CN107057782A - A kind of trinitride for making fuel qualities and effect upgrade and safety and environmental protection synthetic method - Google Patents
A kind of trinitride for making fuel qualities and effect upgrade and safety and environmental protection synthetic method Download PDFInfo
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- CN107057782A CN107057782A CN201710151694.2A CN201710151694A CN107057782A CN 107057782 A CN107057782 A CN 107057782A CN 201710151694 A CN201710151694 A CN 201710151694A CN 107057782 A CN107057782 A CN 107057782A
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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
-
- 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
- C10L1/1216—Inorganic compounds metal compounds, e.g. hydrides, carbides
-
- 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
- C10L1/20—Organic compounds containing halogen
- C10L1/206—Organic compounds containing halogen macromolecular compounds
- C10L1/208—Organic compounds containing halogen macromolecular compounds containing halogen, oxygen, with or without hydrogen
-
- 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
- C10L10/00—Use of additives to fuels or fires for particular purposes
- C10L10/08—Use of additives to fuels or fires for particular purposes for improving lubricity; for reducing wear
-
- 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
- C10L10/00—Use of additives to fuels or fires for particular purposes
- C10L10/18—Use of additives to fuels or fires for particular purposes use of detergents or dispersants for purposes not provided for in groups C10L10/02 - C10L10/16
-
- 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
- C10L2230/00—Function and purpose of a components of a fuel or the composition as a whole
- C10L2230/04—Catalyst added to fuel stream to improve a reaction
-
- 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
- C10L2230/00—Function and purpose of a components of a fuel or the composition as a whole
- C10L2230/22—Function and purpose of a components of a fuel or the composition as a whole for improving fuel economy or fuel efficiency
-
- 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
- C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
- C10L2290/12—Regeneration of a solvent, catalyst, adsorbent or any other component used to treat or prepare a fuel
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- Chemical & Material Sciences (AREA)
- 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 present invention relates to a kind of trinitride for making fuel qualities and effect upgrade, the trinitride refers to that, by saturated alkyl alcohol or phenol, epoxychloropropane, sodium azide is the principal product that raw material is obtained, and a small amount of accessory substance and includes the mixture including nitrine catalyst；Wherein：(1) principal product：Glycidyl azide polymer, abbreviation GAP；(2) accessory substance：The chloride isomers of glycidyl azide polymer, abbreviation GAP CL；(3) nitrine catalyst：Second step reacts the homemade Azide catalyst of synthesis；(4) intermediate：Hydrin, abbreviation PECH is the intermediate product of trinitride synthesis, is not the part of trinitride；Wherein：Aggregate number n=1 8 sodium azide replaces any moL numbers of chloro, and n can not be integer, the alcohol or phenol of the carbon numbers of saturated alkyl R=2 18.The trinitride of the present invention solves safety and the big problem of environmental protection in synthesis, and production and use cost is greatly reduced.
Description
Technical field
The present invention relates to a kind of trinitride for making fuel qualities and effect upgrade and safety and environmental protection synthetic method, belong to fuel oil
Technical field.
Background technology
Fuel energy-saving emission reduction is to be related to national economy major issue, suddenly new breakthrough to be had.Current glycidyl azide polymer
Synthesis technique cost is high, and safety and environmental protection problem is serious, big as fuel oil additive consumption, stores also not safe steady enough in fuel oil
It is fixed, effect purposes underexploitation etc..
The content of the invention
It is an object of the invention to provide a kind of trinitride for making fuel qualities and effect upgrade and safety and environmental protection synthesis side
Method, preferably to improve fuel oil using effect.
To achieve these goals, technical scheme is as follows.
A kind of trinitride for making fuel qualities and effect upgrade, the trinitride refers to by saturated alkyl alcohol or phenol, epoxy chlorine
Propane, sodium azide is the obtained principal product of raw material, a small amount of accessory substance and includes the mixture including nitrine catalyst；Its
In：(1) principal product：Glycidyl azide polymer, abbreviation GAP；(2) accessory substance：The chloride isomers of glycidyl azide polymer,
Abbreviation GAP-CL；(3) nitrine catalyst：Second step reacts the homemade Azide catalyst of synthesis；(4) intermediate：Polycyclic
Oxygen chloropropane, abbreviation PECH is the intermediate product of trinitride synthesis, is not the part of trinitride；Wherein：Aggregate number n=
1-8 sodium azide replaces any moL numbers of chloro, and n can not be integer, the alcohol or phenol of saturated alkyl R=2-18 carbon numbers.
Further, trinitride it is raw materials used/catalyst/solvent is：
(1) trinitride is raw materials used：Saturated alkyl alcohol or phenol ROH, the alkyl that it is all saturated bond in addition to phenyl ring that wherein R, which is,
It is preferred that phenolic group and isomery base；Epoxychloropropane ECH, it is desirable to industrial goods content 99%, preferred content more than 99.5%；Sodium azide
NaN3, it is desirable to industrial goods content more than 99%, or use LiN3/KN3/ tetraalkyl amine azide is raw material.
(2) trinitride used catalyst：Butter of tin SnCl4, it is desirable to select anhydrous stannic chloride；BFEE network
Compound BF3·OEt2, it is desirable to BF3Content is up to 47% or so, and Azide catalyst is the special catalysis of self-control that second step reacts synthesis
Agent.
(3) trinitride solvent for use：120# solvent naphthas require that quality reaches national standard.
Further, saturated alkyl alcohol is ethyl to 18 saturated alkyl alcohol and its different purchase body, including sec-butyl alcohol, uncle penta
Alcohol, cyclohexanol, benzyl carbinol, different tridecanol, i-octadecanol etc.；Saturated alkyl phenol is ethyl to dodecyl phenol and its different purchase
Body, including 2,6- xylenol, 2,4,6- pseudocuminols, 2,4-DTBP, o-sec-butyl phenol, to tertiary pentyl
Phenol, trimerization isobutyl group phenol.
Further, the environmental protection synthetic method and step of this trinitride are as follows：
(1) Hydrin PECH is synthesized：Mechanical agitator, automatic temperature control instrument, nitrogen conduit are installed in cold bath
And three-necked flask, ROH is added, stirring is opened, is slowly introducing drying nitrogen, is then injected into anhydrous SnCl4Or BF3·OEt2, treat temperature
When degree is down to less than 30 DEG C, by ECH completion of dropping, 5-50 DEG C of temperature is controlled, 10-40 DEG C of preferable temperature, stirring reaction 2-10 is small
When, preferably react 3-8 hours；After the completion of reaction, 120# solvent naphthas are added by density domination below 0.88,2-3 times point of washing
From impurity, vacuum distillation sloughs 120# solvent naphthas and produces PECH；
(2) trinitride is synthesized：PECH is added in the three-necked flask equipped with mechanical agitator, self-control nitrine is then added
Change catalyst and be sufficiently stirred for dissolving, add NaN3, it is warming up to 70-100 DEG C of stirring 6-10h；After reaction stops, 50 DEG C are cooled to
120# solvent naphthas are added, by density domination in 0.88g/cm3Hereinafter, impurity elimination is centrifuged after being sufficiently stirred for, vacuum distillation takes off 120#
Solvent naphtha obtains colourless or faint yellow trinitride.
The mechanism of action of the trinitride that the present invention is provided in fuel oil and internal combustion engine：
(1) fuel oil efficiency of combustion is improved, generally using the surface tension of reduction fuel oil, the energy of vaporization demand is reduced, changes
Enter fuel-injecting method etc., in practice it has proved that these physics mode effects are limited, more scientific method is to improve fuel oil combustion intensity, is changed
It is apt to hydrocarbon fuel oil combustibility, and fuel oil combustibility is determined by oil droplets rate of gasification, rate of gasification is by oil droplet phase transformation again
It can be determined with heat transfer.
(2) because GAP burn rates are that (GAP is net typically in 15ms combustions, and the fuel oil of identical boiling point same diameter is oily for 6 times of fuel oil
Drop needs 90ms combustions net), in GAP-CL, faster (GAP burn rates can be improved GAP again with burn rate under self-control Azide catalyst collective effect
1-3 times), 180-200 DEG C is first decomposed generation nitrogen and releases substantial amounts of heat energy, oil droplet is gathered gaseous pressure and is caused unexpected eruption
Microexplosion is produced, oil droplet preignition period is obtained required phase-change energy in advance, it is often more important that trinitride changes heat transfer mode：
Detonation propagation energy, substantially reduces the preignition period before burning from inside to outside.
Effect and performance that the trinitride that the present invention is provided is produced in fuel oil and internal combustion engine：
(1) it is preferable combustion-supporting base that the residue after nitrogen is decomposited due to trinitride, is extremely unstable super freedom base,
The group of even more outstanding chemically cleaning combustion chamber, cleaning speed is calculated with millisecond under microexplosion collective effect, is totally different from poly-
The cleaning principle of ether amines class General Physics absorption dissolving, makes cleaning speed is fast to cross carbon deposit speed, it is ensured that combustion chamber is rapidly and efficiently
Cleaning.
(2) because combustion chamber cleaning makes metal covering exposed, catalysis combustion system, efficient heat radiation energy transmission are changed into
Mode proportion increases, and significantly reduces fuel oil combustive activation energy, and combustion and eventually more than 100 DEG C of combustion temperature drop, cooling are opened in combustion chamber
The energy that water and tail gas are taken away is greatly decreased, and useful work relative increase, efficiency of combustion is significantly improved, thus fuel-economizing is more notable.
(3) due to fuel oil burning initial stage (burning 0-40% periods) microexplosion effect, there is provided more energy and high-effect
Circulation way is measured, makes chamber temperature more balanced, combustion and eventually combustion temperature drop is opened, it is ensured that the nitrogen under conditions of excessive oxygen
Burning is not involved in, NOx generations are significantly reduced, microexplosion and combustor surface metal catalytic fragment into liquid oil molecule first moment
Gaseous state small molecule residue (change oil molecule, which need to be vaporized first, only relies on oxygen radical attack chain rupture traditional combustion mode), then be excited together
Oxygen it is rapid, thoroughly, clean burning, significantly reduce CO and CH and exist, emission reduction is advanceed to combustion chamber and synchronously complete, break away from thing
The three-element catalytic reduction mode made up afterwards.
(4) because fuel oil burn rate is accelerated, the increase of unit interval work done is combustion engine powered to be obviously improved.
Purposes and usage of the trinitride in fuel oil and internal combustion engine：The thing is pressed into 20-800ppm amounts and marketable material
200ppm amounts, which are combined in environment friendly fuel agent addition fuel oil, is changed into environment friendly fuel, obtains following purposes：
The beneficial effect of the invention is：Trinitride MOLECULE DESIGN and synthetic method of the present invention have following outstanding advantage：It is folded
Because R selections are suitable in nitrogen thing MOLECULE DESIGN, it is ensured that security and stability (more than 4 years phase of storage) that product accumulating itself is used and
The security and stability that accumulating is used in fuel oil, is substantially shorter the reaction time, and reduction reaction temperature is saved reaction dissolvent, only divided
From middle use 120# solvent naphthas, yield is significantly improved, and significantly reduces production cost, makes azide general with turning into fuel oil
May.Prepared by trinitride is the Azide under PECH excess, and sodium azide almost all has been reacted, and solves environmental protection in synthesis
With the big problem of safety, environmental protection and safety cost are significantly reduced.Contain unfavorable chlorine essence, addition after being burnt in view of GAP-CL
Self-control nitrine catalyst is another object is that with the chloride generated after GAP-CL burnings, can help combustion chamber wear-resistant, cleaning is vented
System, reduces the pollution to environment.Containing GAP-CL and self-control nitrine catalyst in trinitride, Bu Dan No influence products use effect
Really, microexplosion function is enhanced on the contrary, further increases 1-3 times of burn rate, efficiency of combustion increases to 25% in fuel oil.
Embodiment
The embodiment of the present invention is described with reference to embodiment, to be better understood from the present invention.
Embodiment 1
1st, PECH is synthesized：Mechanical agitator, automatic temperature control instrument, nitrogen conduit and three-necked flask are installed in cold bath, plus
Enter 145g nonyl alcohols, open stirring, be slowly introducing drying nitrogen, be then injected into 1gBF3OEt2, treat that temperature is down to less than 30 DEG C
When, by 222gECH40min completion of dropping, control 30-35 DEG C of temperature, stirring reaction 4 hours.After the completion of reaction, 120# is added molten
Density domination below 0.88, is washed 2-3 separation impurity by agent oil, and vacuum distillation sloughs 120# solvent naphthas and produces colourless liquid
PECH332g, by gpc analysis, number-average molecular weight Mn=366
2nd, trinitride is synthesized：332gPECH is added in the three-necked flask equipped with mechanical agitator, 30g is then added certainly
Azide catalyst processed is sufficiently stirred for dissolving, adds 118gNaN3, is warming up to 80 DEG C of stirring 7h.After reaction stops, it is cooled to
50 DEG C add 120# solvent naphthas, by density domination below 0.88, impurity elimination are centrifuged after being sufficiently stirred for, it is molten that vacuum distillation takes off 120#
Agent is oily to obtain flaxen trinitride 373.9g.Self-control Azide catalyst 30g is reduced, GAP+GAP-CL is obtained for 343.9g, passes through
Gpc analysis, number-average molecular weight Mn=379.4, N content=22.2% (it is equal with theoretical value, illustrate nothing in the salt isolated
NaN3), yield ＞ 90%.
3rd, automobile-used ring is obtained after trinitride obtained above is assembled by 20-800ppm consumptions and commercially available raw material 200ppm
Guarantor safeguards gasoline agent, and addition 20-1000ppm enters driving examination into automobile-used regular gasoline, and test vehicle is that Beijing is modern
BH7162MX gasoline cars, travel 600,000 kilometers of scrap cars, manual, Close loop EFI.
4th, automobile-used ring is obtained after trinitride obtained above is assembled by 20-800ppm consumptions and commercially available raw material 200ppm
Synergistic gasoline agent is protected, addition 20-1000ppm enters driving examination into automobile-used regular gasoline, and test vehicle is Audi's A6L1.8B gasoline
Car, travels 22.3 ten thousand kilometers, manual, Close loop EFI.
5th, the oil product physical and chemical mutagenesis for adding the environmentally friendly Synergistic gasoline agent of 20-1000ppm to store up in national standard regular gasoline 6 months
Embodiment 2
1st, PECH is synthesized：Mechanical agitator, automatic temperature control instrument, nitrogen conduit and three-necked flask are installed in cold bath, plus
Enter the different tridecanols of 200g, open stirring, be slowly introducing drying nitrogen, be then injected into the anhydrous SnCl4 of 1.7g, treat that temperature is down to 30 DEG C
When following, by 222gECH40min completion of dropping, 30-35 DEG C of temperature, stirring reaction 5 hours are controlled.After the completion of reaction, add
Density domination below 0.88, is washed 2-3 separation impurity by 120# solvent naphthas, and vacuum distillation sloughs 120# solvent naphthas and produces nothing
Color liquid PECH384g, by gpc analysis, number-average molecular weight Mn=422.
2nd, trinitride is synthesized：384gPECH is added in the three-necked flask equipped with mechanical agitator, 35g is then added certainly
Azide catalyst processed is sufficiently stirred for dissolving, adds 119gNaN3, is warming up to 90 DEG C of stirring 8h.After reaction stops, it is cooled to
50 DEG C add 120# solvent naphthas, by density domination below 0.88, impurity elimination are centrifuged after being sufficiently stirred for, it is molten that vacuum distillation takes off 120#
Agent is oily to obtain flaxen trinitride 425g.35g self-control Azide catalyst is subtracted, GAP+GAP-CL is 390g, by GPC points
Analysis, number-average molecular weight Mn=422, N content=19.7% (equal with theoretical value, to illustrate in the salt isolated without NaN3), yield
＞ 90%.
3rd, automobile-used ring is obtained after trinitride obtained above is assembled by 20-800ppm consumptions and commercially available raw material 200ppm
Guarantor safeguards gasoline agent, and addition 20-1000ppm enters driving examination into gasoline, and test vehicle is Beijing modern times BH7200MX gasoline cars,
Travel 2.6 ten thousand kilometers of new cars, manual, Close loop EFI.
4th, automobile-used ring is obtained after trinitride obtained above is assembled by 20-800ppm consumptions and commercially available raw material 200ppm
Synergistic diesel oil agent is protected, addition 20-1000ppm enters driving examination into diesel oil, and test vehicle is the commercial diesel vehicle of the auspicious wind of Yangze river and Huai river, discharge capacity
2.0cc, travels 30.2 ten thousand kilometers.
5th, the oil product physical and chemical mutagenesis for adding the environmentally friendly Synergistic diesel oil agent of 20-1000ppm to store up in national standard ordinary diesel oil 6 months
Described above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications are also considered as
Protection scope of the present invention.
Claims (4)
1. a kind of trinitride for making fuel qualities and effect upgrade, it is characterised in that：The trinitride refer to by saturated alkyl alcohol or
Phenol, epoxychloropropane, sodium azide is the obtained principal product of raw material, a small amount of accessory substance and comprising nitrine catalyst including
Mixture；Wherein：(1) principal product：Glycidyl azide polymer, abbreviation GAP；(2) accessory substance：Glycidyl azide polymer contains
Chlorine isomers, abbreviation GAP-CL；(3) nitrine catalyst：Second step reacts the homemade Azide catalyst of synthesis；(4) in
Mesosome：Hydrin, abbreviation PECH is the intermediate product of trinitride synthesis, is not the part of trinitride；Wherein：
Aggregate number n=1-8 sodium azide replaces any moL numbers of chloro, and n can not be integer, saturated alkyl R=2-18 carbon numbers
Alcohol or phenol.
2. the trinitride according to claim 1 for making fuel qualities and effect upgrade, it is characterised in that：
(1) trinitride synthesis is raw materials used：Saturated alkyl alcohol or phenol ROH, wherein R are the alkyl of saturated bond in addition to phenyl ring, excellent
Select phenolic group and isomery base；Epoxychloropropane ECH, it is desirable to industrial goods content 99%, preferred content more than 99.5%；Sodium azide
NaN3, it is desirable to industrial goods content more than 99%, or use LiN3/KN3/ tetraalkyl amine azide is raw material；
(2) trinitride synthesis used catalyst：Butter of tin SnCl4, it is desirable to select anhydrous stannic chloride；BFEE network
Compound BF3·OEt2, it is desirable to BF3Content is up to 47% or so, and two doses of the above is the catalyst that the first step reacts synthesis, is individually made
With or be used in combination；Azide catalyst is the self-control special-purpose catalyst that second step reacts synthesis；
(3) trinitride synthesis solvent for use：120# solvent naphthas require that quality reaches national standard.
3. the trinitride according to claim 2 for making fuel qualities and effect upgrade, it is characterised in that：Saturated alkyl alcohol is
The ethyl of saturation is including sec-butyl alcohol, tert-pentyl alcohol, cyclohexanol, benzyl carbinol, different tridecanol, different to stearyl alcohol and its different purchase body
Octadecyl alcolol etc.；Saturated alkyl phenol for saturation ethyl to dodecyl phenol and its different purchase body, including 2,6- xylenol, 2,
4,6- pseudocuminols, 2,4-DTBP, o-sec-butyl phenol, p-tert-amylphenol, trimerization isobutyl group phenol etc..
4. the trinitride according to claim 1 for making fuel qualities and effect upgrade, it is characterised in that：The peace of this trinitride
Full environmental protection synthetic method and step are as follows：
(1) Hydrin PECH is synthesized：Mechanical agitator, automatic temperature control instrument, nitrogen conduit and three are installed in cold bath
Mouth flask, adds ROH, opens stirring, is slowly introducing drying nitrogen, is then injected into anhydrous SnCl4Or BF3·OEt2, treat that temperature drops
During to less than 30 DEG C, by ECH completion of dropping, 5-50 DEG C of temperature is controlled, 10-40 DEG C of preferable temperature, stirring reaction 2-10 hours is excellent
Choosing reaction 3-8 hours；After the completion of reaction, 120# solvent naphthas are added by density domination below 0.88,2-3 separation of washing is miscellaneous
Matter, vacuum distillation sloughs 120# solvent naphthas and produces PECH；
(2) trinitride is synthesized：PECH is added in the three-necked flask equipped with mechanical agitator, self-control Azide is then added and urges
Agent is sufficiently stirred for dissolving, adds NaN3, it is warming up to 70-100 DEG C of stirring 6-10h；After reaction stops, it is cooled to 50 DEG C and adds again
Enter 120# solvent naphthas, by density domination in 0.88g/cm3Hereinafter, impurity elimination is centrifuged after being sufficiently stirred for, vacuum distillation takes off 120# solvents
It is oily to obtain colourless or faint yellow trinitride.
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Cited By (1)
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| CN114520318A (en) * | 2022-01-27 | 2022-05-20 | 北京理工大学 | High-nickel cobalt-free nickel tungsten lithium manganate positive electrode material for power battery and preparation method thereof |
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