CN111876199B - Method for recycling waste mineral oil - Google Patents
Method for recycling waste mineral oil Download PDFInfo
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- CN111876199B CN111876199B CN202010817335.8A CN202010817335A CN111876199B CN 111876199 B CN111876199 B CN 111876199B CN 202010817335 A CN202010817335 A CN 202010817335A CN 111876199 B CN111876199 B CN 111876199B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
- C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
- C10G53/04—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one extraction step
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1003—Waste materials
- C10G2300/1007—Used oils
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/70—Catalyst aspects
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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- Separation Of Suspended Particles By Flocculating Agents (AREA)
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Abstract
The invention belongs to the technical field of waste mineral oil recovery, and particularly relates to a method for recycling waste mineral oil. The method for recycling the waste mineral oil provided by the invention comprises the following steps: settling and filtering, reduced pressure distillation, catalysis, nanofiltration and the like. The method for recycling the waste mineral oil is simple and easy to operate, the recovery rate of the waste mineral oil can reach more than 80%, and the obtained regenerated base oil has few impurities, high oil product quality, strong oxidation resistance and difficult aging.
Description
Technical Field
The invention belongs to the technical field of waste mineral oil recovery, and particularly relates to a method for recycling waste mineral oil.
Background
The waste mineral oil is mineral oil which is extracted and refined from petroleum, coal and oil shale, changes the original physical and chemical properties due to the action of external factors in the processes of mining, processing and using and cannot be used continuously. The waste mineral oil produced in the market is mainly produced after a product blended by base oil and additives is used for a long time. The content of the additive is about 10 percent generally, the main functions of the additive are to improve the performances of the product in the aspects of antifriction, lubrication, sealing, corrosion prevention, cooling, cleaning, rust prevention and the like, and the main types are as follows: antioxidants, rust inhibitors, antifoaming agents, viscosity index improvers, pour point depressants, dispersants, and the like.
Waste mineral oil contains a variety of toxic substances. Experiments show that toxic substances in the waste mineral oil permeate into blood through the epidermis of human and animals and are accumulated in the body, so that various cells can lose normal functions, and the waste mineral oil is a well-known carcinogenic and mutagenic compound. Waste oil is poured randomly and transferred illegally to sell, so that the human health is influenced, secondary black pollution is brought to living environment, water and soil are seriously polluted, and the growth of animals and plants and the living environment of human are harmed. If the waste mineral oil is poured into the soil, the plant can die, and the microorganism in the polluted soil is killed. If waste mineral oil enters the drinking water source, 1 ton of waste mineral oil can contaminate 100 ten thousand tons of drinking water. At present, about 1000 ten thousand tons of waste mineral oil are produced in China every year. The waste mineral oil contains various toxic substances, and if the waste mineral oil is not properly burnt, a large amount of toxic smoke dust can be released, so that the atmospheric environment pollution is caused; when the fertilizer is poured into soil, plants can die, contaminated soil microorganisms are killed, and soil poisoning is caused; when the waste mineral oil enters a drinking water source, 1 liter of the waste mineral oil causes 100 million liters of water pollution.
The waste mineral oil contains sulfur, so the waste mineral oil needs to be subjected to acid cleaning treatment in recycling, however, acid gas and waste acid residues are generated in the acid cleaning treatment, the acid cleaning process causes great harm to the health of workers, and meanwhile, the waste acid residues in the acid cleaning process cannot be used and have great damage to the environment. Traditional waste mineral oil recovery technology needs to invest certain fund and manpower to carry out pickling treatment on sulfur-containing waste mineral oil, and some desulfurization treatment is carried out by building a desulfurizing tower, however, the product cost is undoubtedly increased by the traditional waste mineral oil recovery technology, and the production efficiency is reduced.
The Chinese patent application CN109054894A discloses a method for vacuum distillation-hydrotreatment of waste mineral oil, which comprises the steps of pretreating the waste mineral oil, distilling the waste mineral oil at normal pressure, then carrying out vacuum distillation, and carrying out hydrofining treatment on the raw material subjected to vacuum distillation to obtain a finished product. Although the waste mineral oil treated by the process has high purity, the service life of the waste mineral oil is prolonged, and the process does not have an acid washing process, the hydrogen process generally needs higher temperature and pressure, has extremely strict requirements on equipment, has larger potential safety hazard, and has lower recovery rate of the waste mineral oil.
Chinese patent application CN107699280A discloses a method for upgrading and regenerating waste oil, comprising the following steps: after being pretreated, the waste oil is subjected to catalytic oxidation-extraction process at the temperature of 0-40 ℃ to remove color, metal impurities and sulfides, and thus regenerated oil is obtained; wherein, the oxidant is a gas oxidant or a gas oxidant and a liquid oxidant. The method can effectively remove decoloration, demetalization and desulfurization at a reduced temperature, does not need hydrogen in the process, does not discharge acid and alkali wastes, is environment-friendly and pollution-free, and has low investment cost.
Therefore, it is urgently needed to develop a method for recycling waste mineral oil, which can effectively improve the recovery rate of the waste mineral oil, so that the recycled base oil has higher quality, less carbon content and other impurities and strong oxidation resistance.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a method for recycling waste mineral oil. The method for recycling the waste mineral oil is simple and easy to operate, the recovery rate of the waste mineral oil can reach more than 80%, and the obtained regenerated base oil has few impurities, high oil product quality, strong oxidation resistance and difficult aging.
The technical scheme of the invention is as follows:
a method for recycling waste mineral oil, which comprises the following steps:
s1, settling: conveying the waste mineral oil into a settling tank, filtering solid impurities with large granularity in the waste mineral oil, and adding a flocculating agent for settling separation to form upper-layer waste oil, middle-layer liquid and bottom-layer slag;
s2, reduced pressure distillation: pumping the upper-layer waste oil obtained in the step S1 into a reaction kettle by a pump, adding an extracting agent and a catalyst, uniformly stirring, directly heating the lower part of the kettle for 1-2 hours by a heating furnace, and separating light components from water;
s3, nanofiltration: filtering the waste oil from which the light components and water are removed in the step S2 by using a nanofiltration membrane to obtain regenerated base oil;
further, the flocculating agent in the step S1 is one of polyacrylamide, zinc chloride or aluminum chloride.
Further, the addition amount of the flocculant in the step S1 is 1-5% of the weight of the waste mineral oil in the step S1.
Further, the extractant added in the step S2 is composed of n-butyl ether and tetramethylethylenediamine in a weight ratio (3.0 to 5.5): 1.
Further, the extractant added in step S2 is prepared from n-butyl ether and tetramethylethylenediamine in a weight ratio of 4.4: 1.
Furthermore, the dosage ratio of the extracting agent added in the step S2 to the upper layer waste oil in the step S2 is (30-60) mL:100 mL.
Further, the catalyst added in the step S2 is a beta-type molecular sieve, a 4A molecular sieve and sodium citrate according to a weight ratio of 4-10: 5-11: 1-3.
Furthermore, the catalyst added in the step S2 is composed of a beta type molecular sieve, a 4A molecular sieve and sodium citrate according to a weight ratio of 7:9: 2.
Further, the adding amount of the catalyst in the step S2 is 2-4% of the weight of the upper layer waste oil in the step S2.
Further, in the step S2, the heating temperature is 85-120 ℃, and the pressure is 5-10 Kpa.
Furthermore, the molecular weight cut-off of the nanofiltration membrane used in the step S3 is 200-1000 Da.
The method for recycling the waste mineral oil provided by the invention firstly enters a settling tank for physical settling to remove large-particle solid impurities; then, carrying out flocculation and precipitation under the action of the added flocculating agent, and further removing solid impurities by virtue of the flocculating agent; then, the invention creatively combines the distillation extraction process with the catalysis process, and the extraction is carried out by adding the extractant consisting of n-butyl ether and tetramethylethylenediamine, thereby effectively improving the recovery rate of the waste mineral oil and simultaneously having synergistic effect with the added catalyst. The catalyst adopted in the invention is composed of a beta-type molecular sieve, a 4A molecular sieve and sodium citrate according to a certain proportion, can selectively carry out cracking reaction on long-chain normal paraffin and single-branch paraffin, keeps cycloparaffin, multi-branch paraffin and aromatic hydrocarbon unchanged, reduces the condensation point of distillate oil, can well remove impurities, colloid and the like, ensures that the obtained regenerated base oil is clear and transparent, has high product quality, reduces the acidity of the product, improves the oxidation stability of the product, has long service life and is not easy to age. Meanwhile, the process of filtering and pickling the finished oil is also omitted. And finally, performing nanofiltration treatment on the waste mineral oil, wherein the nanofiltration membrane can separate substances with charges by utilizing a charge effect, so that metal ion additive components in the waste mineral oil can be removed.
Compared with the prior art, the method for recycling the waste mineral oil has the following advantages:
(1) the method for recycling the waste mineral oil has the advantages of simple process and mild reaction conditions, avoids the acid washing process by simultaneously combining distillation extraction and catalysis, does not produce secondary pollution, ensures that the obtained regenerated base oil has high quality and complete reaction, and does not contain other impurities, and the recovery rate of the product reaches more than 80 percent.
(2) According to the method for recycling the waste mineral oil, the catalyst which is composed of the beta-type molecular sieve, the 4A molecular sieve and the sodium citrate according to a certain proportion and added in the method has a good catalytic effect, impurities in an oil product can be effectively reduced, and the acid value of the regenerated base oil is reduced, so that the oxidation stability of the regenerated base oil is improved, and the service life of the regenerated base oil is prolonged.
Detailed Description
The present invention is further illustrated by the following description of specific embodiments, which are not intended to limit the invention, and various modifications and improvements can be made by those skilled in the art based on the basic idea of the invention, but the invention is within the protection scope of the invention.
Beta type molecular sieves, available from Shanghai coconut Biotechnology Ltd; the 4A molecular sieve was purchased from Shanghai Jiachen chemical Co., Ltd.
The other reagents used in the invention are common reagents and can be purchased from conventional reagent production and sale companies.
EXAMPLE 1A method for the heavy recovery and utilization of waste mineral oil
The method for recycling the waste mineral oil comprises the following steps:
s1, settling: conveying the waste mineral oil into a settling tank, filtering solid impurities with large granularity in the waste mineral oil, and adding a flocculating agent for settling separation to form upper-layer waste oil, middle-layer liquid and bottom-layer slag; the flocculating agent is polyacrylamide; the addition amount of the flocculant is 1 percent of the weight of the waste mineral oil;
s2, reduced pressure distillation: pumping the upper waste oil obtained in the step S1 into a reaction kettle by a pump, adding an extracting agent and a catalyst, uniformly stirring, directly heating the lower part of the kettle for 1 hour by a heating furnace at the heating temperature of 85 ℃ and the pressure of 5Kpa, and separating light components and water; the dosage ratio of the extracting agent to the upper layer waste oil is 30mL to 100 mL; the addition amount of the catalyst is 2% of the weight of the upper layer of waste oil;
s3, nanofiltration: and (5) filtering the waste oil from which the light components and the water are removed in the step (S2) by using a nanofiltration membrane to obtain the regenerated base oil.
The extractant added in the step S2 is prepared from n-butyl ether and tetramethylethylenediamine according to the weight ratio of 3.0: 1.
The catalyst added in the step S2 is composed of a beta type molecular sieve, a 4A molecular sieve and sodium citrate according to the weight ratio of 4:11: 3.
Example 2A method for the heavy recovery and utilization of waste mineral oil
The method for recycling the waste mineral oil comprises the following steps:
s1, settling: conveying the waste mineral oil into a settling tank, filtering solid impurities with large granularity in the waste mineral oil, and adding a flocculating agent for settling separation to form upper-layer waste oil, middle-layer liquid and bottom-layer slag; the flocculating agent is zinc chloride; the addition amount of the flocculant is 3 percent of the weight of the waste mineral oil;
s2, reduced pressure distillation: pumping the upper waste oil obtained in the step S1 into a reaction kettle by a pump, adding an extracting agent and a catalyst, uniformly stirring, directly heating the lower part of the kettle for 1.5 hours by a heating furnace at the heating temperature of 105 ℃ and the pressure of 8Kpa, and separating light components from water; the dosage ratio of the extracting agent to the upper layer waste oil is 45mL to 100 mL; the addition amount of the catalyst is 3% of the weight of the upper layer of waste oil;
s3, nanofiltration: and (5) filtering the waste oil from which the light components and the water are removed in the step (S2) by using a nanofiltration membrane to obtain the regenerated base oil.
The extractant added in the step S2 is prepared from n-butyl ether and tetramethylethylenediamine according to the weight ratio of 4.4: 1.
The catalyst added in the step S2 is composed of a beta type molecular sieve, a 4A molecular sieve and sodium citrate according to the weight ratio of 7:9: 2.
EXAMPLE 3A method for recycling waste mineral oil
The method for recycling the waste mineral oil comprises the following steps:
s1, settling: conveying the waste mineral oil into a settling tank, filtering solid impurities with large granularity in the waste mineral oil, and adding a flocculating agent for settling separation to form upper-layer waste oil, middle-layer liquid and bottom-layer slag; the flocculating agent is aluminum chloride; the addition amount of the flocculant is 5 percent of the weight of the waste mineral oil;
s2, reduced pressure distillation: pumping the upper-layer waste oil obtained in the step S1 into a reaction kettle by using a pump, adding an extracting agent and a catalyst, uniformly stirring, directly heating the lower part of the kettle for 2 hours by using a heating furnace, wherein the heating temperature is 85-120 ℃, the pressure is 10Kpa, and separating light components from water; the dosage ratio of the extracting agent to the upper layer waste oil is 60mL to 100 mL; the addition amount of the catalyst is 2-4% of the weight of the upper layer waste oil;
s3, nanofiltration: and (5) filtering the waste oil from which the light components and the water are removed in the step (S2) by using a nanofiltration membrane to obtain the regenerated base oil.
The extractant added in the step S2 is prepared from n-butyl ether and tetramethylethylenediamine according to the weight ratio of 5.5: 1.
The catalyst added in the step S2 is composed of a beta type molecular sieve, a 4A molecular sieve and sodium citrate according to the weight ratio of 10:5: 1.
Comparative example 1 method for recycling waste mineral oil
The method for recycling the waste mineral oil comprises the following steps:
s1, settling: conveying the waste mineral oil into a settling tank, filtering solid impurities with large granularity in the waste mineral oil, and adding a flocculating agent for settling separation to form upper-layer waste oil, middle-layer liquid and bottom-layer slag; the flocculating agent is zinc chloride; the addition amount of the flocculant is 3 percent of the weight of the waste mineral oil;
s2, reduced pressure distillation: pumping the upper waste oil obtained in the step S1 into a reaction kettle by a pump, adding an extracting agent and a catalyst, uniformly stirring, directly heating the lower part of the kettle for 1.5 hours by a heating furnace at the heating temperature of 105 ℃ and the pressure of 8Kpa, and separating light components from water; the dosage ratio of the extracting agent to the upper layer waste oil is 45mL to 100 mL; the addition amount of the catalyst is 3% of the weight of the upper layer of waste oil;
s3, nanofiltration: and (5) filtering the waste oil from which the light components and the water are removed in the step (S2) by using a nanofiltration membrane to obtain the regenerated base oil.
The extractant added in the step S2 is n-butyl ether.
The catalyst added in the step S2 is composed of a beta type molecular sieve, a 4A molecular sieve and sodium citrate according to the weight ratio of 7:9: 2.
The difference from example 2 is that tetramethylethylenediamine was not added to the extractant.
Comparative example 2 method for recycling waste mineral oil
The method for recycling the waste mineral oil comprises the following steps:
s1, settling: conveying the waste mineral oil into a settling tank, filtering solid impurities with large granularity in the waste mineral oil, and adding a flocculating agent for settling separation to form upper-layer waste oil, middle-layer liquid and bottom-layer slag; the flocculating agent is zinc chloride; the addition amount of the flocculant is 3 percent of the weight of the waste mineral oil;
s2, reduced pressure distillation: pumping the upper waste oil obtained in the step S1 into a reaction kettle by a pump, adding an extracting agent and a catalyst, uniformly stirring, directly heating the lower part of the kettle for 1.5 hours by a heating furnace at the heating temperature of 105 ℃ and the pressure of 8Kpa, and separating light components from water; the dosage ratio of the extracting agent to the upper layer waste oil is 45mL to 100 mL; the addition amount of the catalyst is 3% of the weight of the upper layer of waste oil;
s3, nanofiltration: and (5) filtering the waste oil from which the light components and the water are removed in the step (S2) by using a nanofiltration membrane to obtain the regenerated base oil.
The extractant added in the step S2 is prepared from n-butyl ether and tetramethylethylenediamine according to the weight ratio of 1: 1.
The catalyst added in the step S2 is composed of a beta type molecular sieve, a 4A molecular sieve and sodium citrate according to the weight ratio of 7:9: 2.
The difference from example 2 is that the extractant is prepared from n-butyl ether and tetramethylethylenediamine according to the weight ratio of 1: 1.
Comparative example 3 method for recycling waste mineral oil
The method for recycling the waste mineral oil comprises the following steps:
s1, settling: conveying the waste mineral oil into a settling tank, filtering solid impurities with large granularity in the waste mineral oil, and adding a flocculating agent for settling separation to form upper-layer waste oil, middle-layer liquid and bottom-layer slag; the flocculating agent is zinc chloride; the addition amount of the flocculant is 3 percent of the weight of the waste mineral oil;
s2, reduced pressure distillation: pumping the upper waste oil obtained in the step S1 into a reaction kettle by a pump, adding an extracting agent and a catalyst, uniformly stirring, directly heating the lower part of the kettle for 1.5 hours by a heating furnace at the heating temperature of 105 ℃ and the pressure of 8Kpa, and separating light components from water; the dosage ratio of the extracting agent to the upper layer waste oil is 45mL to 100 mL; the addition amount of the catalyst is 3% of the weight of the upper layer of waste oil;
s3, nanofiltration: and (5) filtering the waste oil from which the light components and the water are removed in the step (S2) by using a nanofiltration membrane to obtain the regenerated base oil.
The extractant added in the step S2 is prepared from n-butyl ether and tetramethylethylenediamine according to the weight ratio of 4.4: 1.
The catalyst added in the step S2 is composed of a beta type molecular sieve and a 4A molecular sieve according to the weight ratio of 7: 9.
The difference from example 2 is that sodium citrate is not added to the catalyst.
Comparative example 4 method for recycling waste mineral oil
The method for recycling the waste mineral oil comprises the following steps:
s1, settling: conveying the waste mineral oil into a settling tank, filtering solid impurities with large granularity in the waste mineral oil, and adding a flocculating agent for settling separation to form upper-layer waste oil, middle-layer liquid and bottom-layer slag; the flocculating agent is zinc chloride; the addition amount of the flocculant is 3 percent of the weight of the waste mineral oil;
s2, reduced pressure distillation: pumping the upper waste oil obtained in the step S1 into a reaction kettle by a pump, adding an extracting agent and a catalyst, uniformly stirring, directly heating the lower part of the kettle for 1.5 hours by a heating furnace at the heating temperature of 105 ℃ and the pressure of 8Kpa, and separating light components from water; the dosage ratio of the extracting agent to the upper layer waste oil is 45mL to 100 mL; the addition amount of the catalyst is 3% of the weight of the upper layer of waste oil;
s3, nanofiltration: and (5) filtering the waste oil from which the light components and the water are removed in the step (S2) by using a nanofiltration membrane to obtain the regenerated base oil.
The extractant added in the step S2 is prepared from n-butyl ether and tetramethylethylenediamine according to the weight ratio of 4.4: 1.
The catalyst added in the step S2 is composed of a beta type molecular sieve, a 4A molecular sieve and sodium citrate according to the weight ratio of 1:1: 1.
The difference from the example 2 is that the catalyst is composed of beta type molecular sieve, 4A molecular sieve and sodium citrate according to the weight ratio of 1:1: 1.
Comparative example 5 method for recycling waste mineral oil
The method for recycling the waste mineral oil comprises the following steps:
s1, settling: conveying the waste mineral oil into a settling tank, filtering solid impurities with large granularity in the waste mineral oil, and adding a flocculating agent for settling separation to form upper-layer waste oil, middle-layer liquid and bottom-layer slag; the flocculating agent is zinc chloride; the addition amount of the flocculant is 3 percent of the weight of the waste mineral oil;
s2, reduced pressure distillation: pumping the upper waste oil obtained in the step S1 into a reaction kettle by a pump, adding an extracting agent and a catalyst, uniformly stirring, directly heating the lower part of the kettle for 1.5 hours by a heating furnace at the heating temperature of 105 ℃ and the pressure of 8Kpa, and separating light components from water; the dosage ratio of the extracting agent to the upper layer waste oil is 45mL to 100 mL; the addition amount of the catalyst is 3% of the weight of the upper layer of waste oil;
s3, nanofiltration: and (5) filtering the waste oil from which the light components and the water are removed in the step (S2) by using a nanofiltration membrane to obtain the regenerated base oil.
The extractant added in the step S2 is prepared from n-butyl ether and tetramethylethylenediamine according to the weight ratio of 4.4: 1.
The catalyst added in the step S2 is a natural zeolite molecular sieve
The difference from example 2 is that the catalyst is a natural zeolite molecular sieve.
Test example I, recovery test of waste mineral oil
1. Test materials: the regenerated base oil prepared by the method for recycling the waste mineral oil in the embodiments 1-3 and the comparative examples 1-5 is adopted.
2. The test method comprises the following steps: 300mL of waste mineral oil was taken and treated by the methods of examples 1 to 3 and comparative examples 1 to 5, respectively, to obtain a recovered regenerated base oil, and further to obtain a recovery rate of the waste mineral oil.
3. Test results
The test results are shown in table 1.
TABLE 1 recovery of waste mineral oil
| Group of | Volume of waste mineral oil (mL) | Volume of regenerated base oil (mL) | Recovery rate |
| Example 1 | 300 | 240 | 80.00％ |
| Example 2 | 300 | 248 | 82.67％ |
| Example 3 | 300 | 242 | 80.67％ |
| Comparative example 1 | 300 | 112 | 37.33％ |
| Comparative example 2 | 300 | 127 | 42.33％ |
| Comparative example 3 | 300 | 210 | 70.00％ |
| Comparative example 4 | 300 | 215 | 71.67％ |
| Comparative example 5 | 300 | 198 | 66.00％ |
As can be seen from Table 1: the recovery rates of the waste mineral oil obtained by the method for recycling the waste mineral oil in the embodiments 1-3 of the invention are all over 80%, wherein the embodiment 2 has the best effect, and the recovery rate is up to 82.67%, which is the best embodiment of the invention. In the comparative examples 1-2, when the components of the extracting agent are changed, the volume of the obtained regenerated base oil is obviously reduced, and the recovery rate is greatly reduced; the extraction agent which is added in the invention and consists of n-butyl ether and tetramethylethylenediamine can effectively improve the recovery rate of the waste mineral oil.
Test example II Performance test of reclaimed base oil
1. Test materials: the regenerated base oil prepared by the method for recycling the waste mineral oil in the embodiments 1-3 and the comparative examples 1-5 is adopted.
2. The test method comprises the following steps: the test of pour point, chroma, density, kinematic viscosity, flash point (closed), viscosity index, oxidation stability, acid number, sulfur content and carbon residue were performed on the waste mineral oil before treatment and the regenerated base oil obtained in examples 1 to 3 and comparative examples 1 to 5, respectively. The detection method is shown in Table 2.
3. Test results
The test results are shown in table 2.
TABLE 2 recycled base oil Performance test data
As can be seen from Table 2: the regenerated base oil obtained by the method for recycling the waste mineral oil in the embodiments 1-3 of the invention has high quality, low pour point and high viscosity index, and the obtained oil has good low-temperature fluidity; the flash point is higher and the volatilization is difficult; the acid number, sulfur content and carbon residue were low, and among them, example 2 is the best example of the present invention, which is the best effect. In comparative examples 3 to 5, when the catalytic components and the proportion are changed, the oxidation stability of the obtained regenerated base oil is obviously reduced compared with that in examples 1 to 3, the acid value is increased, and the sulfur content and the carbon residue are also increased, which shows that the catalyst composed of the beta-type molecular sieve, the 4A molecular sieve and the sodium citrate added in the invention has obvious synergistic effect, good catalytic effect, high quality of the obtained base oil, less impurities, capability of effectively reducing the acid value of the base oil, good oxidation resistance and difficult aging.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (8)
1. A method for recycling waste mineral oil is characterized by comprising the following steps:
s1, settling: conveying the waste mineral oil into a settling tank, filtering solid impurities with large granularity in the waste mineral oil, and adding a flocculating agent for settling separation to form upper-layer waste oil, middle-layer liquid and bottom-layer slag;
s2, reduced pressure distillation: pumping the upper-layer waste oil obtained in the step S1 into a reaction kettle by a pump, adding an extracting agent and a catalyst, uniformly stirring, directly heating the lower part of the kettle for 1-2 hours by a heating furnace, and separating light components from water;
s3, nanofiltration: filtering the waste oil from which the light components and water are removed in the step S2 by using a nanofiltration membrane to obtain regenerated base oil;
the extractant added in the step S2 is prepared from n-butyl ether and tetramethylethylenediamine according to the weight ratio of (3.0-5.5): 1, preparing a composition;
the catalyst added in the step S2 is composed of a beta-type molecular sieve, a 4A molecular sieve and sodium citrate according to a weight ratio of 4-10: 5-11: 1-3.
2. The method for recycling waste mineral oil as claimed in claim 1, wherein the flocculating agent in step S1 is one of polyacrylamide, zinc chloride or aluminum chloride.
3. The method for recycling waste mineral oil as claimed in claim 1, wherein the amount of the flocculant added in step S1 is 1-5% by weight of the waste mineral oil in step S1.
4. The method for recycling waste mineral oil according to claim 1, wherein the extractant added in step S2 is a mixture of n-butyl ether and tetramethylethylenediamine in a weight ratio of 4.4: 1.
5. The method for recycling waste mineral oil as claimed in claim 1, wherein the amount ratio of the extractant added in step S2 to the waste oil on the upper layer in step S2 is (30-60) mL:100 mL.
6. The method for recycling waste mineral oil as claimed in claim 1, wherein the catalyst added in step S2 is beta type molecular sieve, 4A molecular sieve and sodium citrate in a weight ratio of 7:9: 2.
7. The method for recycling waste mineral oil as claimed in claim 1, wherein the amount of the catalyst added in step S2 is 2-4% of the weight of the waste oil on the upper layer in step S2.
8. The method for recycling waste mineral oil as set forth in claim 1, wherein the heating temperature in step S2 is 85 to 120 ℃ and the pressure is 5 to 10 Kpa.
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