Ultralow-temperature anti-freezing isolation oil as well as preparation method and application thereof

By preparing ultra-low temperature antifreeze isolation oil, the chemical stability and low-temperature flowability of waste synthetic oil are used to solve the problem of poor antifreeze effect of water-soluble antifreeze at extremely low temperatures, and the dual effects of low-temperature antifreeze and waste oil resource utilization are achieved.

CN120442219APending Publication Date: 2025-08-08CHINA ENERGY LONGYUAN ENVIRONMENTAL PROTECTION CO LTD
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Patent Information

Application Number
CN202510844600.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-06-23
Publication Date
2025-08-08

AI Technical Summary

Technical Problem

The existing water-soluble antifreeze has limited antifreeze effect at extremely low temperatures, and the recycling and utilization of waste synthetic oil is insufficient, resulting in short-term and high cost of antifreeze.

Method used

Use waste synthetic oil as the main component, and add viscosity-reducing agents, antioxidants and antirust agents after removal of impurities and heating to reduce viscosity, ultra-low temperature antifreeze isolation oil is prepared to form a thin oil film to isolate moisture, meet the needs of low-temperature antifreeze, and use the chemical stability of waste synthetic oil to extend its service life.

Benefits of technology

It effectively prevents coal freezing at extremely low temperatures, reduces coating volume and costs, and provides a resource recycling and utilization method for waste synthetic oil, improving environmental and economic benefits.

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Abstract

The invention provides ultralow-temperature anti-freezing isolation oil as well as a preparation method and application thereof, and the ultralow-temperature anti-freezing isolation oil is a product prepared from a composition comprising the following components in parts by weight: 80-100 parts of waste synthetic oil and 5-20 parts of a viscosity reducer. The waste synthetic oil with high chemical stability and low pour point is selected as a raw material, and the prepared ultralow-temperature anti-freezing isolation oil can form a layer of waterproof oil film between coal and a compartment wall, so that the problems of short acting time and poor acting effect when a water-soluble anti-freezing solution is sprayed are effectively solved; meanwhile, a new resource recycling way can be realized by combining the advantages of the waste synthetic oil, and the method has relatively high environmental value and economic benefit.
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Description

Technical Field

[0001] The present invention relates to the technical field of antifreeze fluids, and in particular to an ultra-low temperature antifreeze isolation oil and a preparation method and application thereof. Background Art

[0002] Due to the way coal is mined and processed, commercial coal contains a certain amount of moisture, which is generally between 6% and 15%. The moisture content of clean coal at some loading stations can even reach 20% to 30%.

[0003] Given the current state of coal transportation, antifreeze spraying on trains must comply with the "Technical Conditions for Antifreeze Operations in Railway Coal Transportation" and relevant regulations. Currently, the antifreeze sprayed on railways is primarily water-soluble. At low temperatures, the remaining moisture in the coal is susceptible to phase change and crystallization, which can adhere to the train walls. Furthermore, the long transit time of coal degrades the antifreeze's effectiveness, posing a risk of freezing. Therefore, if antifreeze is applied to a train and not loaded for more than three hours, it must be re-sprayed before loading.

[0004] Chinese patent application CN106398528A discloses an ultra-low temperature nano antifreeze isolation emulsion and its preparation method, comprising 100 parts by weight of mineral oil and / or bio-oil, 0.1-1 parts by weight of additive A, 1-2 parts by weight of additive B, and 13-50 parts by weight of water. The additive A comprises ethylene / vinyl acetate copolymer, acrylate polymer, maleic anhydride copolymer, polyoxyethylene alkylamine, or a mixture of any two or more of the above, and the additive B comprises sorbitan fatty acid ester, polyglycerol fatty acid ester, polyoxyethylene fatty acid ester, isostearic acid monoglyceride, monoalkenyl succinimide, polyalkenyl succinimide, or a mixture of any two or more of the above. This ultra-low temperature nano antifreeze isolation emulsion is an oily substance with a low pour point, hydrophobicity, and low corrosiveness, and can effectively solve the problem of frozen coal trucks.

[0005] However, the antifreeze barrier emulsion prepared in the aforementioned patent application has limited antifreeze effectiveness in extreme environments with temperatures below -50°C. With the exception of alkylbenzene, which has a freezing point below -40°C, conventional bio-greases, white oil, diesel, kerosene, mineral-based lubricants, and base oils, all have freezing points between -10°C and 40°C. Therefore, the freezing point of the antifreeze barrier emulsion can only drop to -50°C at most. Furthermore, the aforementioned antifreeze barrier emulsion is essentially an oil-water mixture. Despite strict surface tension control, it still presents the risk of instability and demulsification during actual use, thus affecting its antifreeze effectiveness.

[0006] Synthetic oil refers to the base oil component of lubricating oil produced by chemical synthesis. It is also called synthetic lubricant and includes synthetic hydrocarbons, polyethers, polysiloxanes, fluorinated oils, etc. Compared with mineral oil, its molecular structure is generally highly symmetrical and regular, usually with a straight chain or branched structure, and rarely contains polar groups. Therefore, it is not easy to form crystals at low temperatures, thus having good viscosity-temperature and ultra-low temperature performance. It is generally used in gearboxes, hydraulic equipment, steam turbines, compressors, engines and other systems operating under extreme conditions, and can meet strict requirements in terms of long cycles and environmental protection. In addition, synthetic oil is prepared by chemical methods, has a single molecular structure, simple composition, good chemical stability, and low degree of deterioration after long-term use. Compared with traditional waste mineral oils and fats, it still has a higher resource recovery value. However, there is currently no better recycling method, and it is combined with waste mineral oils and fats for disposal as hazardous waste. Summary of the Invention

[0007] The purpose of the present invention is to provide an ultra-low temperature antifreeze isolation oil and its preparation method and application, so as to solve the problems of short action time and poor effect of spraying water-soluble antifreeze liquid and the recycling of waste synthetic oil.

[0008] In order to achieve one aspect of the above purpose, the present invention adopts the following technical solutions:

[0009] In a first aspect, the present invention provides an ultra-low temperature antifreeze isolation oil, which is a product prepared from a composition comprising the following components, in parts by weight: 80 to 100 parts of waste synthetic oil and 5 to 20 parts of a viscosity reducer.

[0010] In the present invention, the amount of the viscosity reducer is adjusted according to the different viscosity grades of the synthetic oil to meet the requirement of the thinnest oil film while ensuring the isolation and antifreeze requirements, thereby reducing the coating amount and lowering the coating cost. At the same time, according to the requirements of coal transportation and use, functional additives such as antioxidants and rust inhibitors suitable for waste synthetic oil can also be introduced to extend the service life of the antifreeze isolation oil.

[0011] In some specific embodiments, the present invention satisfies the requirement of the thinnest oil film by controlling the dynamic viscosity of the ultra-low temperature antifreeze isolation oil. For example, the dynamic viscosity range (20°C) of the ultra-low temperature antifreeze isolation oil is 14.5 to 17 mPa.s.

[0012] In some specific embodiments, the waste synthetic oil is waste synthetic oil that has been treated to remove impurities after use in gearboxes, hydraulic equipment, steam turbines, compressors, and engine systems.

[0013] In some specific embodiments, the waste synthetic oil has an ISO viscosity grade of 32 # , 46 # , 68 # One or more of .

[0014] In some specific embodiments, the viscosity reducing agent is a mixture of methyl silicone oil and dioctyl phthalate or methyl silicone oil and dibutyl phthalate; preferably, the dynamic viscosity of the methyl silicone oil is one of 5 mPa·s and 10 mPa·s, and the mass ratio of methyl silicone oil to dioctyl phthalate or methyl silicone oil to dibutyl phthalate is 6:4 to 9:1 according to the viscosity of the methyl silicone oil.

[0015] In some specific embodiments, the antifreeze isolation oil further includes an antioxidant, and the antioxidant includes one of diphenylamine and N-phenyl-α-naphthylamine.

[0016] In some specific embodiments, the antifreeze isolation oil further includes a rust inhibitor, and the rust inhibitor includes one of barium petroleum sulfonate, barium dinonylnaphthalene sulfonate, and aluminum stearate.

[0017] In a second aspect, the present invention provides a preparation method, which can produce the antifreeze isolation oil described in the first aspect, comprising the following steps:

[0018] S1: removing impurities from waste synthetic oil;

[0019] S2: heating the waste synthetic oil treated in step S1 to reduce its viscosity;

[0020] S3: adding viscosity reducing agents to the waste synthetic oil after viscosity reduction in step S2 in sequence, mixing them evenly, and allowing them to stand to room temperature to prepare ultra-low temperature antifreeze isolation oil.

[0021] In the present invention, after the waste synthetic oil is impurity-removed, degraded component particulate impurities, acidic substances, and organic matter can be removed, thereby improving the purity of the oil product and restoring the low-temperature performance of the waste oil.

[0022] In some specific embodiments, in step S1, the impurity removal treatment includes but is not limited to one or more operations of centrifugation, adsorption and fine filtration; preferably, the impurity removal treatment includes centrifugation, adsorption and fine filtration performed in sequence.

[0023] In the present invention, waste synthetic oil is subjected to centrifugation, adsorption, fine filtration and other operations to remove particulate impurities, acidic substances, organic matter and the like in the waste synthetic oil, thereby improving the quality of the waste synthetic oil and enabling it to be used as a raw material for antifreeze isolation oil.

[0024] In some specific embodiments, the centrifugal operation is used to remove large particle impurities, moisture and colloid to ensure the uniformity of the antifreeze isolation oil. Preferably, the conditions include: temperature controlled at 60-80°C, rotation speed at 6000-7000 r / min, and centrifugation time of not less than 30 min.

[0025] In some specific embodiments, the adsorption operation is used to remove acidic substances and prevent the acidity of the antifreeze isolation oil from corroding the vehicle compartment. Preferably, the conditions include: the amount of adsorbent diatomaceous earth input is 2 to 10 wt%, the adsorption temperature is 60 to 80°C, and the adsorption time is 20 to 40 minutes; the sedimentation temperature is 50 to 60°C, and the sedimentation time is not less than 4 hours.

[0026] In some specific embodiments, the fine filtration operation is used to remove residual adsorbent and colored substances, and a vibrating nanofiltration membrane assembly is used for testing. The preferred conditions include: a membrane pore size of 1-2 μm, a membrane area of 1 m 2 , PTFE material, temperature controlled at 60-70℃.

[0027] In some specific embodiments, the waste synthetic oil obtained after impurity removal has the following index ranges:

[0028] 32 # Synthetic oil: kinematic viscosity (40°C) 30-33 mm 2 / s, density (15℃) 0.83~0.86kg / L, acid value not exceeding 0.08mgKOH / g, pour point -48℃, flash point 220~235℃;

[0029] 46 # Synthetic oil: kinematic viscosity (40°C) 44-47 mm 2 / s, density (15℃) 0.85~0.88kg / L, acid value not exceeding 0.08mgKOH / g, pour point -45℃, flash point 230~240℃;

[0030] 68 # Synthetic oil: kinematic viscosity (40°C) 65-69 mm 2 / s, density (15℃) 0.86~0.88kg / L, acid value not exceeding 0.08mgKOH / g, pour point -42℃, flash point 250~260℃.

[0031] In some specific embodiments, in step S2, the heating and viscosity reduction comprises: heating the waste synthetic oil to 55-65°C.

[0032] In some specific embodiments, in step S3, antioxidants and rust inhibitors are also added.

[0033] In the present invention, after the waste synthetic oil is heated to reduce viscosity, it can be fully and evenly mixed with the antioxidant and the rust inhibitor at low viscosity, thereby improving fluidity and reducing coating amount.

[0034] In some specific embodiments, in step S3, the uniform mixing includes: stirring once after adding the viscosity reducer to the waste synthetic oil, stirring twice after adding the antioxidant, and stirring three times after adding the rust inhibitor.

[0035] In some specific embodiments, the rotation speed and time of the first stirring, second stirring and third stirring are respectively: 200-300 r / min, 40-60 min; 200-250 r / min, 10-15 min; 200-250 r / min, 15-20 min.

[0036] In some specific embodiments, the mixture comprising waste synthetic oil, viscosity reducer and antioxidant is heated to 75-80° C. before adding the rust inhibitor.

[0037] In a third aspect, the present invention further proposes an application of the antifreeze isolation oil prepared by the components described in the first aspect and the preparation method described in the second aspect in antifreeze of coal transportation in winter.

[0038] Preferably, before loading coal into the coal train carriage, apply 0.015-0.03 kg / m 2 Ultra-low temperature antifreeze isolation oil, the specific application amount should be adjusted appropriately according to the temperature and coal moisture content, for example 0.016kg / m 2 0.018kg / m 2 0.020kg / m 2 0.022kg / m 2 0.025kg / m 2 0.028kg / m 2 wait.

[0039] The ultra-low temperature antifreeze isolation oil prepared by the present invention can be applied in a lower amount than conventional application, and only one layer of oil film is needed to separate the coal and the box wall. That is, the present invention can ensure that the oil film is thin, and the antifreeze requirements can be met with less amount than conventional antifreeze isolation agents.

[0040] Compared with the prior art, the present invention has the following advantages:

[0041] The ultra-low-temperature antifreeze barrier oil prepared in this invention differs from conventional water-soluble antifreeze fluids in that it is primarily composed of treated waste synthetic oil. Leveraging its low pour point, good low-temperature fluidity, and defined viscosity, the ultra-low-temperature antifreeze barrier oil is sprayed onto the walls of the train, forming a liquid film between the coal and the train's interior, isolating moisture and preventing freezing. Compared to oil-water antifreeze barrier emulsions, ultra-low-temperature antifreeze barrier oil has simpler ingredients and can be prepared simply by reducing its viscosity. It eliminates the risk of demulsification and extends its service life.

[0042] In addition, the ultra-low temperature antifreeze isolation oil enters the boiler along with the coal, can be consumed in the form of fuel and generate calorific value, thus reducing the fuel cost to a certain extent.

[0043] Finally, the waste synthetic oil used in this invention, along with waste mineral oil, is classified as HW08 hazardous waste and managed as such. However, research has shown that waste synthetic oil exhibits minimal degradation and excellent chemical stability after long-term use, making it highly valuable for recycling compared to traditional waste mineral oils. This invention leverages the performance advantages of waste synthetic oil to produce ultra-low-temperature antifreeze barrier oil, providing a novel approach to resource recovery with high environmental and economic benefits.

[0044] Other features and advantages of the present invention will be described in detail through the following detailed description. DETAILED DESCRIPTION

[0045] The specific embodiments of the present invention are described in detail below. It should be understood that the following examples are only used to more clearly illustrate the technical solutions of the present invention, and are not intended to limit the scope of protection of the present invention. Various changes, modifications, substitutions, and variations made to these embodiments by those of ordinary skill in the art without departing from the principles and purpose of the present invention are intended to be included within the scope of protection of the present invention.

[0046] 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 approximate ranges or values. For numerical ranges, the endpoints of each range, the endpoints of each range and 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.

[0047] 1. Test method:

[0048] The test methods or reference standards for performance indicators such as viscosity, density, and pour point are as follows: the test methods for technical indicators such as kinematic viscosity, pour point, and flash point refer to the national standard "Special lubricants for wind turbines Part 3: Transmission gear oil" (GB / T33540.3-2017); the test method for acid value refers to GB / T 7304-2014; the test method for dynamic viscosity TB / T 3208-2023 and density refers to the industry standard "Technical Conditions for Antifreeze for Bulk Granular Cargo Transport" (SH / T 0068-2002).

[0049] 2. Source of raw materials:

[0050] The source of waste synthetic oil is: Mobil SHC 626 (68 # )、SHC 524(32 # )、525(46 # )、526(68 # Tellus S4 VX 32 # wait.

[0051] Unless otherwise specified, the "parts" of raw materials in each embodiment refer to "parts by mass".

[0052] The technical solution of the present invention is further described in detail below through examples.

[0053] The waste synthetic oil used in the embodiment of the present invention is subjected to impurity removal treatment according to the following steps:

[0054] Centrifuge, adsorb and fine filter the waste synthetic oil:

[0055] The centrifugal operation conditions include: temperature controlled at 80° C., rotation speed at 6800 r / min, and centrifugal time of 45 min.

[0056] The adsorption operation conditions include: the input amount of adsorbent diatomaceous earth is 8 wt%, the adsorption temperature is 70° C., the adsorption time is 30 minutes; the sedimentation temperature is 60° C., and the sedimentation time is 6 hours.

[0057] The fine filtration was tested using a vibrating nanofiltration membrane assembly. The operating conditions included: a membrane pore size of 1-2 μm and a membrane area of 1 m 2 , PTFE material, temperature controlled at 60℃.

[0058] Example 1

[0059] The ultra-low temperature antifreeze isolation oil is prepared from the following raw materials in parts by weight: 92 parts of waste synthetic oil, 8 parts of additive A, 3.5 parts of additive B, and 2.5 parts of additive C.

[0060] Specifically, the waste synthetic oil is 32 from hydraulic equipment that has been treated for impurities. # Waste synthetic oil, specific parameters are: kinematic viscosity (40℃) 30.2mm 2 / s, density (15℃) 0.856kg / L, acid value 0.08mgKOH / g, pour point -48℃, flash point 226℃.

[0061] Specifically, the additive A is a viscosity reducer, which is a mixture of methyl silicone oil and dioctyl phthalate, with a mass mixing ratio of 9:1. The methyl silicone oil has a dynamic viscosity of 5 mPa·s; the additive B is an antioxidant diphenylamine; and the additive C is a rust preventive barium dinonylnaphthalenesulfonate.

[0062] The preparation method of the ultra-low temperature antifreeze isolation oil comprises the following steps:

[0063] S1: centrifuging, adsorbing, and fine filtering the waste synthetic oil in sequence to obtain treated waste synthetic oil;

[0064] S2: Add the above waste synthetic oil to a 500 mL beaker and heat in a 60°C water bath to reduce viscosity;

[0065] S3: Add additive A to the beaker, rotate at 300 r / min, and stir thoroughly for 60 min;

[0066] S4: Continue to add additive B into the beaker, rotate at 200 r / min, and stir thoroughly for 10 minutes;

[0067] S5: Heat to 75°C, add additive C to the beaker, rotate at 200 r / min, and stir thoroughly for 15 minutes;

[0068] S6: Let it stand until it reaches room temperature to obtain ultra-low temperature antifreeze isolation oil.

[0069] Main technical indicators of the product: dynamic viscosity (20℃) 15.6mPa.s, density (20℃) 0.846g / cm 3 , pour point -54℃, and other indicators meet the requirements of TB / T 3208-2008 "Technical Conditions for Antifreeze Fluids for Bulk Granular Cargo Transport".

[0070] The application of the ultra-low temperature antifreeze isolation oil in the antifreeze of coal transportation in winter is investigated in the following manner:

[0071] Simulated carriage test: The simulated carriage is made at a ratio of 1:10 of the 80B carriage and is made of stainless steel.

[0072] Test conditions: temperature -40°C, coal moisture content 25%;

[0073] Test steps: ① Apply the above-mentioned ultra-low temperature antifreeze isolation oil on the bottom and inner wall of the simulated car, with a coating amount of 0.015kg / m 2 ; ② Load 200 kg of coal with a moisture content of 25% into the carriage; ③ Continue freezing for 36 hours and then stop; ④ Unload the coal.

[0074] Test results: The ultra-low temperature antifreeze isolation oil adheres to the wall well, has no frozen bottom, no sticking, and is easy to separate.

[0075] Example 2

[0076] The preparation method described in Example 1 was followed, except that the ultra-low temperature antifreeze isolation oil was made from the following raw materials in parts by weight: 88 parts of waste synthetic oil, 12 parts of additive A, 3.5 parts of additive B, and 2 parts of additive C.

[0077] Specifically, the waste synthetic oil is 32 from hydraulic equipment after impurity removal treatment. # Waste synthetic oil, specific parameters are: kinematic viscosity (40℃) 30.2mm 2 / s, density (15℃) 0.856kg / L, acid value 0.08mgKOH / g, pour point -48℃, flash point 226℃.

[0078] Specifically, the additive A is a viscosity reducer, which is a mixture of methyl silicone oil and dibutyl phthalate, with a mass mixing ratio of 8:2. The methyl silicone oil has a dynamic viscosity of 10 mPa·s; the additive B is an antioxidant diphenylamine; and the additive C is a rust preventive barium petroleum sulfonate.

[0079] Main technical indicators of the product: dynamic viscosity (20℃) 14.7mPa.s, density (20℃) 0.850g / cm 3 , pour point -54℃, and other indicators meet the requirements of TB / T 3208-2008 "Technical Conditions for Antifreeze Fluids for Bulk Granular Cargo Transport".

[0080] The test method described in Example 1 was followed, except that the freezing was continued for 42 h before stopping.

[0081] Test results: The ultra-low temperature antifreeze isolation oil adheres to the wall well, has no frozen bottom, no sticking, and is easy to separate.

[0082] Example 3

[0083] The preparation method and test method described in Example 1 were followed, except that the ultra-low temperature antifreeze isolation oil was made from the following raw materials in parts by weight: 84 parts of waste synthetic oil, 16 parts of additive A, 2.5 parts of additive B, and 2.5 parts of additive C.

[0084] Specifically, the waste synthetic oil is 46% from hydraulic equipment after impurity removal. # Waste synthetic oil, specific parameters are: kinematic viscosity (40℃) 46.4mm 2 / s, density (15℃) 0.849kg / L, acid value 0.08mgKOH / g, pour point -45℃, flash point 238℃.

[0085] Specifically, additive A is a viscosity reducer, comprising a mixture of methyl silicone oil and dibutyl phthalate in a mass ratio of 7:3. The methyl silicone oil has a dynamic viscosity of 5 mPa·s. Additive B is an antioxidant, N-phenyl-α-naphthylamine. Additive C is a rust inhibitor, barium dinonylnaphthalenesulfonate.

[0086] Main technical indicators of the product: dynamic viscosity (20℃) 16.0mPa.s, density (20℃) 0.852g / cm 3 , pour point -51℃, and other indicators meet the requirements of TB / T 3208-2008 "Technical Conditions for Antifreeze Fluids for Bulk Granular Cargo Transport".

[0087] Test results: The ultra-low temperature antifreeze isolation oil adheres to the wall well, has no frozen bottom, no sticking, and is easy to separate.

[0088] Example 4

[0089] The preparation method and test method described in Example 1 were followed, except that the ultra-low temperature antifreeze isolation oil was made from the following raw materials in parts by weight: 80 parts of waste synthetic oil, 20 parts of additive A, 2.5 parts of additive B, and 3 parts of additive C.

[0090] Specifically, the waste synthetic oil is 68 from the gear box after impurity removal treatment. # Waste synthetic oil, specific parameters are: kinematic viscosity (40℃) 65.1mm 2 / s, density (15℃) 0.868kg / L, acid value 0.08mgKOH / g, pour point -42℃, flash point 253℃.

[0091] Specifically, the additive A is a viscosity reducer, comprising a mixture of methyl silicone oil and dibutyl phthalate in a mass ratio of 6:4. The methyl silicone oil has a dynamic viscosity of 5 mPa·s. The additive B is an antioxidant, N-phenyl-α-naphthylamine. The additive C is a rust inhibitor, aluminum stearate.

[0092] Main technical indicators of the product: dynamic viscosity (20℃) 16.8mPa.s, density (20℃) 0.855g / cm 3 , pour point -51℃, and other indicators meet the requirements of TB / T 3208-2008 "Technical Conditions for Antifreeze Fluids for Bulk Granular Cargo Transport".

[0093] Test results: The oil-based antifreeze adheres well to the wall, has no frozen bottom, no sticking, and is easy to separate.

[0094] Comparative Example 1

[0095] The method was carried out according to the composition ratio and preparation method described in Example 1, except that the application amount of the ultra-low temperature antifreeze isolation oil was 0.010 kg / m 2 .

[0096] Test results: The ultra-low temperature antifreeze isolation oil adhered well to the wall, and the coal in the simulated carriage began to stick after 32 hours. After stopping monitoring, there was coal residue in the simulated carriage, with a residual amount of about 1.80 kg, which is equivalent to about 78.54 kg of coal residue in the 80B carriage.

[0097] Comparative Example 2

[0098] Commercially available calcium chloride aqueous solution (calcium chloride content 38 wt%).

[0099] Main technical indicators of the product: dynamic viscosity (20℃) 6.0mPa.s, density (20℃) 1.25g / cm 3 , freezing point -39℃, and other indicators meet the requirements of TB / T 3208-2008 "Technical Conditions for Antifreeze for Bulk Granular Cargo Transport".

[0100] The calcium chloride aqueous solution was applied in the same manner as described in Example 1, except that the amount of calcium chloride aqueous solution applied was 0.03 kg / m 2 .

[0101] Test results: There was a slight dripping phenomenon of calcium chloride aqueous solution, and the coal in the simulated carriage began to stick after 28 hours. After stopping monitoring, there was coal residue in the simulated carriage, with a residual amount of about 3.05kg, which is equivalent to about 130.86kg of coal residue in the 80B carriage.

[0102] Comparative Example 3

[0103] The test was carried out according to the composition ratio and test method described in Example 1, except that the waste synthetic oil was 32% from hydraulic equipment without impurity removal treatment. # Waste synthetic oil, specific parameters are: kinematic viscosity (40℃) 35.6mm 2 / s, density (15℃) 0.982kg / L, acid value 0.24mgKOH / g, pour point -39℃, flash point 224℃.

[0104] Main technical indicators of the product: dynamic viscosity (20℃) 16.7mPa.s, density (20℃) 0.951g / cm 3 , pour point -42℃, and other indicators meet the requirements of TB / T 3208-2008 "Technical Conditions for Antifreeze Fluids for Bulk Granular Cargo Transport".

[0105] Test results: The ultra-low temperature antifreeze isolation oil adhered to the wall well. After stopping monitoring, there was a trace amount of coal remaining in the simulated carriage, with a residual amount of 0.65kg, which is equivalent to about 28.35kg of coal residue in an 80B carriage.

[0106] In Comparative Example 3, impurities, moisture, organic matter, etc. in the waste synthetic oil were not removed, the uniformity could not be guaranteed, and adhesion occurred.

[0107] Comparative Example 4

[0108] The test method described in Example 1 was followed, except that the ultra-low temperature antifreeze isolation oil was made from the following raw materials in parts by weight: 92 parts of waste synthetic oil, 3.5 parts of additive B, and 2.5 parts of additive C.

[0109] Specifically, the waste synthetic oil is 32 # Waste synthetic oil, specific parameters are: kinematic viscosity (40℃) 30.2mm 2 / s, density (15℃) 0.856kg / L, acid value 0.08mgKOH / g, pour point -48℃, flash point 226℃.

[0110] Specifically, the auxiliary agent B is an antioxidant diphenylamine; and the auxiliary agent C is a rust preventive barium dinonylnaphthalenesulfonate.

[0111] The product was prepared according to the method described in Example 1, except that the stirring speed of the additive B was adjusted to 300 r / min and the mixture was stirred for 20 min; the stirring speed of the additive C was adjusted to 350 r / min and the mixture was stirred for 25 min.

[0112] Main technical indicators of the product: dynamic viscosity (20℃) 24.8mPa.s, density (20℃) 0.855g / cm 3 , pour point -51℃, and other indicators meet the requirements of TB / T 3208-2008 "Technical Conditions for Antifreeze Fluids for Bulk Granular Cargo Transport".

[0113] The product was tested according to the test method described in Example 1. The difference was that the ultra-low temperature antifreeze isolation oil had low fluidity and was unevenly applied. The average application amount was 0.035 kg / m 2 .

[0114] Test results: The oil-based antifreeze adheres well to the wall, has no frozen bottom, no sticking, and is easy to separate.

[0115] In Comparative Example 4, no viscosity reducing agent was added, the antifreeze isolation oil had poor fluidity and was easily unevenly applied, and the thinnest oil film could not be guaranteed.

[0116] Although the present invention has been described in detail through the above preferred embodiments, it should be understood that the above description is not intended to limit the present invention. Those skilled in the art will appreciate that, based on the teachings of this specification, modifications or adjustments may be made to the present invention. Such modifications or adjustments should also be within the scope defined by the claims of the present invention.

Claims

1. An ultra-low temperature antifreeze isolation oil, characterized by: The ultra-low temperature antifreeze isolation oil is a product prepared from a composition comprising the following components in parts by weight: 80 to 100 parts of waste synthetic oil and 5 to 20 parts of a viscosity reducer.

2. The ultra-low temperature antifreeze isolation oil according to claim 1, characterized in that: The waste synthetic oil is the waste synthetic oil that has been treated after being used in gearboxes, hydraulic equipment, steam turbines, compressors, and engine systems. Preferably, the waste synthetic oil has an ISO viscosity grade of 32. # , 46 # , 68 # One or more of .

3. The ultra-low temperature antifreeze isolation oil according to claim 1 or 2, characterized in that: The viscosity reducer is a mixture of methyl silicone oil and dioctyl phthalate or methyl silicone oil and dibutyl phthalate; preferably, the dynamic viscosity of the methyl silicone oil is one of 5mPa·s and 10mPa·s, and the mass ratio of methyl silicone oil to dioctyl phthalate or methyl silicone oil to dibutyl phthalate is 6:4 to 9:1 according to the viscosity of the methyl silicone oil.

4. The ultra-low temperature antifreeze isolation oil according to any one of claims 1 to 3, characterized in that: The antifreeze isolation oil further comprises 1 to 5 parts of an antioxidant, and the antioxidant comprises one of diphenylamine and N-phenyl-α-naphthylamine.

5. The ultra-low temperature antifreeze isolation oil according to any one of claims 1 to 4, characterized in that: The antifreeze isolation oil further comprises 1 to 5 parts of a rust inhibitor, wherein the rust inhibitor comprises one of barium petroleum sulfonate, barium dinonylnaphthalene sulfonate and aluminum stearate.

6. The method for preparing the antifreeze isolation oil according to any one of claims 1 to 5, characterized in that: The steps include: S1: removing impurities from waste synthetic oil; S2: heating the waste synthetic oil treated in step S1 to reduce its viscosity; S3: adding viscosity reducing agents to the waste synthetic oil after viscosity reduction in step S2 in sequence, mixing them evenly, and allowing them to stand to room temperature to prepare ultra-low temperature antifreeze isolation oil.

7. The method for preparing the antifreeze isolation oil according to claim 6, characterized in that: In step S1, the impurity removal treatment includes but is not limited to one or more operations of centrifugation, adsorption and fine filtration; preferably, the impurity removal treatment includes centrifugation, adsorption and fine filtration performed in sequence.

8. The method for preparing the antifreeze isolation oil according to claim 6 or 7, characterized in that: In step S2, the heating and viscosity reduction comprises: heating the waste synthetic oil to 55-65° C.; and / or, In step S3, an antioxidant and a rust inhibitor are also added; In step S3, the uniform mixing includes: adding a viscosity reducer to the waste synthetic oil and stirring it once, adding an antioxidant and stirring it twice, and adding a rust inhibitor and stirring it three times. Preferably, the rotation speed and time of the first stirring, second stirring and third stirring are respectively: 200-300 r / min, 40-60 min; 200-250 r / min, 10-15 min; 200-250 r / min, 15-20 min. Preferably, the mixture comprising waste synthetic oil, viscosity reducing agent and antioxidant is heated to 75-80° C. before adding the rust inhibitor.

9. Use of the ultra-low temperature antifreeze isolation oil according to any one of claims 1 to 5 or the ultra-low temperature antifreeze isolation oil prepared by the preparation method according to any one of claims 6 to 8 in antifreeze treatment of coal transportation in winter.

10. The use of the ultra-low temperature antifreeze isolation oil according to claim 9, characterized in that: Before loading coal into the coal train carriage, apply 0.015-0.03kg / m 2 Ultra-low temperature antifreeze isolation oil.

Citation Information

Patent Citations

  • Ultralow temperature nano antifreezing isolating emulsion, and preparation method thereof

    CN106398528A