服务器电源线/数据线/网线和液冷管路的各种配件兼容性良好。
将实施例1-实施例4制得的冷却液分别倒入服务器中，让服务器CPU负载100％浸没在冷却液中运行，测试冷却液与服务器的整体兼容性，测试时间为16个月，每周定期监测服务器参数，试验结果如表6所示。
表6实施例1-实施例4制得的冷却液分别在服务器中装机的运行结果
从表6可以看出：实施例1-实施例4制得的冷却液挥发性小，年挥发损失在2wt％左右，不影响服务器的运维；冷却液不易吸水，16个月的运行过程中，含水量无明显变化，使用安全；与液冷系统材料兼容，满足设备长期使用需求；服务器运行状况良好，各项参数显示正常，表明冷却液导热性好、散热效率高。
物理蒸发(温度升高导致液体变气体)和化学蒸发(氧化反应导致轻组分气体产生)中的任一因素均会使介电冷却液的蒸发损失变大，本发明冷却液的年挥发损失小，说明其物理蒸发和化学蒸发均很小，进一步说明其抗氧剂配方适宜使冷却液的氧化安定性能好。
对比例1
按照实施例2的方法，不同之处在于：不加改性纳米氢氧化镁。
实施例2与对比例1的自燃点和击穿电压对比如表7所示。
表7实施例2与对比例1的自燃点和击穿电压对比

注：*室温，25±5℃。
自燃点是表征冷却液阻燃性能的重要指标，击穿电压是表征冷却液电性能(绝缘性能)的重要指标。从表7可以看出：实施例2的自燃点和室温、低温下的击穿电压均远远高于不加改性纳米氢氧化镁的对比例1，说明本发明的改性纳米氢氧化镁对冷却液的阻燃性能和电性能均有较大改善。
本发明的介电冷却液可应用在电池冷却领域，电池包括储能电池、新能源汽车电池等其它可以采用液体冷却的电池。本发明的介电冷却液作为电池冷却液使用时，具有良好的氧化安定性能，无腐蚀性，避免冷却液与电池外壳产生反应，具有良好的防火安全性能、导热性能和绝缘性能。

Claims (10)

  1. 一种介电冷却液，其特征在于，所述介电冷却液包括基础油和添加剂；
    其中，所述基础油与添加剂的质量比为100:2-12；所述添加剂包括抗氧剂、线缆增容剂和改性纳米材料；
    所述基础油包括环烷基基础油和石蜡基基础油，基于所述基础油的总量，所述基础油中，所述环烷基基础油的含量不低于60wt％，所述石蜡基基础油的含量不低于20wt％，环烷基基础油和石蜡基基础油的总量为100wt％；
    所述改性纳米材料为改性纳米氢氧化镁和改性纳米氢氧化铝中的至少一种，所述改性纳米材料为基础油质量的1-5wt％。
  2. 根据权利要求1所述的介电冷却液，其特征在于，基于所述基础油的总量，所述基础油中，所述环烷基基础油的含量范围为60-80wt％，所述石蜡基基础油的含量范围为20-40wt％。
  3. 根据权利要求1或2所述的介电冷却液，其特征在于，所述环烷基基础油包括第一环烷基油和第二环烷基油，其中，基于所述基础油的总量，所述第一环烷基油在基础油中的含量为0-60wt％，所述第二环烷基油在基础油中的含量为20-60wt％。
  4. 根据权利要求3所述的介电冷却液，其特征在于，所述第一环烷基油的倾点为-50℃至-40℃，第二环烷基油的倾点为-70℃至-60℃；石蜡基基础油的倾点为-70℃至-60℃。
  5. 根据权利要求3或4所述的介电冷却液，其特征在于，所述第一环烷基油、第二环烷基油和石蜡基基础油均经采用高压加氢或深度加氢而制得。
  6. 根据权利要求1-5中任意一项所述的介电冷却液，其特征在于，所述抗氧剂为2,6-二叔丁基对甲酚、2,6-二叔丁基酚和烷基二苯胺中的至少一种，所述抗氧剂的用量为基础油质量的0.2-0.6wt％。
  7. 根据权利要求1-6中任意一项所述的介电冷却液，其特征在于，所述线缆增容剂包括油性环氧树脂和分散剂，其中，所述油性环氧树脂为基础油质量的1-5wt％，所述分散剂的用量为基础油质量的0.03-0.1wt％。
  8. 根据权利要求7所述的介电冷却液，其特征在于，所述分散剂为毕克BYK-2152分散剂和毕克BYK-R605分散剂中的至少一种。
  9. 一种介电冷却液的制备方法，其特征在于，所述方法包括以下过程，
    将含量不低于60wt％的环烷基基础油和含量不低于20wt％的石蜡基基础油在50-60℃下充分调匀后得到介电冷却液的基础油；
    向所述基础油中依次加入抗氧剂、线缆增容剂和改性纳米材料，再在50-60℃下加热并搅拌至澄清透明，冷却至室温后，过滤得到介电冷却液。
  10. 一种介电冷却液的应用，其特征在于，所述介电冷却液应用于IT设备或电池冷却领域。
PCT/CN2023/129991 2022-11-07 2023-11-06 介电冷却液及其制备方法与应用 Ceased WO2024099277A1 (zh)

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