Diesel fuel additive and use thereof

Abstract

The present application relates to a kind of diesel oil additive and its application, belong to biomass diesel oil additive technical field, including the following steps: acid compound is combined with low temperature flow modifier by esterification reaction, and compound is obtained;1,4-cyclohexadiene-1,2-dicarboxylic anhydride is combined with silanization enhancement material, and modified material is obtained;Compound, modified material and methyl methacrylate tetradecyl ester are combined by graft copolymerization, and finally diesel oil additive is obtained.In the technical scheme of the present application, by ricinoleic acid and ferulic acid mixed to form acid compound, 1-adamantanol and three-arm glycerol lactate mixed to form low temperature flow modifier, the low temperature fluidity and oxidation stability of diesel oil additive can be improved better, by 1,4-cyclohexadiene-1,2-dicarboxylic anhydride is combined with silanization enhancement material, further improve the anti-wear performance and oxidation stability of diesel oil additive, overall improve the comprehensive performance of diesel oil additive.

Description

Technical Field

[0001] This invention belongs to the field of biomass diesel additive technology, specifically, it relates to a diesel additive and its application. Background Technology

[0002] Biomass diesel, whose main component is fatty acid methyl ester, is produced by transesterification of oils from oil crops such as soybeans and rapeseed, fruits of oil-bearing forest trees such as oil palm and Chinese pistache, oil-bearing aquatic plants such as engineered microalgae, animal fats, and waste cooking oil with alcohols (such as methanol and ethanol). It is a clean biofuel. Biomass diesel is an excellent alternative to petroleum diesel, not only alleviating human dependence on petroleum but also serving as a renewable energy source. Furthermore, biomass diesel has a high oxygen content and high cetane number, which is highly beneficial for the proper combustion of compression-ignition engines, effectively reducing the emission of harmful substances in exhaust gases. Although biomass diesel possesses many excellent properties, its inherent defects, such as poor low-temperature fluidity and insufficient oxidation stability, severely limit its widespread application. Therefore, specific diesel additives are usually added to biomass diesel to improve its performance indicators and overall properties, making it more suitable for various application scenarios.

[0003] In existing technologies, diesel additives are used to lower the pour point of biodiesel and improve its low-temperature flow properties. However, for some biodiesel with high pour points, the improvement effect of additives is limited and cannot meet the needs of practical applications. Furthermore, the effect of adding antioxidants (such as hindered phenolic antioxidants and p-phenylenediamine derivatives) to improve the oxidation stability of biodiesel is also limited and still cannot meet the high-efficiency requirements for oxidation stability of biodiesel. In addition, although diesel additives can improve the low-temperature flow, oxidation stability, or anti-wear properties of biodiesel to a certain extent, their functions are relatively singular, only improving one property. In some cases, while improving a certain property of biodiesel, they may even reduce other properties and indicators, lacking the synergistic effect between the components. Therefore, it is necessary to prepare a diesel additive with better low-temperature flow, oxidation stability, and anti-wear properties. Summary of the Invention

[0004] The purpose of this invention is to provide a diesel additive and its application. A complex is obtained by combining an acidic compound with a low-temperature flow improver through an esterification reaction; a modified material is obtained by combining 1,4-cyclohexadiene-1,2-dicarboxylic anhydride with a silanized reinforcing material; and a diesel additive is finally obtained by graft copolymerization of the complex from step S1, the modified material from step S2, and tetradecyl methacrylate. The prepared diesel additive not only possesses good low-temperature flow properties, oxidation stability, and anti-wear properties, but also exhibits excellent overall performance. Furthermore, it has a good reinforcing effect on biomass diesel, which can further extend the service life of biomass diesel.

[0005] The technical problem this invention aims to solve is as follows: In the prior art, diesel additives are used to lower the pour point of biodiesel and improve its low-temperature flow properties. However, for some biodiesel with high pour points, the improvement effect of additives is limited and cannot meet the needs of practical applications. Furthermore, the effect of adding antioxidants (such as hindered phenolic antioxidants, p-phenylenediamine derivatives, etc.) to improve the oxidation stability of biodiesel is also limited and still cannot meet the high-efficiency requirements for the oxidation stability of biodiesel. In addition, although diesel additives can improve the low-temperature flow, oxidation stability, or anti-wear properties of biodiesel to a certain extent, their functions are relatively singular, only improving one property. In some cases, while improving a certain property of biodiesel, they may even reduce other properties and indicators, lacking the synergistic effect between the components. Therefore, it is necessary to prepare a diesel additive with better low-temperature flow, oxidation stability, and anti-wear properties.

[0006] The objective of this invention can be achieved through the following technical solutions:

[0007] A method for preparing a diesel additive includes the following steps:

[0008] S1: An acid compound is combined with a low-temperature flow modifier through an esterification reaction to obtain a complex;

[0009] S2: Combining 1,4-cyclohexadiene-1,2-dicarboxylic anhydride with silanized reinforcing materials yields modified materials;

[0010] S3: The complex in step S1, the modified material in step S2, and tetradecyl methacrylate are combined by graft copolymerization to finally obtain a diesel additive.

[0011] Furthermore, step S1 specifically includes:

[0012] An acid compound and a low-temperature flow modifier were added to tetrahydrofuran, followed by a catalyst. The mixture was then stirred and reacted under a nitrogen atmosphere at 95-105°C for 11-13 hours. After the reaction was completed, the tetrahydrofuran was removed by rotary evaporation, washed with ethanol, and finally dried under vacuum at 55-65°C to obtain the complex.

[0013] In the above reaction process, the acid compound has a carboxyl group and the low-temperature flow modifier has a hydroxyl group. The carboxyl group in the acid compound can combine with the hydroxyl group in the low-temperature flow modifier through an esterification reaction, thus combining the acid compound and the low-temperature flow modifier together to finally obtain a complex.

[0014] Furthermore, the mass ratio of the acid compound, the low-temperature flow improver, and the tetrahydrofuran is 1.4-1.6:0.9-1.1:50-60.

[0015] Furthermore, the acidic compound is composed of ricinoleic acid and ferulic acid in a mass ratio of 0.9-1.1:0.7-0.8.

[0016] Furthermore, the low-temperature flow improver is composed of 1-adamantanol and triglyceride lactate in a mass ratio of 0.8-0.9:0.4-0.5.

[0017] Furthermore, the catalyst is p-toluenesulfonic acid.

[0018] Furthermore, the preparation method of the three-arm lactic acid glyceride includes the following steps:

[0019] Glycerol and lactic acid are mixed, then dimethylbenzene and p-toluenesulfonic acid are added, and the mixture is reacted at 180-190℃ for 5-7 hours. After the reaction is completed, residual dimethylbenzene and lactic acid are removed by vacuum distillation. Then, the mixture is added to a saturated sodium chloride solution and stirred evenly. Finally, it is extracted with ethyl acetate and the ethyl acetate is removed by vacuum distillation to obtain three-arm lactic acid glyceride.

[0020] Furthermore, the mass ratio of glycerol to lactic acid is 1:6.

[0021] Furthermore, step S2 specifically includes:

[0022] The silanized reinforcing material was added to dimethyl sulfoxide and mixed evenly to obtain component A. 1,4-cyclohexadiene-1,2-dicarboxylic anhydride, 1-ethyl-(3-dimethylaminopropyl)carbodiimide and N-hydroxysuccinimide were added to dimethyl sulfoxide and stirred for 0.5-1.5 h to obtain component B. Component B was added to component A, and the mixture was reacted at 55-65 °C for 22-24 h. After the reaction was completed, the mixture was filtered, centrifuged for 5-10 min, washed with anhydrous ethanol and deionized water, and finally vacuum dried at 55-65 °C to obtain the modified material.

[0023] In the above reaction process, the silanized reinforcing material has an amino group, and the 1,4-cyclohexadiene-1,2-dicarboxylic anhydride has an anhydride group. The amino group in the silanized reinforcing material can react and combine with the anhydride group in the 1,4-cyclohexadiene-1,2-dicarboxylic anhydride, thus combining the 1,4-cyclohexadiene-1,2-dicarboxylic anhydride with the silanized reinforcing material to finally obtain the modified material.

[0024] Furthermore, the mass ratio of the silanized reinforcing material to dimethyl sulfoxide is 4.8-5.2:50-60.

[0025] Further, the mass ratio of 1,4-cyclohexadiene-1,2-dicarboxylic anhydride, 1-ethyl-(3-dimethylaminopropyl)carbodiimide, N-hydroxysuccinimide, and dimethyl sulfoxide is 21-22:11-12:6.5-7.5:90-110.

[0026] Furthermore, the mass ratio of component A to component B is 4:1.

[0027] Furthermore, the preparation method of the silanized reinforced material includes the following steps:

[0028] The silane coupling agent is added to a mixed solution of ethanol and deionized water and ultrasonically treated for 15-25 minutes. Then, the reinforcing material is added and stirred at 75-85℃ for 5-7 hours. After filtration, the material is washed with ethanol and deionized water and finally vacuum dried at 55-65℃ to obtain the silanized reinforcing material.

[0029] During the above reaction process, the surface of the reinforcing material has hydroxyl groups. After the silane coupling agent is hydrolyzed, silanol groups are generated, which can combine with the hydroxyl groups on the reinforcing material to graft the silane coupling agent onto the surface of the reinforcing material, and finally, silanized reinforcing material is obtained.

[0030] Furthermore, the mass ratio of the silane coupling agent, the ethanol and deionized water mixed solution, and the reinforcing material is 0.4-0.6: 90-110: 1.8-2.

[0031] Furthermore, the silane coupling agent is 3-aminopropyltriethoxysilane.

[0032] Furthermore, the method for preparing the reinforcing material includes the following steps:

[0033] Graphene oxide was added to anhydrous ethanol and sonicated for 0.5-1 h to obtain a graphene oxide dispersion. Cerium nitrate hexahydrate and aluminum nitrate nonahydrate were added to anhydrous ethanol and stirred until homogeneous. Then, deionized water was added and stirred for 25-35 min to obtain a precursor solution. The precursor solution was added to the graphene oxide dispersion and stirred in a water bath at 75-85℃ for 7-9 h. After cooling to room temperature, the mixture was filtered, washed with deionized water, vacuum dried at 45-55℃, and finally calcined at 390-410℃ for 1.5-2.5 h to obtain the reinforcing material.

[0034] In the above reaction process, aluminum oxide and cerium oxide are co-loaded onto the surface of graphene oxide using the sol-gel method, thereby combining aluminum oxide, cerium oxide and graphene oxide together to obtain the reinforcing material.

[0035] Furthermore, the mass ratio of graphene oxide to anhydrous ethanol is 0.5-0.7:90-110.

[0036] Furthermore, the mass ratio of cerium nitrate hexahydrate, aluminum nitrate nonahydrate, anhydrous ethanol, and deionized water is 0.05-0.15:0.05-0.15:45-55:20-30.

[0037] Furthermore, the mass ratio of the precursor solution to the graphene oxide dispersion is 1:2.

[0038] Furthermore, step S3 specifically includes:

[0039] The composite from step S1, the modified material from step S2, and tetradecyl methacrylate were mixed, and then toluene and a catalyst were added. The mixture was then polymerized at 95-105°C for 5-7 hours. After the reaction was completed, toluene was removed by rotary evaporation, the mixture was washed with anhydrous ethanol, and then vacuum dried at 55-65°C to obtain the diesel additive.

[0040] In the above reaction process, the complex in step S1, the modified material in step S2, and tetradecyl methacrylate all have carbon-carbon double bonds. They can be combined through graft copolymerization to combine the complex in step S1, the modified material in step S2, and tetradecyl methacrylate, and finally obtain a diesel additive.

[0041] Furthermore, the mass ratio of the composite, the modified material, and tetradecyl methacrylate is 0.5-1.5:0.5-1.5:9.5-10.5.

[0042] Furthermore, the catalyst is benzoyl peroxide.

[0043] The beneficial effects of this invention are:

[0044] (1) In the technical solution of this invention, an acid compound is obtained by combining it with a low-temperature flow improver through an esterification reaction; the acid compound is composed of ricinoleic acid and ferulic acid, which have a synergistic effect and can effectively improve the oxidation stability and low-temperature flow performance of diesel additives. Ferulic acid, as a phenolic antioxidant, can significantly improve the oxidation stability of biomass diesel, prevent it from oxidizing and deteriorating during storage and use, and thus extend its service life. Ricinoleic acid has a high oxygen content, which helps to promote a more complete combustion process of biomass diesel, which can not only improve fuel efficiency, but also reduce the emission of unburned hydrocarbons. Moreover, ricinoleic acid contains a long-chain fatty acid structure, which can effectively provide additional lubrication effect, protect the internal components of the engine from wear, and further improve the anti-wear effect of diesel additives. Ferulic acid is derived from renewable resources and has good biodegradability, reducing long-term environmental impact. The low-temperature flow improver is composed of a mixture of 1-adamantanol and tri-arm lactic acid glyceride. The rigid group in 1-adamantanol has a steric hindrance effect, which can effectively lower the cold filter plugging point of biodiesel, maintain the fluidity of biodiesel at low temperatures, and promote a more complete combustion process. The tri-arm lactic acid glyceride has good thermal stability and is not easily decomposed at high temperatures, which can improve the oxidation stability and low-temperature fluidity of biodiesel, and provide additional lubrication effect, further enhancing the anti-wear performance of diesel additives. Combining acid compounds with low-temperature flow improvers can have a synergistic effect, effectively improving the performance of diesel additives, giving them better low-temperature fluidity, oxidation stability, and anti-wear performance in biodiesel.

[0045] (2) In the technical solution of this invention, the modified material is obtained by combining 1,4-cyclohexadiene-1,2-dicarboxylic anhydride with a silanized reinforcing material; the silanized reinforcing material is prepared by grafting the reinforcing material with a silane coupling agent, and the reinforcing material is prepared by loading alumina and cerium oxide onto graphene oxide; both alumina and cerium oxide have good catalytic activity, which can promote the complete combustion of biomass diesel and reduce the generation of unburned hydrocarbons. Alumina has a certain antioxidant capacity, which can improve the oxidation stability of diesel additives. Cerium oxide has excellent thermal and chemical stability, which can reduce friction and wear inside the engine, further improving the anti-wear effect of biomass diesel. Graphene oxide also has good wear resistance, which can reduce wear and help reduce wear. To reduce carbon deposits and other sediments generated during combustion, loading alumina and cerium oxide onto graphene oxide enhances its dispersibility, and the three also have a certain synergistic effect, which can effectively improve the anti-wear performance and oxidation stability of diesel additives. Grafting with silane coupling agents can further improve the dispersibility of reinforcing materials in biodiesel, improve its compatibility with biodiesel, and have good binding force with 1,4-cyclohexadiene-1,2-dicarboxylic anhydride. 1,4-cyclohexadiene-1,2-dicarboxylic anhydride can promote a more complete combustion process, has a certain antioxidant capacity, can improve the low-temperature fluidity of diesel additives to a certain extent, and can also provide reaction sites for subsequent reactions, further enhancing the overall performance of diesel additives.

[0046] (3) In the technical solution of the present invention, the diesel additive is finally obtained by graft copolymerization of the complex in step S1, the modified material in step S2 and tetradecyl methacrylate. The complex, the modified material and tetradecyl methacrylate are combined by polymerization reaction, which has good binding force. The tetradecyl methacrylate has long-chain alkyl, which helps to reduce the cold filter plugging point of biomass diesel, improve the low temperature fluidity of diesel additive, and help to improve the combustion efficiency of biomass diesel, and provide additional lubrication effect, reduce wear, further enhance the anti-wear effect of diesel additive, and extend its service life. The combination of complex, modified material and tetradecyl methacrylate can better improve the low temperature fluidity, oxidation stability and anti-wear performance of diesel additive, and can further improve the overall performance of biomass diesel.

[0047] (4) In the technical solution of the present invention, a complex is obtained by combining an acid compound with a low-temperature flow modifier, a modified material is obtained by combining 1,4-cyclohexadiene-1,2-dicarboxylic anhydride with a silanized reinforcing material, and a diesel additive is obtained by combining the complex, the modified material and tetradecyl methacrylate. The prepared diesel additive not only has good low-temperature flow properties, oxidation stability and anti-wear properties, but also has good overall performance. It has a good reinforcing effect when applied to biomass diesel, which can further extend the service life of biomass diesel. Detailed Implementation

[0048] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0049] The specific parameters of the raw materials used in this invention are as follows:

[0050] Castor oil acid, CAS No.: 141-22-0, Trade Code: 01376040, provided by Shanghai Titan Technology Co., Ltd.; ferulic acid, CAS No.: 1135-24-6, provided by Shandong Xiya Chemical Co., Ltd.; 1,4-cyclohexadiene-1,2-dicarboxylic anhydride, CAS No.: 4773-89-1, provided by Shanghai Jixiang Biotechnology Co., Ltd.; 1-adamantanol, CAS No.: 768-95-6, Trade Code: A801417, provided by Shanghai Maclean Biochemical Technology Co., Ltd.; graphene oxide, No.: S25040, provided by Shanghai Yuanye Biotechnology Co., Ltd.; tetradecyl methacrylate, CAS No.: 2549-53-3, Trade Code: 015128678, provided by Shanghai Titan Technology Co., Ltd.

[0051] The preparation method of three-arm lactic acid glyceride includes the following steps:

[0052] Glycerol and lactic acid were mixed at a mass ratio of 1:6, and then dimethylbenzene (10% of the mass of glycerol) and p-toluenesulfonic acid (0.5% of the mass of glycerol) were added. The mixture was then reacted at 180-190℃ for 5-7 hours. After the reaction was completed, residual dimethylbenzene and lactic acid were removed by vacuum distillation at 50-60℃. The mixture was then added to a 26.5wt% saturated sodium chloride solution (20 times the mass of glycerol) and stirred until homogeneous. The mixture was then extracted three times with ethyl acetate (each time the mass of ethyl acetate was 50% of the mass of the saturated sodium chloride solution). The ethyl acetate was removed by vacuum distillation at 50-60℃, and finally, three-arm lactic acid glycerides were obtained. Example 1

[0053] The preparation method of diesel additives includes the following steps:

[0054] S1: The acid compound, low-temperature flow modifier, and tetrahydrofuran were added to tetrahydrofuran in a mass ratio of 1.4:0.9:50. Then, p-toluenesulfonic acid (3% of the mass of the acid compound) was added. The mixture was stirred at 95°C under a nitrogen atmosphere for 13 hours. After the reaction was completed, the tetrahydrofuran was removed by rotary evaporation at 40°C. The mixture was washed three times with ethanol (30% of the mass of tetrahydrofuran each time) and finally dried under vacuum at 55°C for 12 hours to obtain the complex. The acid compound was composed of ricinoleic acid and ferulic acid in a mass ratio of 0.9:0.7. The low-temperature flow modifier was composed of 1-adamantanol and triglyceride lactate in a mass ratio of 0.8:0.4.

[0055] S2: Component A is obtained by adding the silanized reinforcing material to dimethyl sulfoxide at a mass ratio of 4.8:50 and mixing thoroughly. Component A is then prepared by adding the silanized reinforcing material to dimethyl sulfoxide at a mass ratio of 21:11:6.5:90. Component A is further prepared by adding the 1,4-cyclohexadiene-1,2-dicarboxylic anhydride, 1-ethyl-(3-dimethylaminopropyl)carbodiimide, N-hydroxysuccinimide, and dimethyl sulfoxide at a mass ratio of 21:11:6.5:90. Imide was added to dimethyl sulfoxide and stirred for 0.5 h to obtain component B. Component B was added to component A at a mass ratio of 4:1. The mixture was then reacted at 55 °C for 24 h. After the reaction was completed, the mixture was filtered, centrifuged at 10,000 rpm for 10 min, and washed three times each with anhydrous ethanol and deionized water (each time the mass of ethanol was equal to the mass of N-hydroxysuccinimide, and each time the mass of deionized water was equal to the mass of N-hydroxysuccinimide). Finally, the mixture was vacuum dried at 55 °C for 12 h to obtain the modified material.

[0056] The preparation method of silanized reinforced materials includes the following steps:

[0057] The mass ratio of 3-aminopropyltriethoxysilane, ethanol, and deionized water to reinforcing material was 0.4:90:1.8. 3-aminopropyltriethoxysilane was added to the ethanol and deionized water mixture (volume ratio of ethanol to deionized water was 49:1), and the mixture was ultrasonically treated for 15 min (ultrasonic power was 100 W, ultrasonic frequency was 40 kHz). Then, the reinforcing material was added, and the mixture was stirred at 400 rpm for 7 h at 75 °C. After filtration, the mixture was washed three times each with ethanol and deionized water (each time the mass of ethanol was 6 times the mass of the reinforcing material, and each time the mass of deionized water was 7 times the mass of the reinforcing material). Finally, the mixture was vacuum dried at 55 °C for 12 h to obtain the silanized reinforcing material.

[0058] The preparation method of the reinforcing material includes the following steps:

[0059] Graphene oxide was added to anhydrous ethanol at a mass ratio of 0.5:90, and the mixture was ultrasonically treated for 0.5 h (ultrasonic power 100 W, ultrasonic frequency 40 kHz) to obtain a graphene oxide dispersion. Cerium nitrate hexahydrate, aluminum nitrate nonahydrate, anhydrous ethanol, and deionized water were added to anhydrous ethanol at a mass ratio of 0.05:0.05:45:20, and stirred until homogeneous. Then, deionized water was added. The mixture was stirred for 25 minutes to obtain a precursor solution. The precursor solution was added to the graphene oxide dispersion at a mass ratio of 1:2. The mixture was then stirred at 100 rpm for 9 hours in a water bath at 75°C. After cooling to room temperature, the mixture was filtered and washed three times with deionized water (each wash being 60% of the total mass of the deionized water). The mixture was then vacuum dried at 45°C for 24 hours and finally calcined at 390°C for 2.5 hours to obtain the reinforced material.

[0060] S3: According to the mass ratio of the composite, the modifying material, and tetradecyl methacrylate of 0.5:0.5:9.5, the composite from step S1, the modifying material from step S2, and tetradecyl methacrylate are mixed, and then toluene (toluene mass is 6 times the mass of tetradecyl methacrylate) and benzoyl peroxide (benzoyl peroxide mass is 3% of the mass of tetradecyl methacrylate) are added. Then, the polymerization reaction is carried out at 95℃ for 7 hours. After the reaction is completed, toluene is removed by rotary evaporation at 50℃, and the mixture is washed 3 times with anhydrous ethanol (each time the mass of anhydrous ethanol is 20% of the mass of toluene). The mixture is then vacuum dried at 55℃ for 12 hours to obtain the diesel additive. Example 2

[0061] The preparation method of diesel additives includes the following steps:

[0062] S1: The acid compound, low-temperature flow modifier, and tetrahydrofuran were added to tetrahydrofuran in a mass ratio of 1.5:1:55. Then, p-toluenesulfonic acid (3% of the mass of the acid compound) was added. The mixture was stirred at 100°C for 12 hours under a nitrogen atmosphere. After the reaction was completed, the tetrahydrofuran was removed by rotary evaporation at 45°C. The mixture was washed three times with ethanol (30% of the mass of tetrahydrofuran each time). Finally, it was vacuum dried at 60°C for 11 hours to obtain the complex. The acid compound was composed of ricinoleic acid and ferulic acid in a mass ratio of 1:0.75. The low-temperature flow modifier was composed of 1-adamantanol and triglyceride lactate in a mass ratio of 0.85:0.45.

[0063] S2: Component A is obtained by adding the silanized reinforcing material to dimethyl sulfoxide at a mass ratio of 5:55 (silanized reinforcing material:dimethyl sulfoxide) and mixing thoroughly. Component A is then prepared by adding the silanized reinforcing material to dimethyl sulfoxide at a mass ratio of 21.5:11.5:7:100 (1,4-cyclohexadiene-1,2-dicarboxylic anhydride, 1-ethyl-(3-dimethylaminopropyl)carbodiimide, N-hydroxysuccinimide, and dimethyl sulfoxide). Succinimide was added to dimethyl sulfoxide and stirred for 1 hour to obtain component B. Component B was added to component A at a mass ratio of 4:1. The mixture was then reacted at 60°C for 23 hours. After the reaction, the mixture was filtered, centrifuged at 15,000 rpm for 8 minutes, and washed three times each with anhydrous ethanol and deionized water (each time the mass of ethanol was equal to the mass of N-hydroxysuccinimide, and each time the mass of deionized water was equal to the mass of N-hydroxysuccinimide). Finally, the mixture was vacuum dried at 60°C for 12 hours to obtain the modified material.

[0064] The preparation method of silanized reinforced materials includes the following steps:

[0065] The mass ratio of 3-aminopropyltriethoxysilane, ethanol, and deionized water to reinforcing material was 0.5:100:1.9. 3-aminopropyltriethoxysilane was added to the ethanol and deionized water mixture (volume ratio of ethanol to deionized water was 49:1), and the mixture was ultrasonically treated for 20 min (ultrasonic power was 100 W, ultrasonic frequency was 40 kHz). Then, the reinforcing material was added, and the mixture was stirred at 500 rpm for 6 h at 80 °C. After filtration, the mixture was washed three times each with ethanol and deionized water (each time the mass of ethanol was 6 times the mass of the reinforcing material, and each time the mass of deionized water was 7 times the mass of the reinforcing material). Finally, the mixture was vacuum dried at 60 °C for 12 h to obtain the silanized reinforcing material.

[0066] The preparation method of the reinforcing material includes the following steps:

[0067] Graphene oxide was added to anhydrous ethanol at a mass ratio of 0.6:100, and the mixture was ultrasonically treated for 0.7 h (ultrasonic power 100 W, ultrasonic frequency 40 kHz) to obtain a graphene oxide dispersion. Cerium nitrate hexahydrate, aluminum nitrate nonahydrate, anhydrous ethanol, and deionized water were added to anhydrous ethanol at a mass ratio of 0.1:0.1:50:25, and stirred until homogeneous. Then, deionized water was added... Water was added and stirred for 30 minutes to obtain a precursor solution. The precursor solution was added to the graphene oxide dispersion at a mass ratio of 1:2. The mixture was then stirred at 150 rpm for 8 hours in a water bath at 80°C. After cooling to room temperature, the mixture was filtered and washed three times with deionized water (each wash being 60% of the total mass of the deionized water). The mixture was then vacuum dried at 50°C for 24 hours and finally calcined at 400°C for 2 hours to obtain the reinforcing material.

[0068] S3: The composite, the modifying material, and tetradecyl methacrylate were mixed with tetradecyl methacrylate in a mass ratio of 1:1:10. Toluene (toluene mass is 6 times the mass of tetradecyl methacrylate) and benzoyl peroxide (benzoyl peroxide mass is 3% of the mass of tetradecyl methacrylate) were then added. The mixture was polymerized at 100°C for 6 hours. After the reaction was completed, toluene was removed by rotary evaporation at 55°C. The mixture was washed three times with anhydrous ethanol (each time the mass of anhydrous ethanol was 20% of the mass of toluene). The mixture was then vacuum dried at 60°C for 12 hours to obtain the diesel additive. Example 3

[0069] The preparation method of diesel additives includes the following steps:

[0070] S1: The acid compound, low-temperature flow modifier, and tetrahydrofuran were added to tetrahydrofuran in a mass ratio of 1.6:1.1:60. Then, p-toluenesulfonic acid (3% of the mass of the acid compound) was added. The mixture was stirred at 105°C for 11 hours under a nitrogen atmosphere. After the reaction was completed, the tetrahydrofuran was removed by rotary evaporation at 50°C. The mixture was washed three times with ethanol (30% of the mass of tetrahydrofuran each time). Finally, it was vacuum dried at 65°C for 10 hours to obtain the complex. The acid compound was composed of ricinoleic acid and ferulic acid in a mass ratio of 1.1:0.8. The low-temperature flow modifier was composed of 1-adamantanol and triglyceride lactate in a mass ratio of 0.9:0.5.

[0071] S2: Component A is obtained by adding the silanized reinforcing material to dimethyl sulfoxide at a mass ratio of 5.2:60 and mixing thoroughly. Then, component A is obtained by adding the silanized reinforcing material to dimethyl sulfoxide at a mass ratio of 22:12:7.5:110. Succinimide was added to dimethyl sulfoxide and stirred for 1.5 h to obtain component B. Component B was added to component A at a mass ratio of 4:1. The mixture was then reacted at 65 °C for 22 h. After the reaction, the mixture was filtered, centrifuged at 20,000 rpm for 5 min, and washed three times each with anhydrous ethanol and deionized water (each time the mass of ethanol was equal to the mass of N-hydroxysuccinimide, and each time the mass of deionized water was equal to the mass of N-hydroxysuccinimide). Finally, the mixture was vacuum dried at 65 °C for 12 h to obtain the modified material.

[0072] The preparation method of silanized reinforced materials includes the following steps:

[0073] The mass ratio of 3-aminopropyltriethoxysilane, ethanol, and deionized water to reinforcing material was 0.6:110:2. 3-aminopropyltriethoxysilane was added to the ethanol and deionized water mixture (volume ratio of ethanol to deionized water was 49:1), and the mixture was ultrasonically treated for 25 min (ultrasonic power 100 W, ultrasonic frequency 40 kHz). Then, the reinforcing material was added, and the mixture was stirred at 600 rpm for 5 h at 85 °C. After filtration, the mixture was washed three times each with ethanol and deionized water (each time the mass of ethanol was 6 times the mass of the reinforcing material, and each time the mass of deionized water was 7 times the mass of the reinforcing material). Finally, the mixture was vacuum dried at 65 °C for 12 h to obtain the silanized reinforcing material.

[0074] The preparation method of the reinforcing material includes the following steps:

[0075] Graphene oxide was added to anhydrous ethanol at a mass ratio of 0.7:110, and the mixture was ultrasonically treated for 1 hour (ultrasonic power 100W, ultrasonic frequency 40kHz) to obtain a graphene oxide dispersion. Cerium nitrate hexahydrate, aluminum nitrate nonahydrate, anhydrous ethanol, and deionized water were added to anhydrous ethanol at a mass ratio of 0.15:0.15:55:30, and stirred until homogeneous. Then, deionized water was added. The mixture was stirred for 35 minutes to obtain a precursor solution. The precursor solution was added to the graphene oxide dispersion at a mass ratio of 1:2. The mixture was then stirred at 200 rpm for 7 hours in a water bath at 85°C. After cooling to room temperature, the mixture was filtered and washed three times with deionized water (each wash being 60% of the total deionized water mass). The mixture was then vacuum dried at 55°C for 24 hours and finally calcined at 410°C for 1.5 hours to obtain the reinforced material.

[0076] S3: According to the mass ratio of the composite, the modifying material, and tetradecyl methacrylate of 1.5:1.5:10.5, the composite from step S1, the modifying material from step S2, and tetradecyl methacrylate are mixed, and then toluene (toluene mass is 6 times the mass of tetradecyl methacrylate) and benzoyl peroxide (benzoyl peroxide mass is 3% of the mass of tetradecyl methacrylate) are added. Then, the polymerization reaction is carried out at 105℃ for 5 hours. After the reaction is completed, toluene is removed by rotary evaporation at 60℃, and the mixture is washed 3 times with anhydrous ethanol (each time the mass of anhydrous ethanol is 20% of the mass of toluene). Finally, the mixture is vacuum dried at 65℃ for 12 hours to obtain the diesel additive.

[0077] Comparative Example 1

[0078] The difference between this comparative example and Example 3 is that, in the preparation of the diesel additive, in step S1, the acid compound is replaced by an equal mass of ricinoleic acid, while the remaining steps and raw materials are the same as in Example 3.

[0079] S1: Castor oil acid, low-temperature flow modifier, and tetrahydrofuran were added to tetrahydrofuran at a mass ratio of 1.6:1.1:60, followed by the addition of p-toluenesulfonic acid (3% of the mass of castor oil acid). The mixture was then stirred at 105°C for 11 hours under a nitrogen atmosphere. After the reaction was completed, tetrahydrofuran was removed by rotary evaporation at 50°C. The mixture was washed three times with ethanol (each time with ethanol at a mass of 30% of the mass of tetrahydrofuran), and finally dried under vacuum at 65°C for 10 hours to obtain the complex. The low-temperature flow modifier was composed of 1-adamantanol and triglyceride lactate at a mass ratio of 0.9:0.5.

[0080] Comparative Example 2

[0081] The difference between this comparative example and Example 3 is that, in the preparation of the diesel additive, in step S1, the acid compound is replaced by ferulic acid by an equal mass, while the remaining steps and raw materials are the same as in Example 3.

[0082] S1: Ferulic acid, low-temperature flow modifier, and tetrahydrofuran were added to tetrahydrofuran at a mass ratio of 1.6:1.1:60, followed by the addition of p-toluenesulfonic acid (3% of the mass of ferulic acid). The mixture was then stirred at 105°C for 11 hours under a nitrogen atmosphere. After the reaction was completed, the tetrahydrofuran was removed by rotary evaporation at 50°C. The mixture was washed three times with ethanol (each time with ethanol at a mass of 30% of the mass of tetrahydrofuran), and finally dried under vacuum at 65°C for 10 hours to obtain the complex. The low-temperature flow modifier was composed of 1-adamantanol and triglyceride lactate at a mass ratio of 0.9:0.5.

[0083] Comparative Example 3

[0084] The difference between this comparative example and Example 3 is that, in the preparation of the diesel additive, in step S1, the low-temperature flow improver is replaced by 1-adamantanol, while the remaining steps and raw materials are the same as in Example 3.

[0085] S1: The acid compound, 1-adamantanol, and tetrahydrofuran were added to tetrahydrofuran in a mass ratio of 1.6:1.1:60. Then, p-toluenesulfonic acid (3% of the mass of the acid compound) was added. The mixture was stirred at 105°C for 11 h under a nitrogen atmosphere. After the reaction was completed, the tetrahydrofuran was removed by rotary evaporation at 50°C. The mixture was washed three times with ethanol (30% of the mass of tetrahydrofuran each time). Finally, the mixture was vacuum dried at 65°C for 10 h to obtain the complex. The acid compound was composed of ricinoleic acid and ferulic acid in a mass ratio of 1.1:0.8.

[0086] Comparative Example 4

[0087] The difference between this comparative example and Example 3 is that, in the preparation of the diesel additive, in step S1, the low-temperature flow improver is replaced by three-arm lactic acid glyceride, while the remaining steps and raw materials are the same as in Example 3.

[0088] S1: The acid compound, three-arm lactic acid glyceride, and tetrahydrofuran were added to tetrahydrofuran in a mass ratio of 1.6:1.1:60. Then, p-toluenesulfonic acid (3% of the mass of the acid compound) was added. The mixture was stirred at 105°C for 11 h under a nitrogen atmosphere. After the reaction was completed, the tetrahydrofuran was removed by rotary evaporation at 50°C. The mixture was washed three times with ethanol (30% of the mass of tetrahydrofuran each time). Finally, the mixture was vacuum dried at 65°C for 10 h to obtain the complex. The acid compound was composed of ricinoleic acid and ferulic acid in a mass ratio of 1.1:0.8.

[0089] Comparative Example 5

[0090] The difference between this comparative example and Example 3 is that, in the preparation of the diesel additive, in step S2, the reinforcing material is prepared by loading alumina onto graphene oxide, while the remaining steps and raw materials are the same as in Example 3.

[0091] The preparation method of the reinforcing material includes the following steps:

[0092] Graphene oxide was added to anhydrous ethanol at a mass ratio of 0.7:110 and ultrasonically treated for 1 hour (ultrasonic power 100W, ultrasonic frequency 40kHz) to obtain a graphene oxide dispersion. Aluminum nitrate nonahydrate was added to anhydrous ethanol at a mass ratio of 0.3:55:30 and stirred evenly. Then deionized water was added and stirred for 35 minutes to obtain a precursor solution. The precursor solution was added to the graphene oxide dispersion at a mass ratio of 1:2. The mixture was then stirred at 200 rpm for 7 hours in a water bath at 85°C. After cooling to room temperature, the mixture was filtered, washed three times with deionized water (each time the deionized water mass was 60% of the above deionized water mass), vacuum dried at 55°C for 24 hours, and finally calcined at 410°C for 1.5 hours to obtain the reinforcing material.

[0093] Comparative Example 6

[0094] The difference between this comparative example and Example 3 is that, in the preparation of the diesel additive, in step S2, the reinforcing material is prepared by loading cerium oxide onto graphene oxide, while the remaining steps and raw materials are the same as in Example 3.

[0095] The preparation method of the reinforcing material includes the following steps:

[0096] Graphene oxide was added to anhydrous ethanol at a mass ratio of 0.7:110 and ultrasonically treated for 1 hour (ultrasonic power 100W, ultrasonic frequency 40kHz) to obtain a graphene oxide dispersion. Cerium nitrate hexahydrate was added to anhydrous ethanol at a mass ratio of 0.3:55:30 and stirred evenly. Then deionized water was added and stirred for 35 minutes to obtain a precursor solution. The precursor solution was added to the graphene oxide dispersion at a mass ratio of 1:2. The mixture was then stirred at 200 rpm for 7 hours in a water bath at 85°C. After cooling to room temperature, the mixture was filtered, washed three times with deionized water (each time the deionized water mass was 60% of the above deionized water mass), vacuum dried at 55°C for 24 hours, and finally calcined at 410°C for 1.5 hours to obtain the reinforcing material.

[0097] Comparative Example 7

[0098] The difference between this comparative example and Example 3 is that, in the preparation of diesel additive, in step S2, 1,4-cyclohexadiene-1,2-dicarboxylic anhydride is replaced by maleic anhydride by an equal mass, while the remaining steps and raw materials are the same as in Example 3.

[0099] S2: Following a mass ratio of silanized reinforcing material to dimethyl sulfoxide of 5.2:60, the silanized reinforcing material was added to dimethyl sulfoxide and mixed thoroughly to obtain component A. Then, following a mass ratio of maleic anhydride, 1-ethyl-(3-dimethylaminopropyl)carbodiimide, N-hydroxysuccinimide, and dimethyl sulfoxide of 22:12:7.5:110, maleic anhydride, 1-ethyl-(3-dimethylaminopropyl)carbodiimide, and N-hydroxysuccinimide were added to dimethyl sulfoxide. Stirring for 1.5 h yielded component B. Component B was added to component A at a mass ratio of 4:1. The mixture was then reacted at 65 °C for 22 h. After the reaction, the mixture was filtered, centrifuged at 20,000 rpm for 5 min, and washed three times each with anhydrous ethanol and deionized water (each time the mass of ethanol was equal to the mass of N-hydroxysuccinimide, and each time the mass of deionized water was equal to the mass of N-hydroxysuccinimide). Finally, the mixture was vacuum dried at 65 °C for 12 h to obtain the modified material.

[0100] Comparative Example 8

[0101] The difference between this comparative example and Example 3 is that, in the preparation of the diesel additive, in step S3, the complex is combined with tetradecyl methacrylate through a polymerization reaction, while the remaining steps and raw materials are the same as in Example 3.

[0102] S3: The complex from step S1 was mixed with tetradecyl methacrylate at a mass ratio of 3:10.5, and then toluene (toluene mass is 6 times the mass of tetradecyl methacrylate) and benzoyl peroxide (benzoyl peroxide mass is 3% of the mass of tetradecyl methacrylate) were added. The mixture was then polymerized at 105℃ for 5 hours. After the reaction was completed, toluene was removed by rotary evaporation at 60℃. The mixture was washed three times with anhydrous ethanol (each time anhydrous ethanol mass is 20% of the mass of toluene), and then vacuum dried at 65℃ for 12 hours to obtain the diesel additive.

[0103] Comparative Example 9

[0104] The difference between this comparative example and Example 3 is that, in the preparation of the diesel additive, in step S3, the modified material is combined with tetradecyl methacrylate through a polymerization reaction, while the remaining steps and raw materials are the same as in Example 3.

[0105] S3: The modified material and tetradecyl methacrylate were mixed in step S2 at a mass ratio of 3:10.5. Toluene (toluene mass is 6 times the mass of tetradecyl methacrylate) and benzoyl peroxide (benzoyl peroxide mass is 3% of the mass of tetradecyl methacrylate) were then added. The mixture was polymerized at 105℃ for 5 hours. After the reaction was completed, toluene was removed by rotary evaporation at 60℃. The mixture was washed three times with anhydrous ethanol (each time the mass of anhydrous ethanol was 20% of the mass of toluene). The mixture was then vacuum dried at 65℃ for 12 hours to obtain the diesel additive.

[0106] The performance of the diesel additives prepared in Examples 1-3 and Comparative Examples 1-9 was tested. Diesel additives prepared in Examples 1-3 and Comparative Examples 1-9 were added to palm acidified oil biodiesel at a concentration of 1000 mg / kg. The palm acidified oil biodiesel used was provided by Fujian Longyan Zhuoyue New Energy Co., Ltd. Diesel additives prepared in Examples 1-3 and Comparative Examples 1-9 were added to biodiesel produced from waste cooking oil at a concentration of 1500 mg / kg. The waste cooking oil biodiesel used was produced by Zhejiang Ningbo Jiesheng Bioenergy Co., Ltd. The low-temperature flow properties, oxidation stability, and anti-wear properties of the two types of biodiesel were tested.

[0107] Low temperature flow performance test: The cold filter point test was conducted according to the SH / T 0248-2006 standard. The cold filter point is the highest temperature at which the volume of liquid passing through the filter screen of the sample does not exceed 20 ml within a specified time. The arithmetic mean of two repeated measurements was taken as the cold filter point of the sample. The test results are shown in Table 1 and Table 2 below.

[0108] Oxidative stability test: The oxidative stability of biodiesel was evaluated by determining the induction period at 110°C using the EN 14112 method (Racimat method). The instrument used was a Metrohm 743 oil oxidative stability tester from Switzerland. A longer induction period indicates better oxidative stability of biodiesel, while a shorter induction period indicates poorer oxidative stability. The Chinese national standard stipulates that the oxidative stability induction period of biodiesel shall not be less than 6 hours. The test results are shown in Tables 1 and 2 below.

[0109] Wear resistance test: The wear resistance test was conducted according to the SH / T 0756-2005 standard. The wear scar diameter (µm) was measured. The larger the wear scar diameter, the worse the wear resistance. The test results are shown in Table 1 and Table 2 below.

[0110] Table 1 Performance parameters of palm oil biodiesel

[0111]

[0112] Table 2 Performance parameters of biodiesel produced from waste cooking oil

[0113]

[0114] As shown in Tables 1 and 2 above, and comparing Comparative Examples 1-4 with Example 3, in step S1, replacing the acidic compounds with ricinoleic acid or ferulic acid by the same mass, or replacing the low-temperature flow improver with 1-adamantanol or tri-arm lactic acid glyceride by the same mass, the test results of the diesel additive were worse than those of Example 3. This indicates that the acidic compounds composed of ricinoleic acid and ferulic acid have a synergistic effect, which can effectively improve the oxidation stability and low-temperature flow performance of the diesel additive, and further improve the anti-wear effect of the diesel additive. The low-temperature flow improver composed of 1-adamantanol and tri-arm lactic acid glyceride has a synergistic effect, which can better improve the low-temperature flow performance and oxidation stability of the diesel additive, effectively reduce the cold filter plugging point of biomass diesel, and provide additional lubrication effect, further enhancing the anti-wear performance of the diesel additive.

[0115] Comparing Comparative Examples 5-7 and Example 3, it can be seen that in step S2, the reinforcing material is prepared by loading alumina onto graphene oxide, or by loading cerium oxide onto graphene oxide, or by replacing 1,4-cyclohexadiene-1,2-dicarboxylic anhydride with maleic anhydride by mass, and finally preparing diesel additive. The test results are worse than those of Example 3, indicating that loading alumina and cerium oxide together onto graphene oxide can play a synergistic role, effectively improving the anti-wear performance, oxidation stability and low-temperature flowability of diesel additive. Furthermore, combining 1,4-cyclohexadiene-1,2-dicarboxylic anhydride with silanized reinforcing material not only has good bonding force, but also improves the dispersibility of reinforcing material, further improving the low-temperature flowability, oxidation stability and anti-wear performance of diesel additive.

[0116] Comparing Comparative Examples 8-9 and Example 3, it can be seen that in step S3, the test results of combining the complex with tetradecyl methacrylate through a polymerization reaction, or combining the modified material with tetradecyl methacrylate through a polymerization reaction, to finally prepare the diesel additive are worse than those of Example 3. This indicates that combining the complex, the modified material, and tetradecyl methacrylate through a polymerization reaction results in better bonding and synergistic effects, further improving the low-temperature flow properties, oxidation stability, and anti-wear properties of the diesel additive.

[0117] As shown in Tables 1 and 2 above, the diesel additives prepared in Examples 1-3, compared to those prepared in Comparative Examples 1-9, achieved the required performance by combining acid compounds with low-temperature flow modifiers to obtain a complex, combining 1,4-cyclohexadiene-1,2-dicarboxylic anhydride with silanized reinforcing materials to obtain a modified material, and combining the complex, modified material, and tetradecyl methacrylate to finally obtain the diesel additive. In contrast, the diesel additives prepared in Comparative Examples 1-9 did not meet the performance requirements. This indicates that the diesel additives prepared in this invention not only possess good low-temperature flow properties, oxidation stability, and anti-wear properties, but also exhibit excellent overall performance and enhance the performance of biomass diesel, extending its service life.

[0118] In the description of this specification, the references to terms such as "an embodiment," "example," "specific example," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0119] The above description is merely an example and illustration of the present invention. Those skilled in the art can make various modifications or additions to the specific embodiments described or use similar methods to replace them, as long as they do not deviate from the invention or exceed the scope defined by the present invention, they should all fall within the protection scope of the present invention.

Claims

1. A method for preparing a diesel additive, characterized in that, Includes the following steps: S1: An acid compound is combined with a low-temperature flow modifier through an esterification reaction to obtain a complex; The acidic compound is composed of ricinoleic acid and ferulic acid in a mass ratio of 0.9-1.1:0.7-0.

8. The low-temperature flow improver is composed of a mixture of 1-adamantanol and triglyceride lactate in a mass ratio of 0.8-0.9:0.4-0.

5. S2: Combining 1,4-cyclohexadiene-1,2-dicarboxylic anhydride with silanized reinforcing materials yields modified materials; The method for preparing the silanized reinforced material includes the following steps: The silane coupling agent is added to a mixed solution of ethanol and deionized water and ultrasonically treated for 15-25 minutes. Then, the reinforcing material is added and stirred at 75-85℃ for 5-7 hours. After filtration, the material is washed with ethanol and deionized water and finally vacuum dried at 55-65℃ to obtain the silanized reinforcing material. The method for preparing the reinforcing material includes the following steps: Graphene oxide was added to anhydrous ethanol and sonicated for 0.5-1 h to obtain a graphene oxide dispersion. Cerium nitrate hexahydrate and aluminum nitrate nonahydrate were added to anhydrous ethanol and stirred until homogeneous. Then, deionized water was added and stirred for 25-35 min to obtain a precursor solution. The precursor solution was added to the graphene oxide dispersion and stirred in a water bath at 75-85℃ for 7-9 h. After cooling to room temperature, the mixture was filtered, washed with deionized water, vacuum dried at 45-55℃, and finally calcined at 390-410℃ for 1.5-2.5 h to obtain the reinforced material. S3: The complex in step S1, the modified material in step S2, and tetradecyl methacrylate are combined by graft copolymerization to finally obtain a diesel additive.

2. The method for preparing a diesel additive according to claim 1, characterized in that, Step S1 is as follows: An acid compound and a low-temperature flow modifier were added to tetrahydrofuran, followed by a catalyst. The mixture was then stirred and reacted under a nitrogen atmosphere at 95-105°C for 11-13 hours. After the reaction was completed, the tetrahydrofuran was removed by rotary evaporation, washed with ethanol, and finally dried under vacuum at 55-65°C to obtain the complex.

3. The method for preparing a diesel additive according to claim 1, characterized in that, Step S2 is as follows: The silanized reinforcing material was added to dimethyl sulfoxide and mixed evenly to obtain component A. 1,4-cyclohexadiene-1,2-dicarboxylic anhydride, 1-ethyl-(3-dimethylaminopropyl)carbodiimide and N-hydroxysuccinimide were added to dimethyl sulfoxide and stirred for 0.5-1.5 h to obtain component B. Component B was added to component A, and the mixture was reacted at 55-65 °C for 22-24 h. After the reaction was completed, the mixture was filtered, centrifuged for 5-10 min, washed with anhydrous ethanol and deionized water, and finally vacuum dried at 55-65 °C to obtain the modified material.

4. The method for preparing a diesel additive according to claim 1, characterized in that, Step S3 is as follows: The composite from step S1, the modified material from step S2, and tetradecyl methacrylate were mixed, and then toluene and a catalyst were added. The mixture was then polymerized at 95-105°C for 5-7 hours. After the reaction was completed, toluene was removed by rotary evaporation, the mixture was washed with anhydrous ethanol, and then vacuum dried at 55-65°C to obtain the diesel additive.

5. A diesel additive prepared by the method according to any one of claims 1-4.

6. The application of the diesel additive as described in claim 5 in biodiesel.

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