CN114250096A - Complex ester type nano refrigerator oil and preparation method thereof - Google Patents
Complex ester type nano refrigerator oil and preparation method thereof Download PDFInfo
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- CN114250096A CN114250096A CN202111442527.6A CN202111442527A CN114250096A CN 114250096 A CN114250096 A CN 114250096A CN 202111442527 A CN202111442527 A CN 202111442527A CN 114250096 A CN114250096 A CN 114250096A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
- C10M105/32—Esters
- C10M105/42—Complex esters, i.e. compounds containing at least three esterified carboxyl groups and derived from the combination of at least three different types of the following five types of compound: monohydroxy compounds, polyhydroxy compounds, monocarboxylic acids, polycarboxylic acids and hydroxy carboxylic acids
- C10M105/44—Complex esters, i.e. compounds containing at least three esterified carboxyl groups and derived from the combination of at least three different types of the following five types of compound: monohydroxy compounds, polyhydroxy compounds, monocarboxylic acids, polycarboxylic acids and hydroxy carboxylic acids derived from the combination of monocarboxylic acids, dicarboxylic acids and dihydroxy compounds only and having no free hydroxy or carboxyl groups
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/30—Complex esters, i.e. compounds containing at leasst three esterified carboxyl groups and derived from the combination of at least three different types of the following five types of compounds: monohydroxyl compounds, polyhydroxy xompounds, monocarboxylic acids, polycarboxylic acids or hydroxy carboxylic acids
- C10M2207/302—Complex esters, i.e. compounds containing at leasst three esterified carboxyl groups and derived from the combination of at least three different types of the following five types of compounds: monohydroxyl compounds, polyhydroxy xompounds, monocarboxylic acids, polycarboxylic acids or hydroxy carboxylic acids derived from the combination of monocarboxylic acids, dicarboxylic acids and dihydroxy compounds only and having no free hydroxy or carboxyl groups
- C10M2207/3025—Complex esters, i.e. compounds containing at leasst three esterified carboxyl groups and derived from the combination of at least three different types of the following five types of compounds: monohydroxyl compounds, polyhydroxy xompounds, monocarboxylic acids, polycarboxylic acids or hydroxy carboxylic acids derived from the combination of monocarboxylic acids, dicarboxylic acids and dihydroxy compounds only and having no free hydroxy or carboxyl groups used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/30—Refrigerators lubricants or compressors lubricants
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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Abstract
The invention discloses a complex ester type nanometer refrigerator oil and a preparation method thereof, wherein diethylene glycol, dibasic acid, a metal oxide nanometer material and a water carrying agent are mixed for a first step of esterification reaction; then, adding monobasic fatty acid with the carbon chain length of 5-12, and performing a second esterification reaction to obtain a reaction product; and finally, refining the reaction product to obtain the catalyst. The product has excellent lubricating property, good stability and good intermiscibility with refrigerant.
Description
Technical Field
The invention relates to complex ester type nanometer refrigerator oil and a preparation method thereof, in particular to complex ester type nanometer refrigerator oil. Belongs to the technical field of industrial lubricating oil.
Background
The refrigerator oil is special lubricating oil for the refrigeration compressor, and has the functions of lubrication, sealing, cooling and the like. The high-quality refrigerator oil has excellent lubricating property, viscosity-temperature property, oxidation stability and chemical stability, and also has good compatibility with refrigerants. With the updating of the refrigerant, the development of the refrigerating machine oil matched with the refrigerant not only influences the working efficiency and the service life of the compressor, but also is important for reducing the energy consumption.
The HFCs refrigerant refrigerating machine oil is roughly divided into two types of synthetic ester and polyether, and the two types of base oil have respective advantages and make up for respective defects through additive formulas. HFCs refrigerants are typically used primarily in refrigerators, household air conditioners, and automotive air conditioning systems. Polyethers were initially selected due to poor compatibility of mineral oil and alkylbenzenes with HFCs refrigerants. However, since the refrigerator employs a fully-enclosed compressor, the refrigerator oil is required to have high electrical insulation, and the use of polyether in the fully-enclosed compressor is challenging because of the inferior electrical insulation compared to other refrigerator oils, and the refrigerator oil manufacturers have turned to research on ester oils. The reliability test of the refrigerator reciprocating compressor proves that the ester oil has good reliability.
At present, the synthetic ester type refrigerator oil has the problems of poor viscosity-temperature performance and obviously poor compatibility with a refrigerant along with the increase of viscosity, and the complex ester is used as one of ester lubricating oil, researches show that the complex ester has the characteristics of high viscosity and excellent viscosity-temperature performance, and can be used as a viscosity regulator.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the complex ester type nanometer refrigerator oil and the preparation method thereof, and the complex ester type nanometer refrigerator oil has excellent lubricating property and good compatibility with refrigerant.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of complex ester type nanometer refrigerator oil comprises the following specific steps:
(1) firstly, mixing diethylene glycol, dibasic acid, a metal oxide nano material and a water carrying agent to carry out a first-step esterification reaction;
(2) then, adding monobasic fatty acid with the carbon chain length of 5-12, and performing a second esterification reaction to obtain a reaction product;
(3) and finally, refining the reaction product to obtain the complex ester type nano refrigerating machine oil.
Preferably, the molar ratio of the diethylene glycol to the dibasic acid to the monobasic fatty acid is 5-6: 3: 6-9.
Preferably, the dosage of the nano metal oxide and the water carrying agent is 1-1.5% and 35-45% of the mass of the dibasic acid respectively.
Preferably, in step (1), the dibasic acid is at least one selected from oxalic acid or adipic acid.
Preferably, in the step (1), the metal oxide nano material is nano zinc oxide or nano aluminum oxide.
Preferably, in the step (1), the metal oxide nano-material is prepared by the following method in parts by weight:
(A) firstly, 0.002-0.003 part of graphene oxide is ultrasonically dispersed in 15-20 parts of deionized water, then 8-10 parts of 0.02-0.04 mol/L manganese nitrate solution and 2-3 parts of 0.006-0.008 mol/L cerium nitrate solution are added, ultrasonic dispersion is continued to be uniform, then an ammonia water solution with the mass concentration of 25-28% is slowly dripped under the ultrasonic oscillation condition until the pH value is 8-10, 0.12-0.15 part of sodium borohydride is added, stirring reaction is carried out, precipitates are centrifugally taken, washed, dried and calcined, and the metal oxide-graphene composite material is obtained;
(B) and (B) ultrasonically dispersing the metal oxide-graphene composite material obtained in the step (A) into 12-15 parts of absolute ethyl alcohol, adding 0.05-0.07 part of furfural and 0.095-0.105 part of 3-aminopropyltriethoxysilane, stirring for reaction, and performing post-treatment to obtain the metal oxide nano material.
Further preferably, in the step (a), the process conditions of the stirring reaction are as follows: stirring and reacting for 2-3 hours at 80-85 ℃.
Further preferably, in the step (a), the calcination process conditions are as follows: calcining for 6-7 hours at 250-300 ℃ in an argon atmosphere.
Further preferably, in the step (B), the process conditions of the stirring reaction are as follows: stirring and reacting for 3-4 hours at 94-98 ℃.
Further preferably, in the step (B), the post-treatment includes: and (4) removing ethanol by rotary evaporation, washing for 2-3 times, and drying.
Preferably, in the step (1), the water carrying agent is selected from any one of toluene, xylene or petroleum ether.
Preferably, in the step (1), the first esterification reaction is carried out under the protection of high-purity nitrogen, and the nitrogen flow is 20-80 mL/min.
Preferably, in the step (1), the process conditions of the first esterification reaction are as follows: stirring and reacting for 150-170 minutes at 130-180 ℃.
Preferably, in the step (2), the monobasic fatty acid is at least one of valeric acid, caproic acid, enanthic acid, caprylic acid, pelargonic acid, capric acid, undecanoic acid or dodecanoic acid.
Preferably, in the step (2), the process conditions of the second esterification reaction are as follows: stirring and reacting for 100-120 minutes at 190-230 ℃.
Preferably, in the step (3), the specific method of the purification treatment is: and cooling the reaction product to 60-100 ℃, adding an adsorbent accounting for 0.5-5% of the mass of the reaction product, standing for adsorption, carrying out reduced pressure distillation, and filtering to obtain the catalyst.
More preferably, the adsorbent is selected from activated carbon or clay, and the standing adsorption time is 30-40 minutes.
Further preferably, the vacuum distillation method comprises the following steps: and carrying out reduced pressure distillation at the temperature of 200-240 ℃ and the vacuum degree of-0.095-0.100 MPa, and stopping heating until no fraction is generated.
The complex ester type nanometer refrigerator oil obtained by the preparation method is provided.
The invention has the beneficial effects that:
firstly, mixing diethylene glycol, dibasic acid, a metal oxide nano material and a water carrying agent to carry out a first-step esterification reaction; then, adding monobasic fatty acid with the carbon chain length of 5-12, and performing a second esterification reaction to obtain a reaction product; and finally, refining the reaction product to obtain the complex ester type nano refrigerating machine oil. The product has excellent lubricating property, good stability and good intermiscibility with refrigerant.
The added metal oxide nano material can play a catalytic role in the synthetic reaction process, and a part of metal oxide nano material can be contained in the final product, so that the performance of the refrigerating machine oil can be improved. The invention uses diethylene glycol as raw material alcohol, which can make the synthesized complex ester refrigerator oil have excellent low-temperature performance, and the organic alcohol with the relative hydroxyl number of the diethylene glycol more than 4 is easier to generate esterification reaction, and the compatibility with refrigerant is also better.
When the metal oxide nano material is screened, the novel metal oxide nano material is introduced by taking graphene oxide, manganese nitrate and cerium nitrate as raw materials. The core structure of the metal oxide nano material is a composite material consisting of nano manganese oxide, nano cerium oxide and graphene, and the surface of the composite material is modified by virtue of Schiff base generated by the reaction of furfural and 3-aminopropyltriethoxysilane, so that the compatibility in a system is further improved, and the product performance is improved.
Detailed Description
The present invention will be further illustrated by the following examples, which are intended to be merely illustrative and not limitative.
Example 1
A preparation method of complex ester type nanometer refrigerator oil comprises the following specific steps:
(1) firstly, 530.6g of diethylene glycol, 438.4g of adipic acid, 4.4g of nano zinc oxide and 153.4g of toluene are mixed for carrying out the first-step esterification reaction;
(2) then 865.2g of isooctanoic acid is added for the second esterification reaction to obtain a reaction product;
(3) and finally, refining the reaction product to obtain the complex ester type nano refrigerating machine oil.
In the step (1), the first step of esterification reaction is carried out under the protection of high-purity nitrogen, and the nitrogen flow is 20 mL/min.
In the step (1), the technological conditions of the first esterification reaction are as follows: the reaction was stirred at 130 ℃ for 150 minutes.
In the step (2), the process conditions of the second esterification reaction are as follows: the reaction was stirred at 190 ℃ for 100 minutes.
In the step (3), the specific method of the refining treatment is as follows: cooling the reaction product to 60 ℃, adding active carbon with the mass of 0.5 percent of that of the reaction product, standing and adsorbing for 30 minutes, distilling under reduced pressure, and filtering to obtain the product. The vacuum distillation method comprises the following steps: distilling under reduced pressure at 200 deg.C and vacuum degree of-0.095 MPa, and stopping heating until no distillate is produced.
Example 2
A preparation method of complex ester type nanometer refrigerator oil comprises the following specific steps:
(1) firstly, 636.7g of diethylene glycol, 438.4g of adipic acid, 6.5g of nano-alumina and 197.2g of petroleum ether are mixed for carrying out the first-step esterification reaction;
(2) then 1297.8g of isooctanoic acid is added for the second esterification reaction to obtain a reaction product;
(3) and finally, refining the reaction product to obtain the complex ester type nano refrigerating machine oil.
In the step (1), the first step of esterification reaction is carried out under the protection of high-purity nitrogen, and the nitrogen flow is 80 mL/min.
In the step (1), the technological conditions of the first esterification reaction are as follows: the reaction was stirred at 180 ℃ for 170 minutes.
In the step (2), the process conditions of the second esterification reaction are as follows: the reaction was stirred at 230 ℃ for 120 minutes.
In the step (3), the specific method of the refining treatment is as follows: cooling the reaction product to 100 ℃, adding argil accounting for 5% of the mass of the reaction product, standing and adsorbing for 40 minutes, distilling under reduced pressure, and filtering to obtain the product. The vacuum distillation method comprises the following steps: distilling under reduced pressure at 240 deg.C and vacuum degree of-0.100 MPa, and stopping heating until no distillate is produced.
Example 3
A preparation method of complex ester type nanometer refrigerator oil comprises the following specific steps:
(1) firstly, 600g of diethylene glycol, 438.4g of adipic acid, 5.5g of metal oxide nano material and 180g of xylene are mixed for carrying out first-step esterification reaction;
(2) then adding 1000g of isooctanoic acid for a second esterification reaction to obtain a reaction product;
(3) and finally, refining the reaction product to obtain the complex ester type nano refrigerating machine oil.
In the step (1), the metal oxide nano material is prepared by the following method:
(A) firstly, 0.003g of graphene oxide is ultrasonically dispersed in 20g of deionized water, then 10g of 0.04mol/L manganese nitrate solution and 3g of 0.008mol/L cerium nitrate solution are added, the ultrasonic dispersion is continued to be uniform, then ammonia water solution with the mass concentration of 28% is slowly dripped under the ultrasonic oscillation condition until the pH value is 10, 0.15g of sodium borohydride is added, the mixture is stirred and reacted for 3 hours at 85 ℃, the precipitate is centrifugally taken, washed, dried and calcined for 7 hours at 300 ℃, and the metal oxide-graphene composite material is obtained;
(B) and (2) ultrasonically dispersing the metal oxide-graphene composite material obtained in the step (A) in 15g of absolute ethyl alcohol, adding 0.07g of furfural and 0.105g of 3-aminopropyltriethoxysilane, stirring and reacting for 4 hours at 98 ℃, removing the ethyl alcohol by rotary evaporation, washing for 3 times, and drying to obtain the metal oxide nano material.
In the step (1), the first esterification reaction is carried out under the protection of high-purity nitrogen, and the nitrogen flow is 65 mL/min.
In the step (1), the technological conditions of the first esterification reaction are as follows: the reaction was stirred at 150 ℃ for 160 minutes.
In the step (2), the process conditions of the second esterification reaction are as follows: the reaction was stirred at 205 ℃ for 110 minutes.
In the step (3), the specific method of the refining treatment is as follows: cooling the reaction product to 80 ℃, adding active carbon with the mass of 2.5 percent of that of the reaction product, standing and adsorbing for 35 minutes, distilling under reduced pressure, and filtering to obtain the product. The vacuum distillation method comprises the following steps: distilling under reduced pressure at 220 deg.C and vacuum degree of-0.100 MPa, and stopping heating until no distillate is produced.
Example 4
A preparation method of complex ester type nanometer refrigerator oil comprises the following specific steps:
(1) firstly, 600g of diethylene glycol, 438.4g of adipic acid, 5.5g of metal oxide nano material and 180g of xylene are mixed for carrying out first-step esterification reaction;
(2) then adding 1000g of isooctanoic acid for a second esterification reaction to obtain a reaction product;
(3) and finally, refining the reaction product to obtain the complex ester type nano refrigerating machine oil.
In the step (1), the metal oxide nano material is prepared by the following method:
(A) firstly, 0.002g of graphene oxide is ultrasonically dispersed in 15g of deionized water, then 8g of 0.02mol/L manganese nitrate solution and 2g of 0.006mol/L cerium nitrate solution are added, ultrasonic dispersion is continued to be uniform, then an ammonia water solution with the mass concentration of 25% is slowly dripped under the ultrasonic oscillation condition until the pH value is 8, 0.12g of sodium borohydride is added, stirring reaction is carried out for 2 hours at 80 ℃, precipitates are centrifugally taken, washed, dried and calcined for 6 hours at 250 ℃, and a metal oxide-graphene composite material is obtained;
(B) and (2) ultrasonically dispersing the metal oxide-graphene composite material obtained in the step (A) in 12g of absolute ethyl alcohol, adding 0.05g of furfural and 0.095g of 3-aminopropyltriethoxysilane, stirring and reacting at 94 ℃ for 3 hours, removing the ethyl alcohol by rotary evaporation, washing for 2 times, and drying to obtain the metal oxide nano material.
In the step (1), the first esterification reaction is carried out under the protection of high-purity nitrogen, and the nitrogen flow is 65 mL/min.
In the step (1), the technological conditions of the first esterification reaction are as follows: the reaction was stirred at 150 ℃ for 160 minutes.
In the step (2), the process conditions of the second esterification reaction are as follows: the reaction was stirred at 205 ℃ for 110 minutes.
In the step (3), the specific method of the refining treatment is as follows: cooling the reaction product to 80 ℃, adding active carbon with the mass of 2.5 percent of that of the reaction product, standing and adsorbing for 35 minutes, distilling under reduced pressure, and filtering to obtain the product. The vacuum distillation method comprises the following steps: distilling under reduced pressure at 220 deg.C and vacuum degree of-0.100 MPa, and stopping heating until no distillate is produced.
Test examples
The results of the performance test of the complex ester type nano refrigerator oils obtained in examples 1 to 4 are shown in Table 1.
Wherein, the viscosity at 40 ℃ is referred to GB/T265-1988, the acid value is referred to GB/T7304-2014, and the oxidation stability is referred to SH/T0193.
The compatibility was examined with reference to SH/T0699, and R32 refrigerant was used as the refrigerant.
TABLE 1 Performance test results
As can be seen from table 1, the refrigerating machine oils obtained in examples 1 to 4 have high viscosity, low acid value, good stability, and good compatibility with refrigerants, and particularly, the examples 3 and 4 introduce new metal oxide nanomaterials, which are significantly superior in various properties.
The working volumes of the refrigerating machine oils obtained in examples 1 to 4 were 5.56cm3The same batch of connecting rod compressors (the connecting rod is made of aluminum alloy, the crankshaft is made of carbon steel, and the piston and the cylinder are made of cast iron) are subjected to a 500-hour accelerated life test, and the performance investigation results before and after the test are shown in table 2.
TABLE 2 Experimental results of 500-hour accelerated life of link type compressor
As can be seen from Table 2, the refrigerating machine oil obtained in examples 1 to 4 can greatly improve the service life of the link compressor.
Although the present invention has been described with reference to the specific embodiments, it is not intended to limit the scope of the present invention, and various modifications and variations can be made by those skilled in the art without inventive changes based on the technical solution of the present invention.
Claims (10)
1. A preparation method of complex ester type nanometer refrigerator oil is characterized by comprising the following specific steps:
(1) firstly, mixing diethylene glycol, dibasic acid, a metal oxide nano material and a water carrying agent to carry out a first-step esterification reaction;
(2) then, adding monobasic fatty acid with the carbon chain length of 5-12, and performing a second esterification reaction to obtain a reaction product;
(3) and finally, refining the reaction product to obtain the complex ester type nano refrigerating machine oil.
2. The method according to claim 1, wherein the molar ratio of diethylene glycol, dibasic acid, and monobasic fatty acid is 5 to 6: 3: 6-9.
3. The preparation method according to claim 1, wherein the amounts of the nano metal oxide and the water carrying agent are 1-1.5% and 35-45% of the mass of the dibasic acid, respectively.
4. The method according to claim 1, wherein in the step (1), the dibasic acid is at least one selected from the group consisting of oxalic acid and adipic acid.
5. The preparation method according to claim 1, wherein in the step (1), the metal oxide nanomaterial is nano zinc oxide or nano aluminum oxide.
6. The preparation method according to claim 1, wherein in the step (1), the water carrying agent is any one selected from toluene, xylene or petroleum ether.
7. The preparation method according to claim 1, wherein in the step (1), the first esterification reaction is performed under the protection of high-purity nitrogen, and the nitrogen flow is 20-80 mL/min.
8. The preparation method according to claim 1, wherein in the step (1), the process conditions of the first esterification reaction are as follows: stirring and reacting for 150-170 minutes at 130-180 ℃.
9. The method according to claim 1, wherein in the step (2), the process conditions of the second esterification reaction are as follows: stirring and reacting for 100-120 minutes at 190-230 ℃.
10. A complex ester type nanometer refrigerator oil obtained by the preparation method of any one of claims 1 to 9.
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