CN103013591B - Microemulsified diesel and preparation method thereof - Google Patents
Microemulsified diesel and preparation method thereof Download PDFInfo
- Publication number
- CN103013591B CN103013591B CN201210590857.4A CN201210590857A CN103013591B CN 103013591 B CN103013591 B CN 103013591B CN 201210590857 A CN201210590857 A CN 201210590857A CN 103013591 B CN103013591 B CN 103013591B
- Authority
- CN
- China
- Prior art keywords
- mentioned
- minutes
- emulsifying agent
- raw material
- diesel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Liquid Carbonaceous Fuels (AREA)
Abstract
The invention relates to a microemulsified diesel and a preparation method thereof. The preparation method comprises the following steps: proportionally preparing oleic acid, ammonia water, n-butanol, OP-10 and triethanolamine into a composite emulsifier; and preparing n-butanol and methanol in a proportion of 4:1 into a composite co-emulsifier, thereby preparing the microemulsified diesel which has the characteristics of clear and transparent appearance, high viscosity, high stability and lower price than 0# diesel. The microemulsified diesel has the advantages of low ash content, low sulfur content, low solidifying point, low cold filter plugging point and low density, and satisfies the requirements of Automotive Diesel Fuel for performance indexes of 0# diesel. Meanwhile, the preparation method provided by the invention is simple and easy to implement, and has low environmental pollution.
Description
Technical field
The invention belongs to technical field of fuel oil, be specifically related to a kind of micro emulsion diesel fuel and preparation method thereof.
Background technology
Present increasingly can reduce for exploitation quantity at petroleum resources, under the international big environment of supply growing tension, China's consumption of petroleum in recent ten years but presents the situation increased fast.Severe Energy situation will aggravate the risk of China's oil supply further, also will future period China's oil be caused will to face very severe situation safely.So, tap a new source of energy most important to China with development utilization power-saving technology.
In oil consumption, gasoline and diesel oil occupy sizable ratio.And diesel engine has lot of advantages compared with petrol motor, as long service life, thermo-efficiency is high, power is large and oil consumption is low etc.In recent years, the share that motor vehicle diesel was occupying in European countries is increasing.The potentiality that future diesel car develops in China will be huge, and micro emulsion diesel fuel reduces diesel consumption as diesel engine and improves a kind of new technology of discharge, and the value of its research will be huge.
Had a lot of people to be studied for micro emulsion diesel fuel at present, but the performances such as the ash content of most micro emulsion diesel fuel, sulphur content, condensation point, cold filter clogging temperature and density are difficult to all meet " derv fuel oil " requirement for 0# diesel fuel characteristics index.
Summary of the invention
A technical problem to be solved by this invention is to provide the micro emulsion diesel fuel that a kind of viscosity is high, stability is good.
Another technical problem to be solved by this invention there are provided the preparation method of the micro emulsion diesel fuel that a kind of method is simple, environmental pollution is little.
The technical scheme that technical solution problem of the present invention adopts is made up of the raw material of following proportion by weight:
Mediation basic fuel oil 100 parts
Ethylene-vinyl acetate copolymer 0.02 ~ 0.12 part
Composite antioxidant 0.04 ~ 0.12 part
Ferrocene 0.06 ~ 0.16 part
Above-mentioned mediation basic fuel oil is made up of the raw material of following proportion by weight:
0# diesel oil 76 ~ 86 parts
Compound emulsifying agent 5 ~ 10 parts
8 ~ 13 parts, tap water
Compound helps emulsion 0.8 ~ 1.3 part
Above-mentioned compound emulsifying agent is made up of the raw material of following proportion by weight:
Above-mentioned compound helps emulsion to be made up of the raw material of following proportion by weight:
Propyl carbinol 80 ~ 90 parts
Methyl alcohol 10 ~ 20 parts
Above-mentioned composite antioxidant is that 2,6-di-t-butyl-2-methylamino p-cresol of 1:2 ~ 8 and 2,6-di-tert-butylphenol form by mass ratio.
Above-mentioned micro emulsion diesel fuel, the raw material of preferred following proportion by weight is made:
Mediation basic fuel oil 100 parts
Ethylene-vinyl acetate copolymer 0.04 ~ 0.08 part
Composite antioxidant 0.04 ~ 0.1 part
Ferrocene 0.12 ~ 0.14 part
Above-mentioned mediation basic fuel oil is made up of the raw material of following preferred mass part proportioning:
0# diesel oil 82 ~ 86 parts
Compound emulsifying agent 5 ~ 7 parts
8 ~ 10 parts, water
Compound helps emulsion 0.8 ~ 1.3 part
Above-mentioned compound emulsifying agent is made up of the raw material of following preferred mass part proportioning:
Above-mentioned compound helps emulsion to be made up of the raw material of following preferred mass part proportioning:
Propyl carbinol 80 ~ 85 parts
Methyl alcohol 15 ~ 20 parts
Above-mentioned composite antioxidant is that 2,6-di-t-butyl-2-methylamino p-cresol of 1:2 ~ 6 and 2,6-di-tert-butylphenol form by mass ratio.
Above-mentioned oleic acid acid number is 190 ~ 203mgKOH/g; Containing NH in ammoniacal liquor
3amount is 25% ~ 28%(quality).
In above-mentioned ethylene-vinyl acetate copolymer, vinyl acetate content is 35%(quality).
A preparation method for above-mentioned micro emulsion diesel fuel, comprises following performing step:
Step 1) 25 ~ 35 DEG C, according to corresponding proportioning, first mixes 0# diesel oil and compound emulsifying agent, churning time is 5 ~ 10 minutes, and stirring velocity is 300 ~ 500r/min, adds water stirring and mixes for 5 ~ 10 minutes, add compound and help emulsion, stirring and evenly mixing, make mediation basic fuel oil;
Step 2) in mediation basic fuel oil, add ethylene-vinyl acetate copolymer, composite antioxidant, ferrocene successively, 25 ~ 35 DEG C, constant temperature stirs 20 minutes, obtains micro emulsion diesel fuel.
Above-mentioned steps 1) in compound emulsifying agent be made up of following steps:
A) oleic acid and ammoniacal liquor generate ammonium oleate after 10 ~ 30 DEG C of mixing and stirring react 30 minutes;
B) 60 ~ 70 DEG C, in the ammonium oleate prepared, add propyl carbinol, stir mixing in 15 minutes, stirring velocity is 300 ~ 400r/min;
C) in the solution of step b), add OP-10, stir mixing in 15 minutes, stirring velocity is 300 ~ 400r/min;
D) in the solution after step c), add trolamine, stir mixing in 15 minutes, stirring velocity is 300 ~ 400r/min, obtains compound emulsifying agent.
The present invention utilizes oleic acid, ammoniacal liquor, propyl carbinol, OP-10 and trolamine according to certain ratio, be mixed with compound emulsifying agent, compound is become to help emulsion with methyl alcohol according to the proportions of 4:1 with propyl carbinol, thus make a kind of outward appearance clear, viscosity is high, stability good, price is lower relative to 0# diesel oil micro emulsion diesel fuel, its ash content is low, sulphur content is low, condensation point is low, cold filter clogging temperature is low and density is little, meets " derv fuel oil " to the requirement of 0# diesel fuel characteristics index.Meanwhile, preparation method of the present invention is simple, and environmental pollution is little.
Embodiment
Now in conjunction with specific embodiments micro emulsion diesel fuel of the present invention is further described, but the present invention is not limited only to following embodiment.
Embodiment 1
To generate micro emulsion diesel fuel composition raw materials used mediation basic fuel oil 100kg, other raw materials and quality proportioning as follows:
The oily 100kg of the basic fuel that is in harmonious proportion
Ethylene-vinyl acetate copolymer 0.08kg
Composite antioxidant 0.08kg
Ferrocene 0.13kg
Wherein, in ethylene-vinyl acetate copolymer, the content of vinyl acetate is 35%(quality).
The mediation basic fuel oil of above-mentioned 100kg is made up of the raw material of following proportion by weight:
0# diesel oil 84kg
Compound emulsifying agent 6kg
Tap water 9kg
Compound helps emulsion 1kg
The compound emulsifying agent of above-mentioned 6kg is made up of the raw material of following proportion by weight:
The compound of above-mentioned 1kg helps emulsion to be made up of the raw material of following proportion by weight:
Propyl carbinol 0.83kg, namely 83 parts
Methyl alcohol 0.17kg, namely 17 parts
Above-mentioned composite antioxidant is that 2, the 6-di-t-butyl-2-methylamino p-cresol of 0.016kg and 2, the 6-di-tert-butylphenols of 0.064kg mix and form, and the mass ratio of 2,6-di-t-butyl-2-methylamino p-cresol and 2,6-di-tert-butylphenol is 1:4.
Above-mentioned oleic acid acid number is 196mgKOH/g; NH in ammoniacal liquor
3content be 26%.
Above-mentioned micro emulsion diesel fuel is specifically prepared by following performing step:
Step 1:30 DEG C, first mixes the 0# diesel oil of above-mentioned quality proportioning and compound emulsifying agent, and churning time is 8 minutes, stirring velocity is 400r/min, adds water and stirs and mix for 8 minutes, add compound and help emulsion, stir mixing in 8 minutes, make mediation basic fuel oil;
Wherein, compound emulsifying agent is specifically made up of following steps:
A) according to above-mentioned quality proportioning, oleic acid and ammoniacal liquor are generated ammonium oleate after 20 DEG C of mixing and stirring react 30 minutes;
B) 65 DEG C, in the ammonium oleate prepared, add propyl carbinol, stir mixing in 15 minutes, stirring velocity is 350r/min;
C) in the solution of step b), add OP-10 again, stir mixing in 15 minutes, stirring velocity is 350r/min;
D) in the solution after step c), add trolamine, stir mixing in 15 minutes, stirring velocity is 350r/min, obtains compound emulsifying agent.
The compound method that above-mentioned compound helps emulsion concrete is: 20 DEG C, according to above-mentioned raw materials proportion by weight by propyl carbinol and methanol mixed evenly.
Step 2: add ethylene-vinyl acetate copolymer, composite antioxidant, ferrocene successively in mediation basic fuel oil, 30 DEG C of constant temperature stir 20 minutes, obtain micro emulsion diesel fuel.
Embodiment 2
To generate micro emulsion diesel fuel composition raw materials used mediation basic fuel oil 100kg, other raw materials and quality proportioning as follows:
The oily 100kg of the basic fuel that is in harmonious proportion
Ethylene-vinyl acetate copolymer 0.08kg
Composite antioxidant 0.10kg
Ferrocene 0.14kg
Wherein, containing vinyl acetate amount in ethylene-vinyl acetate copolymer is 35%(quality).
Above-mentioned mediation basic fuel oil is made up of the raw material of following proportion by weight:
0# diesel oil 82.5kg, namely 86 parts
Compound emulsifying agent 6.7kg, namely 7 parts
Tap water 9.6kg, namely 10 parts
Compound helps emulsion 1.2kg, namely 1.3 parts
The compound emulsifying agent of above-mentioned 6.7kg is made up of the raw material of following proportion by weight:
The compound of above-mentioned 1.3kg helps emulsion to be made up of the raw material of following proportion by weight:
Propyl carbinol 1.1kg, namely 85 parts
Methyl alcohol 0.2kg, namely 15 parts
The composite antioxidant of above-mentioned 0.1kg mixes composition by 2, the 6-di-tert-butylphenols of 2, the 6-di-t-butyl-2-methylamino p-cresol of 0.014kg and 0.086kg.
Above-mentioned oleic acid acid number 203mgKOH/g; NH in ammoniacal liquor
3content 28%.
The preparation method of above-mentioned micro emulsion diesel fuel is identical with the preparation method of embodiment 1.
Embodiment 3
To generate micro emulsion diesel fuel composition raw materials used mediation basic fuel oil 100kg, other raw materials and quality proportioning as follows:
The oily 100kg of the basic fuel that is in harmonious proportion
Ethylene-vinyl acetate copolymer 0.04kg
Composite antioxidant 0.04kg
Ferrocene 0.12kg
Wherein, containing vinyl acetate amount in ethylene-vinyl acetate copolymer is 35%(quality).
Above-mentioned mediation basic fuel oil is made up of the raw material of following proportion by weight:
0# diesel oil 85.59kg, namely 82 parts
Compound emulsifying agent 5.22kg, namely 5 parts
Tap water 8.35kg, namely 8 parts
Compound helps emulsion 0.84kg, namely 0.8 part
The compound emulsifying agent of above-mentioned 5.22kg is made up of the raw material of following proportion by weight:
The compound of above-mentioned 0.8kg helps emulsion to be made up of the raw material of following proportion by weight:
Propyl carbinol 0.64kg, namely 80 parts
Methyl alcohol 0.16kg, namely 20 parts
The composite antioxidant of above-mentioned 0.04kg mixes composition by 2, the 6-di-tert-butylphenols of 2, the 6-di-t-butyl-2-methylamino p-cresol of 0.013kg and 0.027kg.
Above-mentioned oleic acid acid number 190mgKOH/g; NH in ammoniacal liquor
3content 25%.
The preparation method of above-mentioned micro emulsion diesel fuel is identical with the preparation method of embodiment 1.
Embodiment 4
To generate micro emulsion diesel fuel composition raw materials used mediation basic fuel oil 100kg, other raw materials and quality proportioning as follows:
The oily 100kg of the basic fuel that is in harmonious proportion
Ethylene-vinyl acetate copolymer 0.02kg
Composite antioxidant 0.04kg
Ferrocene 0.06kg
Wherein, containing vinyl acetate amount in ethylene-vinyl acetate copolymer is 35%(quality).
Above-mentioned mediation basic fuel oil is made up of the raw material of following proportion by weight:
0# diesel oil 77.97kg, namely 86 parts
Compound emulsifying agent 9.1kg, namely 10 parts
Tap water 11.76kg, namely 13 parts
Compound helps emulsion 1.17kg, namely 1.3 parts
The compound emulsifying agent of above-mentioned 9.1kg is made up of the raw material of following proportion by weight:
The compound of above-mentioned 1.3kg helps emulsion to be made up of the raw material of following proportion by weight:
Propyl carbinol 0.117kg, namely 90 parts
Methyl alcohol 0.013kg, namely 10 parts
Above-mentioned 0.04kg composite antioxidant is 2, the 6-di-tert-butylphenols of 0.0356kg and 2, the 6-di-t-butyl-2-methylamino p-cresol mixing compositions of 0.0044kg.
Above-mentioned oleic acid acid number 196mgKOH/g; NH in ammoniacal liquor
3content 26%.
The preparation method of above-mentioned micro emulsion diesel fuel is identical with the preparation method of embodiment 1.
Embodiment 5
To generate micro emulsion diesel fuel composition raw materials used mediation basic fuel oil 100kg, other raw materials and quality proportioning as follows:
The oily 100kg of the basic fuel that is in harmonious proportion
Ethylene-vinyl acetate copolymer 0.12kg
Composite antioxidant 0.12kg
Ferrocene 0.16kg
Wherein, containing vinyl acetate amount in ethylene-vinyl acetate copolymer is 35%(quality).
Above-mentioned mediation basic fuel oil is made up of the raw material of following proportion by weight:
0# diesel oil 84.63kg, namely 76 parts
Compound emulsifying agent 5.57kg, namely 5 parts
Tap water 8.9kg, namely 8 parts
Compound helps emulsion 0.89kg, namely 0.8 part
The compound emulsifying agent of above-mentioned 5.57kg is made up of the raw material of following proportion by weight:
The compound of above-mentioned 0.89kg helps emulsion to be made up of the raw material of following proportion by weight:
Propyl carbinol 0.712kg, namely 80 parts
Methyl alcohol 0.178kg, namely 20 parts
Above-mentioned 0.12kg composite antioxidant mixes composition by 2, the 6-di-tert-butylphenols of 2, the 6-di-t-butyl-2-methylamino p-cresol of 0.024kg and 0.096kg.
Above-mentioned oleic acid acid number is 196mgKOH/g; NH in ammoniacal liquor
3content be 26%.
The preparation method of above-mentioned micro emulsion diesel fuel is identical with the preparation method of embodiment 1.
Embodiment 6
In the step 1 of above-described embodiment 1 ~ 5, at 25 DEG C, according to corresponding proportioning, first 0# diesel oil and compound emulsifying agent are mixed, churning time is 10 minutes, and stirring velocity is 300r/min, adds water and stirs and mix for 10 minutes, add compound and help emulsion;
Above-mentioned compound emulsifying agent is prepared by following steps:
A) oleic acid and ammoniacal liquor generate ammonium oleate after 10 DEG C of mixing and stirring react 30 minutes;
B) 60 DEG C, in the ammonium oleate prepared, add propyl carbinol, stir mixing in 15 minutes, stirring velocity is 400r/min;
C) in the solution of step b), add OP-10 again, stir mixing in 15 minutes, stirring velocity is 400r/min;
D) in the solution after step c), add trolamine, stir mixing in 15 minutes, stirring velocity is 400r/min, obtains compound emulsifying agent.
In step 1, other step is identical with corresponding embodiment.
In step 2, in mediation basic fuel oil, add ethylene-vinyl acetate copolymer, composite antioxidant, ferrocene successively, 25 DEG C, constant temperature stirs 20 minutes, obtains micro emulsion diesel fuel.
Embodiment 7
In the step 1 of above-described embodiment 1 ~ 5, at 35 DEG C, according to corresponding proportioning, first 0# diesel oil and compound emulsifying agent are mixed, churning time is 5 minutes, and stirring velocity is 500r/min, adds water and stirs and mix for 5 minutes, add compound and help emulsion;
Above-mentioned compound emulsifying agent is prepared by following steps:
A) oleic acid and ammoniacal liquor generate ammonium oleate after 30 DEG C of mixing and stirring react 30 minutes;
B) 70 DEG C, in the ammonium oleate prepared, add propyl carbinol, stir mixing in 15 minutes, stirring velocity is 300r/min;
C) in the solution of step b), add OP-10 again, stir mixing in 15 minutes, stirring velocity is 300r/min;
D) in the solution after step c), add trolamine, stir mixing in 15 minutes, stirring velocity is 300r/min, obtains compound emulsifying agent.
In step 1, other step is identical with corresponding embodiment.
In step 2, in mediation basic fuel oil, add ethylene-vinyl acetate copolymer, composite antioxidant, ferrocene successively, 35 DEG C, constant temperature stirs 20 minutes, obtains micro emulsion diesel fuel.
In order to determine optimum proportioning of the present invention, inventors performed a large amount of laboratory study tests, various test situation is as follows:
1, compound emulsifying agent optimum proportioning test
Contriver is by the proportioning of each reagent the best in even test method determination compound emulsifying agent.The compound emulsifying agent preparation technology adopted is the first hybrid reaction in 10 ~ 30 DEG C of temperature ranges by oleic acid and ammoniacal liquor, propyl carbinol, trolamine, OP-10 is added successively again after fully reacting and terminating, under constant temperature 50 DEG C of conditions, fully mixing is reacted, and adopts manual stir about to cool after 20 minutes and obtains compound emulsifying agent.Micro emulsion diesel fuel preparation technology initial setting is first by the diesel oil mix and blend of the compound emulsifying agent of 7 parts and 83 parts after 5 minutes at 30 DEG C, then the water adding 10 parts stirs 10 minutes, and stirring velocity is 500r/min, adopts oar propeller blade agitator to stir.The determination of each level of factor of even test, testing program and test-results are in table 1 and table 2.
Table 1 compound emulsifying agent formula test level of factor table
Table 2 compound emulsifying agent formula test result
His-and-hers watches 2 test-results adopts intiutive analysis method, and optimum proportion scheme is A-8, and being converted according to centesimal system by the 8th each reagent numerical value of test rounds as oleic acid 73 parts, ammoniacal liquor 13 parts, propyl carbinol 12 parts, trolamine 1 part, OP-101 part.
2, compound emulsifying agent preparation technology test
By even test method determination compound emulsifying agent preparation technology.Compound emulsifying agent formula rate is: oleic acid 73 parts, ammoniacal liquor 13 parts, propyl carbinol 12 parts, trolamine 1 part, OP-10 1 part.Micro emulsion diesel fuel preparation technology is first by the diesel oil mix and blend of the compound emulsifying agent of 7 parts and 83 parts after 5 minutes at 30 DEG C, then the water adding 10 parts stirs 10 minutes, and stirring velocity is 500r/min, adopts oar propeller blade agitator to stir.Contriver is with temperature (X
1), reagent order of addition (X
2), each stage churning time (X
3) and stirring velocity (X
4) be the examination factor, select and mix design table U
12(12 × 6
2× 4) test, the determination of each level of factor of even test, even test scheme and test-results are in table 3 and table 4.
Table 3 compound emulsifying agent preparation technology experimental factor water-glass
Table 4 even test scheme and test-results
The numerology that in table 4, each is tested corresponding to each factor contrasted with numeral in table 3, test-results adopts intiutive analysis method to analyze, preferred plan is B-7, temperature is 60 DEG C, stirring velocity reaches 300r/min, churning time each stage reaches 15 minutes, and reagent order of addition is ammonium oleate-propyl carbinol-OP-10-trolamine.
3, determine that compound helps the optimum proportioning of emulsion
Determine that compound helps optimum proportioning between emulsion propyl carbinol and methyl alcohol.Compound emulsifying agent formula rate is: oleic acid 73 parts, ammoniacal liquor 13 parts, propyl carbinol 12 parts, trolamine 1 part, OP-10 1 part.Micro emulsion diesel fuel preparation technology is first by the diesel oil mix and blend of the compound emulsifying agent of 7 parts and 82 parts after 5 minutes at 30 DEG C, the water adding 10 parts again stirs 5 minutes, finally adding 1 part of compound helps emulsion to stir 5 minutes, and stirring velocity is 500r/min, adopts oar propeller blade agitator to stir.Testing program and test-results are in table 5.
Table 5 propyl carbinol and methyl alcohol proportioning test
From table 5, when propyl carbinol and methanol ratio are 8:2, micro emulsion diesel fuel stablizes number of days great lifting, and in the preferred compound emulsifying agent of the present invention, propyl carbinol and methanol quality are than being 4:1.
4, micro emulsion diesel fuel preparation technology is determined
In determination micro emulsion diesel fuel preparation technology of the present invention, contriver for the examination factor, adopts orthogonal test L with temperature, stirring velocity, reagent order of addition, churning time, alr mode
18(3
7) test, the determination of each level of factor of orthogonal test, orthogonal test scheme and test-results are in table 6 and table 7.
Table 6 preparation technology is because of prime number and number of levels
Table 7 test-results and intuitive analysis thereof
From table 7 intuitive analysis, temperature is within the scope of 25 ~ 35 DEG C; Reagent order of addition first diesel oil and compound emulsifying agent is mixed, then add water slowly and stir, and finally adds compound and help emulsion; Stirring velocity remains within the scope of 300 ~ 500r/min, and each stage churning time is 5 ~ 10 minutes.Optimum optimization scheme is temperature 30 DEG C; Reagent order of addition first diesel oil and compound emulsifying agent is mixed, then add water slowly and stir, and finally adds compound and help emulsion; Stirring velocity 400r/min; Each stage stirs 8 minutes; Stir and adopt high-speed shearing machine.
5, the proportioning of basic fuel oil is determined
By 0
#diesel oil, compound emulsifying agent, water, compound help emulsion to mix by the mass ratio of following five kinds of schemes:
Scheme 1:0
#diesel oil, compound emulsifying agent, water and compound help the mass ratio of emulsion to be 86:5:8:1
Scheme 2:0
#diesel oil, compound emulsifying agent, water and compound help the mass ratio of emulsion to be 82:7:10:1
Scheme 3:0
#diesel oil, compound emulsifying agent, water and compound help the mass ratio of emulsion to be 76:10:13:1
Scheme 4:0
#diesel oil, compound emulsifying agent, water and compound help the mass ratio of emulsion to be 71:12:16:1
Scheme 5:0
#diesel oil, compound emulsifying agent, water and compound help the mass ratio of emulsion to be 64:15:20:1
0
#diesel oil, compound emulsifying agent, water and compound help emulsion first diesel oil and compound emulsifying agent to be mixed under 25 DEG C of constant temperature, then add water slowly and stir, and finally add compound and help emulsion; Stirring velocity 300r/min; Each stage stirs 5 minutes; Stir and adopt high-speed shearing machine to obtain being in harmonious proportion base oil.The mediation base oil obtained measures 20 DEG C of kinematic viscosities according to GB265-88 " petroleum products kinematic viscosity assay method and coefficient of dynamic viscosity computing method ", GB/T1884 " crude oil and liquid petroleum product density experiment room assay method (densimeter method) " measures 20 DEG C of lower densities, GB/T386 " diesel oil catch fire character assay method " measures cetane value, SH/T0248 " distillate fuel cold filter clogging temperature assay method " measures cold filter clogging temperature, and test-results is in table 8.
The test-results of table 8 different mass proportioning mediation basic fuel oil
From table 8, the oily scheme 1 of the basic fuel that is in harmonious proportion and scheme 2 consist of 0
#when diesel oil 82 ~ 86 parts, compound emulsifying agent 5 ~ 7 parts, 8 ~ 10 parts, water, compound help emulsion 1 part, meet GB/T19147-2003 " derv fuel oil " to 0
#the requirement of diesel oil kinematic viscosity, density and cetane value.
6, the add-on of single additive is determined
By 0
#diesel oil, compound emulsifying agent, water and compound help the mass ratio of emulsion to be that 82:7:10:1 mixes, and first diesel oil and compound emulsifying agent are mixed under 25 DEG C of constant temperature, then add water slowly and stir, and finally add compound and help emulsion; Stirring velocity 300r/min; Each stage stirs 5 minutes; Stir and adopt high-speed shearing machine to obtain being in harmonious proportion base oil.
(1) add-on of pour point depressant is determined
Get mediation basic fuel oil totally 6 parts, what add 0.02%, 0.04%, 0.06%, 0.08%, 0.10%, 0.12% of mediation basic fuel oil quality respectively is that the ethylene-vinyl acetate copolymer (T1804) of 35% is as pour point depressant containing vinyl acetate amount, measure condensation point according to GB/T 510 " petroleum products questionable points assay method ", SH/T0248 " distillate fuel cold filter clogging temperature assay method " measures cold filter clogging temperature, test-results is in table 9.
Table 9 T1804 add-on is on the impact of condensation point and cold filter clogging temperature
| T1804 add-on/% | 0.02 | 0.04 | 0.06 | 0.08 | 0.10 | 0.12 |
| Condensation point (DEG C) | -3 | -5 | -6 | -8 | -10 | -10 |
| Cold filter clogging temperature (DEG C) | 2 | 1 | -2 | -2 | -3 | -3 |
From table 9, along with being in harmonious proportion the increase of T1804 addition in basic fuel oil, condensation point and cold filter clogging temperature first reduce and remain unchanged afterwards, when addition is 0.04 ~ 0.10% condensation point and cold filter clogging temperature lowering speed very fast.It is the addition of the ethylene-vinyl acetate copolymer of 35% is be in harmonious proportion 0.04 ~ 0.10% of basic fuel oil quality that the present invention selects containing vinyl acetate amount, preferably 0.06 ~ 0.08%.
(2) amount of falling into of oxidation inhibitor is determined
1) mediation basic fuel oil totally 5 parts is got, add 2 of 0.04%, 0.06%, 0.08%, 0.10%, 0.12% of mediation basic fuel oil quality respectively, 6-di-tert-butylphenol (T502) is as oxidation inhibitor, keep the stable number of days of clear state as measurement index using micro emulsion diesel fuel outward appearance, test-results is in table 10.
Table 10 T502 add-on is on the impact of stable number of days
| T502 adds % | 0.04 | 0.06 | 0.08 | 0.10 | 0.12 |
| Stablize number of days/sky | 178 | 189 | 195 | 210 | 190 |
From table 10, along with the increase of T502 addition in mediation basic fuel oil, stable number of days first increases rear reduction, stablizes number of days and gather way comparatively fast when addition is 0.04 ~ 0.10%.The present invention selects the addition of 2,6-di-tert-butylphenol to be in harmonious proportion 0.04 ~ 0.10% of basic fuel oil quality, and preferably 0.08 ~ 0.10%.
2) mediation basic fuel oil totally 5 parts is got, add 2 of 0.02%, 0.04%, 0.06%, 0.08%, 0.10% of mediation basic fuel oil quality respectively, 6-di-t-butyl-2-methylamino p-cresol (T521) is as oxidation inhibitor, keep the stable number of days of clear state as measurement index using micro emulsion diesel fuel outward appearance, test-results is in table 11.
Table 11 T521 add-on is on the impact of stable number of days
| T521 adds % | 0.02 | 0.04 | 0.06 | 0.08 | 0.10 |
| Stablize number of days/sky | 190 | 202 | 198 | 170 | 165 |
From table 11, along with the increase of T521 addition in mediation basic fuel oil, stable number of days first increases rear reduction, stablizes number of days and gather way comparatively fast when addition is 0.02 ~ 0.04%.The present invention selects the addition of 2,6-di-t-butyl-2-methylamino p-cresol to be in harmonious proportion 0.02 ~ 0.06% of basic fuel oil quality, and preferably 0.02 ~ 0.04%.
3) 2,6-di-tert-butylphenol (T502) and 2,6-di-t-butyl-2-methylamino p-cresol (T521) optimum proportioning and addition is determined.Adopt even test method U
9 *(9
4) determine composite antioxidant proportioning and addition, with T502:T521 ratio and addition for the examination factor, keep the stable number of days of clear state as measurement index using micro emulsion diesel fuel outward appearance, the determination of each level of factor of even test and test-results are in table 12 ~ 13.
The composite experimental factor number of table 12 oxidation inhibitor and number of levels
The composite testing program of table 13 oxidation inhibitor and test-results
| Test number | T502:T521 | Oxidation inhibitor use % | Stablize number of days/sky |
| D-1 | 1（9:1） | 7（0.10） | 298 |
| D-2 | 2（8:2） | 4（0.07） | 325 |
| D-3 | 3（7:3） | 1（0.04） | 302 |
| D-4 | 4（6:4） | 8（0.11） | 273 |
| D-5 | 5（5:5） | 5（0.08） | 260 |
| D-6 | 6（4:6） | 2（0.05） | 249 |
| D-7 | 7（3:7） | 9（0.12） | 242 |
| D-8 | 8（2:8） | 6（0.09） | 237 |
| D-9 | 9（1:9） | 3（0.06） | 230 |
As can be seen from table 13 test-results, preferred plan is D-2, and namely T502:T521 mass ratio is 8:2, and addition is be in harmonious proportion 0.07% of basic fuel oil quality, be in harmonious proportion micro emulsion diesel fuel and stablize number of days and reach 325 days.It is the mixture of 4:1 with 2,6-di-t-butyl-2-methylamino p-cresol (T521) mass ratioes that the present invention selects compound emulsifying agent to be 2,6-di-tert-butylphenol (T502), and preferred addition is be in harmonious proportion 0.08% of basic fuel oil quality.
(3) addition of ignition dope is determined
Get mediation basic fuel oil totally 7 parts, add the ferrocene of 0.04%, 0.06%, 0.08%, 0.10%, 0.12%, 0.14%, 0.16% of mediation basic fuel oil quality respectively as ignition dope, using micro emulsion diesel fuel rate of economizing gasoline as measurement index, test-results is in table 14.
Table 14 T502 add-on is on the impact of stable number of days
| Ferrocene add-on/% | 0.04 | 0.06 | 0.08 | 0.10 | 0.12 | 0.14 | 0.16 |
| Rate of economizing gasoline/% | 2.1 | 2.3 | 2.5 | 2.6 | 2.7 | 3.0 | 3.0 |
From table 14, along with the increase of ferrocene addition in mediation basic fuel oil, fuel-economizing takes the lead in remaining unchanged after increase, and when addition is 0.10 ~ 0.14%, rate of economizing gasoline is larger.The present invention selects ferrocene addition to be in harmonious proportion 0.10 ~ 0.14% of basic fuel oil quality, and preferably 0.12 ~ 0.14%.
7, full formula test
Contriver is with the ethylene-vinyl acetate copolymer (T1804), the composite antioxidant [2 that containing vinyl acetate amount are 35%, 6-di-tert-butylphenol (T502) and 2,6-di-t-butyl-2-methylamino p-cresol (T521) mass ratio is 4:1], ferrocene for examination the factor, adopt L
9(3
4) gauge outfit design orthogonal test, the determination of each level of factor of orthogonal test, orthogonal experiments and intuitive analysis are in table 15 ~ 17.
Table 15 full formula experimental factor and water-glass
Table 16 full formula testing program and test-results
Table 17 full formula test result analysis
As shown in Table 17, show that excellent scheme is A from cold filter clogging temperature interpretation of result
3c
2b
1, stablize number of days interpretation of result and show that excellent scheme is B
3c
2a
1, comprehensive analysis show that the prioritization scheme that full formula test is best is A
3b
3c
2namely be ethylene-vinyl acetate copolymer (T1804), the composite antioxidant [2 of 35% containing vinyl acetate amount, the optimum addition that 6-di-tert-butylphenol (T502) and 2,6-di-t-butyl-2-methylamino p-cresol (T521) mass ratioes are 4:1, ferrocene adds is followed successively by and is in harmonious proportion 0.08%, 0.08%, 0.13% of basic fuel oil quality.
In order to prove beneficial effect of the present invention, the various performances of contriver to novel microemulsion Dresel fuel compositions prepared by the embodiment of the present invention 1 are tested, and concrete test situation is as follows:
Testing method: measure flash-point according to GB/T261 " Flash Point for Petroleum Products assay method (agar diffusion method of remaining silent) ", GB/T265 " petroleum products kinematic viscosity assay method and kinetic viscosity computing method " measures 20 DEG C of kinematic viscosities, GB/T268 " petroleum products Conradson method " measures 10% steaming excess carbon residue, GB/T380 " petroleum products sulphur content determination method (Ignition Lamp Method) " measures sulphur content, GB/T386 " diesel oil catch fire character assay method (cetane value method) " measures cetane value, GB/T508 " petroleum products Ash determination method " measures ash content, GB/T510 " petroleum products questionable points assay method " measures condensation point, GB/T511 " petroleum products and additive mechanical impurity assay method (weighting method) " measures mechanical impurity, GB/T1884 " crude oil and liquid petroleum product density experiment room assay method (densimeter method) " measures 20 DEG C of lower densities, GB/T5096 " petroleum products copper strip test method " measures copper strip test, GB/T6536 " measured for petroleum product distillation method " measures 50%, 90%, 95% recovered temperature, SH/T0248 " distillate fuel cold filter clogging temperature assay method " measures cold filter clogging temperature.Micro emulsion diesel fuel antioxidant property is preserved with its sealing the number of days leaving standstill outward appearance maintenance clear state and is weighed.Test-results is shown in 18.
Table 18 embodiment of the present invention 1 micro emulsion diesel fuel testing performance index result
From table 18, novel microemulsion Dresel fuel compositions performance index prepared by the embodiment of the present invention 1 all meet in GB/T 19147-2003 " derv fuel oil " 0
#the requirement of diesel fuel characteristics index, can be used as the micro emulsion diesel fuel that diesel car uses.
Claims (4)
1. a micro emulsion diesel fuel, is characterized in that being made up of the raw material of following proportion by weight:
Above-mentioned mediation basic fuel oil is made up of the raw material of following proportion by weight:
Above-mentioned compound emulsifying agent is made up of the raw material of following proportion by weight:
Above-mentioned compound helps emulsion to be made up of the raw material of following proportion by weight:
Propyl carbinol 80 ~ 90 parts
Methyl alcohol 10 ~ 20 parts
Above-mentioned composite antioxidant is that 2,6-di-t-butyl-2-methylamino p-cresol of 1:2 ~ 8 and 2,6-di-tert-butylphenol form by mass ratio;
Above-mentioned oleic acid acid number is 190 ~ 203mgKOH/g; Containing NH in ammoniacal liquor
3amount is 25% ~ 28% (quality);
In above-mentioned ethylene-vinyl acetate copolymer, vinyl acetate content is 35% (quality).
2. micro emulsion diesel fuel according to claim 1, is characterized in that being made up of the raw material of following proportion by weight:
Above-mentioned mediation basic fuel oil is made up of the raw material of following proportion by weight:
Above-mentioned compound emulsifying agent is made up of the raw material of following proportion by weight:
Above-mentioned compound helps emulsion to be made up of the raw material of following proportion by weight:
Propyl carbinol 80 ~ 85 parts
Methyl alcohol 15 ~ 20 parts
Above-mentioned composite antioxidant is that 2,6-di-t-butyl-2-methylamino p-cresol of 1:2 ~ 6 and 2,6-di-tert-butylphenol form by mass ratio.
3. a preparation method for micro emulsion diesel fuel according to claim 1, comprises following performing step:
Step 1) 25 ~ 35 DEG C, according to corresponding proportioning, first 0# diesel oil and compound emulsifying agent are mixed, churning time is 5 ~ 10 minutes, stirring velocity is 300 ~ 500r/min, adds water stirring and mixes for 5 ~ 10 minutes, add compound and help emulsion, stirring and evenly mixing, makes mediation basic fuel oil;
Step 2) in mediation basic fuel oil, add ethylene-vinyl acetate copolymer, composite antioxidant, ferrocene successively, 25 ~ 35 DEG C, constant temperature stirs 20 minutes, obtains micro emulsion diesel fuel.
4. the preparation method of micro emulsion diesel fuel according to claim 3, is characterized in that: step 1) in compound emulsifying agent be made up of following steps:
A) oleic acid and ammoniacal liquor generate ammonium oleate after 10 ~ 30 DEG C of mixing and stirring react 30 minutes;
B) 60 ~ 70 DEG C, in the ammonium oleate prepared, add propyl carbinol, stir mixing in 15 minutes, stirring velocity is 300 ~ 400r/min;
C) to step b) solution in add OP-10, stir mixing in 15 minutes, stirring velocity is 300 ~ 400r/min;
D) to step c) after solution in add trolamine, stir mixing in 15 minutes, stirring velocity is 300 ~ 400r/min, obtains compound emulsifying agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210590857.4A CN103013591B (en) | 2012-12-28 | 2012-12-28 | Microemulsified diesel and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210590857.4A CN103013591B (en) | 2012-12-28 | 2012-12-28 | Microemulsified diesel and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103013591A CN103013591A (en) | 2013-04-03 |
| CN103013591B true CN103013591B (en) | 2015-07-08 |
Family
ID=47962713
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210590857.4A Expired - Fee Related CN103013591B (en) | 2012-12-28 | 2012-12-28 | Microemulsified diesel and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103013591B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104232189A (en) * | 2014-06-03 | 2014-12-24 | 长春工业大学 | Preparation method of microemulsified diesel |
| CN105273784A (en) * | 2014-07-24 | 2016-01-27 | 北京南亚节能技术研究院 | High-energy microemulsion gasoline |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101538490A (en) * | 2009-04-30 | 2009-09-23 | 合肥工业大学 | Micro-emulsified biomass fuel and preparation method thereof |
| CN101838566A (en) * | 2009-03-16 | 2010-09-22 | 郁光耀 | Oil-water copolymerization synthesized environment-friendly and energy-saving diesel |
| CN102250656A (en) * | 2011-06-21 | 2011-11-23 | 李立芬 | Method for preparing micro-emulsified procetane |
-
2012
- 2012-12-28 CN CN201210590857.4A patent/CN103013591B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838566A (en) * | 2009-03-16 | 2010-09-22 | 郁光耀 | Oil-water copolymerization synthesized environment-friendly and energy-saving diesel |
| CN101538490A (en) * | 2009-04-30 | 2009-09-23 | 合肥工业大学 | Micro-emulsified biomass fuel and preparation method thereof |
| CN102250656A (en) * | 2011-06-21 | 2011-11-23 | 李立芬 | Method for preparing micro-emulsified procetane |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103013591A (en) | 2013-04-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101906329B (en) | Methanol gasoline for vehicles and preparation method thereof | |
| CN101519610B (en) | Methanol gasoline additive and preparation method thereof and methanol gasoline | |
| CN102517101B (en) | Automobile methanol diesel fuel and preparation method thereof | |
| CN102660337A (en) | Method for preparing novel clean synthetic diesel oil | |
| CN102585941A (en) | Microemulsification diesel fuel and preparation method thereof | |
| CN101914393B (en) | Methanol gasoline for vehicles and preparation method thereof | |
| CN103013591B (en) | Microemulsified diesel and preparation method thereof | |
| CN100469859C (en) | Ethanol modifier and application thereof | |
| CN109504360A (en) | A kind of heavy crude thinner and its preparation method and application | |
| CN104673408A (en) | Alcohol hydrocarbon fuel and preparation method thereof | |
| CN103254952A (en) | Preparation method of water-based micro-emulsion diesel oil | |
| CN100569929C (en) | Automobile-used environmental protection, low emission, coal-based alcohol ether gasoline and preparation method thereof | |
| CN101967411A (en) | Microemulsified watered diesel, additive used thereby and preparation process thereof | |
| CN102127477B (en) | Petrochemical additive and preparation method thereof | |
| CN104818057A (en) | Automobile alcohol-based diesel oil composite resin type emulsifier, preparation method and auxiliary agent with application of emulsifier | |
| CN107312579A (en) | A kind of energy-efficient fuel oil additive for improving power and preparation method thereof | |
| CN106701050B (en) | A kind of heavy crude thinner, preparation method and application | |
| CN110330261A (en) | A kind of fretting map asphalt warm-mix agent, Warm-Mix Bitumen Mixture and preparation method | |
| CN110257110A (en) | It is a kind of based on dimethyl ether be raw material vehicle fuel | |
| CN102061199A (en) | Clean diesel oil | |
| CN103087785B (en) | Clean fuel for vehicles and preparation method thereof | |
| CN100357406C (en) | Synthetic vehicular fuel and its preparation method | |
| CN105001998A (en) | Method for lowering condensation point of biodiesel | |
| CN205627909U (en) | Continuous ageing device of catalyst | |
| CN100410353C (en) | Ethanol diesel oil mixing fuel |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150708 Termination date: 20151228 |
|
| EXPY | Termination of patent right or utility model |