CN114479965A - Composite nano diesel oil pour point depressant and preparation method and application thereof - Google Patents
Composite nano diesel oil pour point depressant and preparation method and application thereof Download PDFInfo
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- 230000000994 depressogenic effect Effects 0.000 title claims abstract description 56
- 239000002131 composite material Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000002283 diesel fuel Substances 0.000 title claims description 52
- 238000002156 mixing Methods 0.000 claims abstract description 27
- 239000002086 nanomaterial Substances 0.000 claims abstract description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 17
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 9
- -1 aminopropyl Chemical group 0.000 claims abstract description 8
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 22
- 238000005406 washing Methods 0.000 claims description 15
- 238000009833 condensation Methods 0.000 claims description 13
- 230000005494 condensation Effects 0.000 claims description 13
- 235000019441 ethanol Nutrition 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001291 vacuum drying Methods 0.000 claims description 11
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical group CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 239000000155 melt Substances 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- 238000010025 steaming Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- 238000002390 rotary evaporation Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 3
- 125000003944 tolyl group Chemical group 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 abstract description 11
- 229920000642 polymer Polymers 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000013078 crystal Substances 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000008014 freezing Effects 0.000 description 3
- 238000007710 freezing Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 239000000446 fuel Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 239000003209 petroleum derivative Substances 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000000881 depressing effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical class O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 229920013639 polyalphaolefin Polymers 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
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- 238000001308 synthesis method Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L1/00—Liquid carbonaceous fuels
- C10L1/10—Liquid carbonaceous fuels containing additives
- C10L1/106—Liquid carbonaceous fuels containing additives mixtures of inorganic compounds with organic macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L1/00—Liquid carbonaceous fuels
- C10L1/10—Liquid carbonaceous fuels containing additives
- C10L1/12—Inorganic compounds
- C10L1/1291—Silicon and boron containing compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L1/00—Liquid carbonaceous fuels
- C10L1/10—Liquid carbonaceous fuels containing additives
- C10L1/14—Organic compounds
- C10L1/18—Organic compounds containing oxygen
- C10L1/192—Macromolecular compounds
- C10L1/195—Macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C10L1/196—Macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds derived from monomers containing a carbon-to-carbon unsaturated bond and a carboxyl group or salts, anhydrides or esters thereof homo- or copolymers of compounds having one or more unsaturated aliphatic radicals each having one carbon bond to carbon double bond, and at least one being terminated by a carboxyl radical or of salts, anhydrides or esters thereof
- C10L1/1963—Macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds derived from monomers containing a carbon-to-carbon unsaturated bond and a carboxyl group or salts, anhydrides or esters thereof homo- or copolymers of compounds having one or more unsaturated aliphatic radicals each having one carbon bond to carbon double bond, and at least one being terminated by a carboxyl radical or of salts, anhydrides or esters thereof mono-carboxylic
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- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
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Abstract
The invention relates to a composite nano diesel pour point depressant, a preparation method and application thereof, wherein the preparation method comprises the following steps: 1) adding a silane coupling agent with aminopropyl and nano silicon dioxide into a solvent A, heating and stirring, and carrying out post-treatment to obtain a nano material; 2) and adding the nano material and polyethylene-vinyl acetate into the solvent B, performing melt blending, and separating to obtain the composite nano diesel pour point depressant. Compared with the prior art, the nano-silica material treated by the silane coupling agent has organic compatibility, and is compounded with the oil-soluble polymer to prepare the composite nano-diesel pour point depressant, so that the pour point depression effect is effectively enhanced, the low-temperature flow property of diesel is improved, and the application prospect of the nano-silica material in the field of diesel pour point depressants is expanded.
Description
Technical Field
The invention belongs to the technical field of diesel pour point depressants, and relates to a composite nano diesel pour point depressant, and a preparation method and application thereof.
Background
The diesel oil is a light petroleum product mainly containing long-chain carbon number alkane, and has wide application in national defense, industry, agriculture, logistics transportation, life and other aspects. However, diesel oil in China has high wax content, is easy to wax under low temperature conditions, wax crystals grow rapidly at low temperature and lose low-temperature fluidity rapidly, so that a fuel pipeline or a filter in a diesel engine fuel system is blocked, and the storage, transportation and use of oil products in cold regions are seriously influenced.
The low-temperature fluidity of the diesel can be obviously enhanced by adding a small amount of pour point depressant. At present, common diesel pour point depressants include polymethacrylates, polyethylene-vinyl acetates, poly-alpha-olefins, maleic anhydrides and the like. However, the existing diesel oil pour point depressant is of a single type, and the type of the extended pour point depressant is the focus of continuous research in the field.
Disclosure of Invention
The invention aims to provide a composite nano diesel pour point depressant and a preparation method and application thereof. According to the invention, the nano-silica material treated by the silane coupling agent obtains organic compatibility, and is compounded with the oil-soluble polymer to prepare the composite nano-diesel pour point depressant, so that the pour point depression effect is effectively enhanced, the low-temperature flow property of diesel is improved, and the application prospect of the nano-material in the field of diesel pour point depressants is expanded.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of a composite nano diesel pour point depressant comprises the following steps:
1) adding a silane coupling agent with aminopropyl and nano silicon dioxide (the preferable particle size is 18-22nm) into a solvent A, heating and stirring, and carrying out post-treatment to obtain a nano material;
2) and adding the nano material and polyethylene-vinyl acetate (EVA) into a solvent B, performing melt blending, and separating to obtain the composite nano diesel pour point depressant.
Further, in the step 1), the silane coupling agent is aminopropyl-triethoxysilane, the solvent A is formed by mixing ethanol and water according to a volume ratio of (8-10) to 1 (stirring at room temperature for 0.8-1.2h after mixing), and the mass ratio is preferably 9: 1.
Further, in the step 1), the mass ratio of the silane coupling agent to the nano silica is 1 (2.5-3.5), preferably 1: 3.
Further, in the step 1), the heating and stirring temperature is 70-80 ℃, preferably 75 ℃, and the time is 2.5-3.5h, preferably 3 h; the post-treatment comprises centrifugation, washing, drying and grinding.
Further, the centrifugation temperature is 50-70 ℃, preferably 60 ℃, and the time is 8-12min, preferably 10 min; washing with water; vacuum drying is adopted for drying, the drying temperature is 50-70 ℃, preferably 60 ℃, and the drying time is 10-14h, preferably 12 h; after grinding, the particle size of the nanomaterial is 18-22nm, preferably 20 nm.
Further, in the step 2), the solvent B is toluene; the mass ratio of the nano material to the polyethylene-vinyl acetate is (0.5-1.5): 1.
Further, in the step 2), the melt blending is carried out under stirring, the temperature of the melt blending is 75-85 ℃, preferably 80 ℃, and the time is 2.5-3.5h, preferably 3 h; the separation comprises rotary steaming, washing and drying.
Further, the rotary steaming temperature is 50-70 ℃, preferably 60 ℃, and the time is 30-40min, preferably 35 min; washing with absolute ethyl alcohol; the drying is carried out in vacuum at 50-70 deg.C, preferably 60 deg.C for 10-14h, preferably 12 h.
The composite nano diesel oil pour point depressant is prepared by adopting the method.
The application of the composite nano diesel oil pour point depressant is used for reducing the cold filter plugging point and the condensation point of diesel oil.
Compared with the prior art, the invention has the following characteristics:
1) in the invention, the silane coupling agent with aminopropyl is mixed with the nano-silica to realize better fusion of inorganic matters and organic matters, and the silane coupling agent containing N is introduced into the nano-silica to increase the polarity of the nano-silica and the solubility and the dispersibility of the nano-silica in diesel oil;
2) the polymer polyethylene-vinyl acetate (EVA) used in the invention is a polymer with very good oil solubility, the ester group structure of the polymer provides a large number of crystallization sites for diesel oil, and a part of wax crystals grow on the crystallization sites and are mutually dispersed rather than clustered together, so that the size of the wax crystals is reduced, the condensation point and the cold filter plugging point of the diesel oil are reduced, and the low-temperature flow property of the diesel oil is improved;
3) in the composite nano diesel pour point depressant obtained by melting and blending the nano material and the EVA, the inorganic silicon material and the organic polymer generate synergistic action, and the inorganic silicon material and the organic polymer provide a larger amount of crystallization sites, so that wax crystals are more uniformly dispersed in the diesel, and the low-temperature fluidity of the diesel is further improved;
4) in the invention, the composite nano diesel pour point depressant has simple synthesis method, small dosage and stable performance;
5) the composite nano diesel oil pour point depressant prepared by the invention effectively reduces the condensation point and the cold filter plugging point of diesel oil, and experiments show that the composite nano diesel oil pour point depressant is added into the commercially available 0#In the diesel oil, the condensation point can be reduced by 6-12 ℃, the cold filter plugging point can be reduced by 3-8 ℃, the pour point depressing effect is effectively enhanced, the low-temperature flow property of the diesel oil is improved, and the application prospect of the nano material in the field of diesel oil pour point depressants is expanded.
Drawings
Fig. 1 is a photograph of the prepared nanomaterial.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
The invention provides a preparation method of a composite nano diesel pour point depressant, which comprises the following steps:
1) adding a silane coupling agent with aminopropyl and nano silicon dioxide into a solvent A, heating and stirring, and carrying out post-treatment to obtain a nano material, wherein the nano material is shown in figure 1;
2) and adding the nano material and polyethylene-vinyl acetate into the solvent B, performing melt blending, and separating to obtain the composite nano diesel pour point depressant.
In the step 1), the silane coupling agent is aminopropyl-triethoxysilane, and the solvent A is formed by mixing ethanol and water according to the volume ratio (8-10) to 1. The mass ratio of the silane coupling agent to the nano silicon dioxide is 1 (2.5-3.5). Heating and stirring at 70-80 deg.C for 2.5-3.5 h; the post-treatment comprises centrifugation, washing, drying and grinding. Centrifuging at 50-70 deg.C for 8-12 min; washing with water; the drying adopts vacuum drying, the drying temperature is 50-70 ℃, and the drying time is 10-14 h.
In the step 2), the solvent B is toluene; the mass ratio of the nano material to the polyethylene-vinyl acetate is (0.5-1.5): 1. The melt blending is carried out under stirring, the temperature of the melt blending is 75-85 ℃, and the time is 2.5-3.5 h; the separation comprises rotary steaming, washing and drying. The rotary steaming temperature is 50-70 deg.C, and the time is 30-40 min; washing with absolute ethyl alcohol; vacuum drying at 50-70 deg.C for 10-14 h; after grinding, the particle size of the nano material is 18-22 nm.
The invention also provides a composite nano diesel oil pour point depressant which is prepared by the method.
The invention also provides an application of the composite nano diesel oil pour point depressant, and the composite nano diesel oil pour point depressant is used for reducing the cold filter plugging point and the condensation point of diesel oil. Particularly, when in application, the composite nano diesel oil pour point depressant is added into the commercially available 0#In the diesel oil, the adding amount is 0.05wt percent of the mass of the diesel oil-0.2 wt% and sonicating at 30-40 ℃ for 30-40 min.
In the following examples, each of the raw materials used was purchased from Shanghai Tantake technology, Inc.; the measuring method of the condensation point and the cold filter plugging point is carried out according to GB/T510-1991 petroleum product condensation point measuring method and SH/T0248-2006 diesel oil and civil heating oil cold filter plugging point measuring method respectively.
Example 1:
a composite nano diesel pour point depressant for reducing the cold filter plugging point and the condensation point of diesel is prepared by mixing aminopropyl-triethoxysilane and nano-silica, separating and purifying the mixture, and then melting and blending the mixture with a polyethylene vinyl acetate (EVA) copolymer, wherein the preparation process comprises the following steps:
1) putting the single-neck flask into a constant-temperature magnetic stirrer, adding 45ml of ethanol and 5ml of deionized water into the single-neck flask, mixing and stirring at room temperature for 1 h;
after stirring, 2.0g of aminopropyl-triethoxysilane and 6.0g of nanosilicon dioxide were added to the ethanol solution and stirred at 75 ℃ for 3 h.
And after the reaction is finished, centrifuging the product at 60 ℃ for 10min to completely separate the solution from the nano material, drying the solution in a vacuum drying oven at 60 ℃ for 12h to remove a small amount of residual ethanol and water, and grinding the solution by using a mortar to obtain fine and compact nano particles.
2) Putting the single-neck flask into a constant-temperature magnetic stirrer, installing a reflux condenser tube, ultrasonically dissolving 0.5g of nano material and 1.0g of polyethylene-vinyl acetate polymer into 20ml of toluene, mixing, heating to 80 ℃, stirring to completely dissolve solids, and continuously heating for 3 hours;
and after the reaction is finished, cooling to room temperature, carrying out rotary evaporation for 35min at 60 ℃ by using a rotary evaporator, removing the solvent toluene, washing by using excessive absolute ethyl alcohol, removing the reactants which are not melted and blended, then putting into a vacuum drying oven, and drying for 12h at 60 ℃ to finally obtain the composite nano diesel oil pour point depressant.
3) Adding the prepared pour point depressant into commercially available 0# diesel oil, wherein the addition amount is 0.05-0.2 wt% of the mass of the diesel oil, and performing ultrasonic treatment at 35 ℃ for 35min to completely dissolve the pour point depressant in the diesel oil.
4) The freezing point was determined according to GB/T510-1991, the cold filter point was determined according to SH/T0248-2006, and the average of the two repeated determinations was taken as the measurement value. The diesel pour point depressant prepared in the example is added before and after 0#The results of the cold filter plugging point and cold filter plugging point tests for diesel fuel are shown in table 1.
TABLE 1
Example 2:
a composite nano diesel pour point depressant for reducing the cold filter plugging point and the condensation point of diesel is prepared by mixing aminopropyl-triethoxysilane and nano-silica, separating and purifying the mixture, and then melting and blending the mixture with a polyethylene vinyl acetate (EVA) copolymer, wherein the preparation process comprises the following steps:
1) putting the single-neck flask into a constant-temperature magnetic stirrer, adding 45ml of ethanol and 5ml of deionized water into the single-neck flask, mixing and stirring at room temperature for 1 h;
after stirring, 2.0g of aminopropyl-triethoxysilane and 6.0g of nanosilicon dioxide were added to the ethanol solution and stirred at 75 ℃ for 3 h.
And after the reaction is finished, centrifuging the product at 60 ℃ for 10min to completely separate the solution from the nano material, drying the solution in a vacuum drying oven at 60 ℃ for 12h to remove a small amount of residual ethanol and water, and grinding the solution by using a mortar to obtain fine and compact nano particles.
2) Putting a single-neck flask into a constant-temperature magnetic stirrer, installing a reflux condenser tube, ultrasonically dissolving 1.0g of nano material and 1.0g of polyethylene-vinyl acetate polymer into 20ml of toluene, mixing, heating to 80 ℃, stirring to completely dissolve solids, and continuously heating for 3 hours;
and after the reaction is finished, cooling to room temperature, carrying out rotary evaporation for 35min at 60 ℃ by using a rotary evaporator, removing the solvent toluene, washing by using excessive absolute ethyl alcohol, removing the reactants which are not melted and blended, then putting into a vacuum drying oven, and drying for 12h at 60 ℃ to finally obtain the composite nano diesel oil pour point depressant.
3) Adding the prepared pour point depressant into commercially available 0# diesel oil, wherein the addition amount is 0.05-0.2 wt% of the mass of the diesel oil, and performing ultrasonic treatment at 35 ℃ for 35min to completely dissolve the pour point depressant in the diesel oil.
4) The freezing point was determined according to GB/T510-1991, the cold filter point was determined according to SH/T0248-2006, and the average of the two repeated determinations was taken as the measurement value. The diesel pour point depressant prepared in the example is added before and after 0#The results of the cold filter plugging point and cold filter plugging point tests for diesel fuel are shown in table 2.
TABLE 2
Example 3:
a composite nano diesel pour point depressant for reducing the cold filter plugging point and the condensation point of diesel is prepared by mixing aminopropyl-triethoxysilane and nano-silica, separating and purifying the mixture, and then melting and blending the mixture with a polyethylene vinyl acetate (EVA) copolymer, wherein the preparation process comprises the following steps:
1) putting the single-neck flask into a constant-temperature magnetic stirrer, adding 45ml of ethanol and 5ml of deionized water into the single-neck flask, mixing and stirring at room temperature for 1 h;
after stirring, 2.0g of aminopropyl-triethoxysilane and 6.0g of nanosilicon dioxide were added to the ethanol solution and stirred at 75 ℃ for 3 h.
And after the reaction is finished, centrifuging the product at 60 ℃ for 10min to completely separate the solution from the nano material, drying the solution in a vacuum drying oven at 60 ℃ for 12h to remove a small amount of residual ethanol and water, and grinding the solution by using a mortar to obtain fine and compact nano particles.
2) Putting a single-neck flask into a constant-temperature magnetic stirrer, installing a reflux condenser tube, ultrasonically dissolving 1.5g of nano material and 1.0g of polyethylene-vinyl acetate polymer into 20ml of toluene, mixing, heating to 80 ℃, stirring to completely dissolve solids, and continuously heating for 3 hours;
and after the reaction is finished, cooling to room temperature, carrying out rotary evaporation for 35min at 60 ℃ by using a rotary evaporator, removing the solvent toluene, washing by using excessive absolute ethyl alcohol, removing the reactants which are not melted and blended, then putting into a vacuum drying oven, and drying for 12h at 60 ℃ to finally obtain the composite nano diesel oil pour point depressant.
3) Adding the prepared pour point depressant into commercially available 0# diesel oil, wherein the addition amount is 0.05-0.2 wt% of the mass of the diesel oil, and performing ultrasonic treatment at 35 ℃ for 35min to completely dissolve the pour point depressant in the diesel oil.
4) The freezing point was determined according to GB/T510-1991, the cold filter point was determined according to SH/T0248-2006, and the average of the two repeated determinations was taken as the measurement value. The diesel pour point depressant prepared in the example is added before and after 0#The results of the cold filter plugging point and cold filter plugging point tests for diesel fuel are shown in table 3.
TABLE 3
Δ SP represents 0 after addition of the diesel pour point depressant of the present invention#The reduction value of the condensation point of the diesel oil relative to the 0# diesel oil. Δ CFPP represents 0 after addition of the diesel pour point depressant of the present invention#The cold filter plugging point of diesel oil is reduced relative to 0# diesel oil. The test results of the examples 1-3 show that the composite nano diesel oil pour point depressant has obvious improvement effect on the condensation point and the cold filter plugging point of diesel oil compared with pure diesel oil. Especially, when the nano material and the EVA are melted and blended in a mass ratio of 0.5:1, the best pour point depression effect is obtained, the highest pour point depression is 12 ℃ and the cold filter plugging point depression is 8 ℃ under the condition of 0.2 wt% of addition amount.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A preparation method of a composite nano diesel pour point depressant is characterized by comprising the following steps:
1) adding a silane coupling agent with aminopropyl and nano silicon dioxide into the solvent A, heating and stirring, and carrying out post-treatment to obtain a nano material;
2) and adding the nano material and polyethylene-vinyl acetate into the solvent B, performing melt blending, and separating to obtain the composite nano diesel pour point depressant.
2. The preparation method of the composite nano diesel oil pour point depressant according to claim 1, wherein in the step 1), the silane coupling agent is aminopropyl-triethoxysilane, and the solvent A is formed by mixing ethanol and water according to a volume ratio of (8-10) to 1.
3. The preparation method of the composite nano diesel oil pour point depressant according to claim 1, wherein in the step 1), the mass ratio of the silane coupling agent to the nano silicon dioxide is 1 (2.5-3.5).
4. The preparation method of the composite nano diesel pour point depressant according to claim 1, wherein in the step 1), the heating and stirring temperature is 70-80 ℃ and the time is 2.5-3.5 h; the post-treatment comprises centrifugation, washing, drying and grinding.
5. The preparation method of the composite nano diesel pour point depressant according to claim 4, wherein the centrifugation temperature is 50-70 ℃ and the time is 8-12 min; washing with water; vacuum drying at 50-70 deg.C for 10-14 h; after grinding, the particle size of the nano material is 18-22 nm.
6. The method for preparing the composite nano diesel oil pour point depressant according to claim 1, wherein in the step 2), the solvent B is toluene; the mass ratio of the nano material to the polyethylene-vinyl acetate is (0.5-1.5): 1.
7. The preparation method of the composite nanometer diesel pour point depressant according to claim 1, wherein in the step 2), the melt blending is performed under stirring, the temperature of the melt blending is 75-85 ℃, and the time is 2.5-3.5 h; the separation comprises rotary steaming, washing and drying.
8. The preparation method of the composite nano diesel pour point depressant according to claim 7, wherein the rotary evaporation temperature is 50-70 ℃ and the time is 30-40 min; washing with absolute ethyl alcohol; the drying adopts vacuum drying, the drying temperature is 50-70 ℃, and the drying time is 10-14 h.
9. A composite nano diesel oil pour point depressant, characterized in that the composite nano diesel oil pour point depressant is prepared by the method of any one of claims 1 to 8.
10. The use of the composite nano diesel pour point depressant according to claim 9, wherein the composite nano diesel pour point depressant is used for reducing the cold filter plugging point and the condensation point of diesel.
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| CN202210054994.XA CN114479965A (en) | 2022-01-18 | 2022-01-18 | Composite nano diesel oil pour point depressant and preparation method and application thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127409A (en) * | 2011-01-10 | 2011-07-20 | 中国科学院化学研究所 | Crude oil viscosity-breaking pour-point depressant composition, and preparation method and application thereof |
| CN104154422A (en) * | 2014-07-15 | 2014-11-19 | 中国石油天然气股份有限公司 | Crude oil pour point depression and viscosity reduction nano base material compound, preparation method thereof and crude oil |
| CN104984746A (en) * | 2015-07-30 | 2015-10-21 | 西南石油大学 | Modification method for nano silicon dioxide |
| CN105969433A (en) * | 2016-05-23 | 2016-09-28 | 上海应用技术学院 | Nano compound pour point depressant and preparation method thereof |
| CN110016242A (en) * | 2019-04-04 | 2019-07-16 | 深圳先进技术研究院 | The monolayer surface modifying method of nano silica |
-
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127409A (en) * | 2011-01-10 | 2011-07-20 | 中国科学院化学研究所 | Crude oil viscosity-breaking pour-point depressant composition, and preparation method and application thereof |
| CN104154422A (en) * | 2014-07-15 | 2014-11-19 | 中国石油天然气股份有限公司 | Crude oil pour point depression and viscosity reduction nano base material compound, preparation method thereof and crude oil |
| CN104984746A (en) * | 2015-07-30 | 2015-10-21 | 西南石油大学 | Modification method for nano silicon dioxide |
| CN105969433A (en) * | 2016-05-23 | 2016-09-28 | 上海应用技术学院 | Nano compound pour point depressant and preparation method thereof |
| CN110016242A (en) * | 2019-04-04 | 2019-07-16 | 深圳先进技术研究院 | The monolayer surface modifying method of nano silica |
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