CN106281501B - A kind of preparation method of methanol gasoline rubber swelling inhibitor - Google Patents

A kind of preparation method of methanol gasoline rubber swelling inhibitor Download PDF

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CN106281501B
CN106281501B CN201610806942.8A CN201610806942A CN106281501B CN 106281501 B CN106281501 B CN 106281501B CN 201610806942 A CN201610806942 A CN 201610806942A CN 106281501 B CN106281501 B CN 106281501B
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hydroxy benzaldehyde
reaction vessel
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ratio
technical grade
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CN106281501A (en
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顾雪凡
张洁
汤颖
马超
张黎
吴亚
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Xian Shiyou University
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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
    • C10L1/14—Organic compounds
    • C10L1/18—Organic compounds containing oxygen
    • C10L1/1817—Compounds of uncertain formula; reaction products where mixtures of compounds are obtained
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/02—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using non-aqueous solutions

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  • General Chemical & Material Sciences (AREA)
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  • Health & Medical Sciences (AREA)
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Abstract

A kind of preparation method of methanol gasoline rubber swelling inhibitor, it is related under methanol gasoline additive technical field, normal temperature and hydroxy benzaldehyde is dissolved in solvent in reaction vessel, adds fatty amine and alkali under stirring into reaction vessel, 50 140 DEG C are heated to, is reacted 28 hours；Halogenated hydrocarbons is added under stirring into reaction vessel, continues to react 28 hours at 50 140 DEG C, is cooled to room temperature；Mixture in reaction vessel is filtered; alkyl phenol is added into filtrate; stir; obtain methanol gasoline rubber swelling inhibitor; gained methanol gasoline rubber swelling inhibitor of the invention adds 0.01% 1% in M15 ~ M100 different trade mark methanol gasolines; rubber volume can be made to be swelled reduction 40% ~ 90%, the agent not only can effectively suppress methanol gasoline and is swelled to General Purpose Rubber, also there is certain inhibition protection effect to engine metal part.

Description

A kind of preparation method of methanol gasoline rubber swelling inhibitor
Technical field
The present invention relates to methanol gasoline additive technical field, and in particular to a kind of methanol gasoline rubber swelling inhibitor Preparation method.
Background technology
With energy-conserving and environment-protective and the proposition of low-carbon economy, vehicle alternative fuel is received significant attention.The property of methanol is being permitted It is many-sided similar to gasoline, therefore be considered as in internal combustion engine, particularly spark ignition engine is most hopeful that vapour can be replaced The new energy of oil.Current China has had multiple provinces and cities such as Shanxi, Henan to promote the use of methanol gasoline.Methanol gasoline anti-knock properties Can be good, research octane number (RON) increases with the increase of methanol incorporation, and motor octane number is then unaffected.Methanol gasoline burns The toxicity of effluent is smaller than common doped fuel, and carbon monoxide content is also less in exhaust.But methanol gasoline lacks there is also some Point, is easily caused rubber components on automobile and is damaged because of being swelled, particularly to hair wherein larger to the swelling ratio of elastomeric material Elastic gel, the seal of motivation have swelling action, sealing position can be caused to be cracked and oil leak, so as to hinder methanol gasoline Popularization and application.The research for also having some corresponding rubber swelling inhibitors at present is reported, but wherein contains sulfate, sulfonic acid more The component of the sulfur-bearings such as salt and metal ion, easily produces sulfur-containing compound in waste gas when using, and residues of combustion is easily in combustion Burn indoor fouling.
The content of the invention
In order to overcome the shortcoming of above-mentioned prior art, it is an object of the invention to provide a kind of methanol gasoline swell rubber The preparation method of inhibitor, can effectively suppress swell rubber.
In order to achieve the above object, the technical solution adopted by the present invention is：
A kind of preparation method of methanol gasoline rubber swelling inhibitor, comprises the following steps：
Hydroxy benzaldehyde is dissolved in 5-20 times of mass solvent in reaction vessel under the first step, normal temperature, the hydroxy benzenes Salicylaldhyde of the formaldehyde including technical grade and its above purity, m-hydroxybenzaldehyde, parahydroxyben-zaldehyde and combinations thereof, The solvent is technical grade and its methanol of above purity, ethanol, propyl alcohol, isopropanol, n-butanol, isobutanol, the tert-butyl alcohol, positive penta Alcohol, isoamyl alcohol, n-hexyl alcohol and its mixed liquor；
Second step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 0.9-1.1 under stirring：1 fat Fat amine and be 2-10 with the ratio of the amount of hydroxy benzaldehyde material：1 alkali, is heated to 50-140 DEG C, reacts 2-8 hours, the fat Fat amine is technical grade and its n-butylamine of above purity, n-hexylamine, lauryl amine, cetylamine, octadecylamine and combinations thereof, the alkali For technical grade and its sodium carbonate of above purity, sodium acid carbonate, potassium carbonate, saleratus and combinations thereof；
3rd step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 0.9-1 under stirring：1 halo Hydrocarbon, continues to react 2-8 hour at 50-140 DEG C, is cooled to room temperature, the halogenated hydrocarbons is technical grade and its above purity chloroethanes, Chloropropane, chloro-normal butane, chloro normal heptane, chlorinated dodecane, chloro-tetradecane, chloro-hexadecane, chlorooctadecane, bromine second Alkane, N-Propyl Bromide, bromination of n-butane, bromo heptane, bromododecane, bromotetradecane, bromohexadecane, bromo-octadecane and Its composition；
4th step, mixture in reaction vessel is filtered, and the ratio added into filtrate with the amount of hydroxy benzaldehyde material is 1：1-6 alkyl phenol, stirs, that is, obtains methanol gasoline rubber swelling inhibitor, the alkyl phenol be technical grade and its The nonyl phenol of above purity, anacardol and combinations thereof.
Beneficial effects of the present invention are：Different trade mark first of the gained methanol gasoline rubber swelling inhibitor in M15 ~ M100 0.01%-1% is added in alcohol gasoline, rubber volume can be made to be swelled reduction 40% ~ 90%, the agent not only can effectively suppress methanol gasoline General Purpose Rubber is swelled, also there is certain inhibition protection effect to engine metal part.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
A kind of preparation method of methanol gasoline rubber swelling inhibitor, comprises the following steps：
Hydroxy benzaldehyde is dissolved in 5 times of mass solvents in reaction vessel under the first step, normal temperature, the hydroxy benzaldehyde For the salicylaldhyde of technical grade, the solvent is the methanol of technical grade；
Second step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 0.9 under stirring：1 fatty amine With with the ratio of the amount of hydroxy benzaldehyde material be 2：1 alkali, is heated to 50 DEG C, reacts 8 hours, and the fatty amine is technical grade N-butylamine, the alkali is the sodium carbonate of technical grade；
3rd step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 0.9 under stirring：1 halogenated hydrocarbons, Continue to react 6 hours at 50 DEG C, be cooled to room temperature, the halogenated hydrocarbons is the chlorooctadecane of technical grade；
4th step, mixture in reaction vessel is filtered, and the ratio added into filtrate with the amount of hydroxy benzaldehyde material is 1：1 alkyl phenol, stirs, that is, obtains methanol gasoline rubber swelling inhibitor, and the alkyl phenol is the nonyl of technical grade Phenol.
The present embodiment has the beneficial effect that：Gained methanol gasoline rubber swelling inhibitor is added in M15 methanol gasolines 0.1%, rubber volume can be made to be swelled reduction 54%.
Embodiment 2
A kind of preparation method of methanol gasoline rubber swelling inhibitor, comprises the following steps：
Hydroxy benzaldehyde is dissolved in 8 times of mass solvents in reaction vessel under the first step, normal temperature, the hydroxy benzaldehyde For the pure m-hydroxybenzaldehyde of chemistry, the solvent is the pure ethanol of chemistry；
Second step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 1 under stirring：1 fatty amine and Ratio with the amount of hydroxy benzaldehyde material is 5：1 alkali, is heated to 80 DEG C, reacts 4 hours, and the fatty amine is pure just for chemistry Hexylamine, the alkali is the pure sodium acid carbonate of chemistry；
3rd step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 1 under stirring：1 halogenated hydrocarbons, after Continue and reacted 6 hours at 80 DEG C, be cooled to room temperature, the halogenated hydrocarbons is the pure chlorinated dodecane of chemistry；
4th step, mixture in reaction vessel is filtered, and the ratio added into filtrate with the amount of hydroxy benzaldehyde material is 1：2 alkyl phenol, stirs, that is, obtains methanol gasoline rubber swelling inhibitor, the alkyl phenol be technical grade and its with The anacardol of upper purity.
The present embodiment has the beneficial effect that：Gained methanol gasoline rubber swelling inhibitor is added in M30 methanol gasolines 0.05%, rubber volume can be made to be swelled reduction 51%.
Embodiment 3
A kind of preparation method of methanol gasoline rubber swelling inhibitor, comprises the following steps：
Hydroxy benzaldehyde is dissolved in 12 times of mass solvents in reaction vessel under the first step, normal temperature, the hydroxy benzenes first Aldehyde is analytically pure parahydroxyben-zaldehyde, and the solvent is analytically pure normal propyl alcohol；
Second step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 1.1 under stirring：1 fatty amine With with the ratio of the amount of hydroxy benzaldehyde material be 6：1 alkali, is heated to 97 DEG C, reacts 4 hours, and the fatty amine is analytically pure Lauryl amine, the alkali is analytically pure potassium carbonate；
3rd step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 1 under stirring：1 halogenated hydrocarbons, after Continue and reacted 4 hours at 97 DEG C, be cooled to room temperature, the halogenated hydrocarbons is analytically pure chloro-normal butane；
4th step, mixture in reaction vessel is filtered, and the ratio added into filtrate with the amount of hydroxy benzaldehyde material is 1：5 alkyl phenol, stirs, that is, obtains methanol gasoline rubber swelling inhibitor, the alkyl phenol be technical grade and its with The nonyl phenol of upper purity.
The present embodiment has the beneficial effect that：Gained methanol gasoline rubber swelling inhibitor is added in M15 methanol gasolines 0.08%, rubber volume can be made to be swelled reduction 62%.
Embodiment 4
A kind of preparation method of methanol gasoline rubber swelling inhibitor, comprises the following steps：
Hydroxy benzaldehyde is dissolved in 15 times of mass solvents in reaction vessel under the first step, normal temperature, the hydroxy benzenes first Aldehyde compares 1 for the amount of the material of technical grade purity:1 salicylaldhyde and parahydroxyben-zaldehyde, the solvent is that technical grade is pure The isopropanol of degree；
Second step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 1.1 under stirring：1 fatty amine With with the ratio of the amount of hydroxy benzaldehyde material be 10：1 alkali, is heated to 82 DEG C, reacts 4 hours, and the fatty amine is technical grade The cetylamine of purity, the alkali is the saleratus of technical grade purity；
3rd step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 1 under stirring：1 halogenated hydrocarbons, after Continue and reacted 4 hours at 82 DEG C, be cooled to room temperature, the halogenated hydrocarbons is technical grade purity bromination of n-butane；
4th step, mixture in reaction vessel is filtered, and the ratio added into filtrate with the amount of hydroxy benzaldehyde material is 1：3 alkyl phenol, stirs, that is, obtains methanol gasoline rubber swelling inhibitor, and the alkyl phenol is technical grade purity Anacardol.
The present embodiment has the beneficial effect that：Gained methanol gasoline rubber swelling inhibitor is added in M50 methanol gasolines 0.3%, rubber volume can be made to be swelled reduction 67%.
Embodiment 5
A kind of preparation method of methanol gasoline rubber swelling inhibitor, comprises the following steps：
Hydroxy benzaldehyde is dissolved in 20 times of mass solvents in reaction vessel under the first step, normal temperature, the hydroxy benzenes first Aldehyde is that the amount ratio of chemical pure material is 1:2 salicylaldhyde and parahydroxyben-zaldehyde, the solvent is the pure isobutyl of chemistry Alcohol；
Second step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 1.1 under stirring：1 fatty amine With with the ratio of the amount of hydroxy benzaldehyde material be 8：1 alkali, is heated to 108 DEG C, reacts 2 hours, and the fatty amine is pure for chemistry Octadecylamine, the alkali is the pure sodium carbonate of chemistry；
3rd step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 1 under stirring：1 halogenated hydrocarbons, after Continue and reacted 3 hours at 108 DEG C, be cooled to room temperature, the halogenated hydrocarbons is analytically pure bromoethane；
4th step, mixture in reaction vessel is filtered, and the ratio added into filtrate with the amount of hydroxy benzaldehyde material is 1：2 alkyl phenol, stirs, that is, obtains methanol gasoline rubber swelling inhibitor, and the alkyl phenol is the pure nonyl of chemistry Phenol.
The present embodiment has the beneficial effect that：Different trade mark methanol of the gained methanol gasoline rubber swelling inhibitor in M65 1% is added in gasoline, rubber volume can be made to be swelled reduction 65%.
Embodiment 6
A kind of preparation method of methanol gasoline rubber swelling inhibitor, comprises the following steps：
Hydroxy benzaldehyde is dissolved in 20 times of mass solvents in reaction vessel under the first step, normal temperature, the hydroxy benzenes first Aldehyde is the salicylaldhyde of technical grade purity, and the solvent is the isoamyl alcohol of technical grade purity；
Second step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 1.1 under stirring：1 fatty amine With with the ratio of the amount of hydroxy benzaldehyde material be 8：1 alkali, is heated to 140 DEG C, reacts 2 hours, and the fatty amine is technical grade The lauryl amine of purity, the alkali is the potassium carbonate of technical grade purity；
3rd step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 0.9 under stirring：1 halogenated hydrocarbons, Continue to react 2 hours at 140 DEG C, be cooled to room temperature, the halogenated hydrocarbons is that the amount ratio of technical grade purity material is 1:2 chloro Normal butane and chlorinated dodecane；
4th step, mixture in reaction vessel is filtered, and the ratio added into filtrate with the amount of hydroxy benzaldehyde material is 1：1 alkyl phenol, stirs, that is, obtains methanol gasoline rubber swelling inhibitor, and the alkyl phenol is technical grade purity matter Amount is than being 1:3 nonyl phenol and the composition of anacardol.
The present embodiment has the beneficial effect that：Gained methanol gasoline rubber swelling inhibitor adds in M85 methanol gasoline Plus 0.8%, rubber volume can be made to be swelled reduction 75%.

Claims (7)

1. a kind of preparation method of methanol gasoline rubber swelling inhibitor, it is characterised in that comprise the following steps：
Hydroxy benzaldehyde is dissolved in 5-20 times of mass solvent in reaction vessel under the first step, normal temperature, the hydroxy benzaldehyde Salicylaldhyde, m-hydroxybenzaldehyde, parahydroxyben-zaldehyde including technical grade and its above purity and combinations thereof, it is described Solvent be the methanol of technical grade and its above purity, ethanol, propyl alcohol, isopropanol, n-butanol, isobutanol, the tert-butyl alcohol, n-amyl alcohol, Isoamyl alcohol, n-hexyl alcohol and its mixed liquor；
Second step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 0.9-1.1 under stirring：1 fatty amine With with the ratio of the amount of hydroxy benzaldehyde material be 2-10：1 alkali, is heated to 50-140 DEG C, reacts 2-8 hours, the fatty amine For technical grade and its n-butylamine of above purity, n-hexylamine, lauryl amine, cetylamine, octadecylamine and combinations thereof, the alkali is work Industry level and its sodium carbonate of above purity, sodium acid carbonate, potassium carbonate, saleratus and combinations thereof；
3rd step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 0.9-1 under stirring：1 halogenated hydrocarbons, after Continue and reacted 2-8 hours at 50-140 DEG C, be cooled to room temperature, the halogenated hydrocarbons is technical grade and its above purity chloroethanes, chlorine third Alkane, chloro-normal butane, chloro normal heptane, chlorinated dodecane, chloro-tetradecane, chloro-hexadecane, chlorooctadecane, bromoethane, N-Propyl Bromide, bromination of n-butane, bromo heptane, bromododecane, bromotetradecane, bromohexadecane, bromo-octadecane and its Composition；
4th step, mixture in reaction vessel is filtered, and the ratio added into filtrate with the amount of hydroxy benzaldehyde material is 1：1-6 Alkyl phenol, stir, that is, obtain methanol gasoline rubber swelling inhibitor, the alkyl phenol is that technical grade and its above are pure The nonyl phenol of degree, anacardol and combinations thereof.
2. a kind of preparation method of methanol gasoline rubber swelling inhibitor according to claim 1, it is characterised in that bag Include following steps：
Hydroxy benzaldehyde is dissolved in 5 times of mass solvents in reaction vessel under the first step, normal temperature, the hydroxy benzaldehyde is work The salicylaldhyde of industry level, the solvent is the methanol of technical grade；
Second step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 0.9 under stirring：1 fatty amine and with The ratio of the amount of hydroxy benzaldehyde material is 2：1 alkali, is heated to 50 DEG C, reacts 8 hours, and the fatty amine is the positive fourth of technical grade Amine, the alkali is the sodium carbonate of technical grade；
3rd step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 0.9 under stirring：1 halogenated hydrocarbons, continues Reacted 6 hours at 50 DEG C, be cooled to room temperature, the halogenated hydrocarbons is the chlorooctadecane of technical grade；
4th step, mixture in reaction vessel is filtered, and the ratio added into filtrate with the amount of hydroxy benzaldehyde material is 1：1 Alkyl phenol, stirs, that is, obtains methanol gasoline rubber swelling inhibitor, and the alkyl phenol is the nonyl phenol of technical grade.
3. a kind of preparation method of methanol gasoline rubber swelling inhibitor according to claim 1, it is characterised in that bag Include following steps：
Hydroxy benzaldehyde is dissolved in 8 times of mass solvents in reaction vessel under the first step, normal temperature, the hydroxy benzaldehyde is change Pure m-hydroxybenzaldehyde is learned, the solvent is the pure ethanol of chemistry；
Second step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 1 under stirring：1 fatty amine and and hydroxyl The ratio of the amount of benzaldehyde material is 5：1 alkali, is heated to 80 DEG C, reacts 4 hours, the fatty amine for chemistry it is pure just oneself Amine, the alkali is the pure sodium acid carbonate of chemistry；
3rd step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 1 under stirring：1 halogenated hydrocarbons, continues 80 DEG C are reacted 6 hours, are cooled to room temperature, and the halogenated hydrocarbons is the pure chlorinated dodecane of chemistry；
4th step, mixture in reaction vessel is filtered, and the ratio added into filtrate with the amount of hydroxy benzaldehyde material is 1：2 Alkyl phenol, stirs, that is, obtains methanol gasoline rubber swelling inhibitor, and the alkyl phenol is technical grade and its above purity Anacardol.
4. a kind of preparation method of methanol gasoline rubber swelling inhibitor according to claim 1, it is characterised in that bag Include following steps：
Hydroxy benzaldehyde is dissolved in 12 times of mass solvents in reaction vessel under the first step, normal temperature, the hydroxy benzaldehyde is Analytically pure parahydroxyben-zaldehyde, the solvent is analytically pure normal propyl alcohol；
Second step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 1.1 under stirring：1 fatty amine and with The ratio of the amount of hydroxy benzaldehyde material is 6：1 alkali, is heated to 97 DEG C, reacts 4 hours, and the fatty amine is analytically pure 12 Amine, the alkali is analytically pure potassium carbonate；
3rd step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 1 under stirring：1 halogenated hydrocarbons, continues 97 DEG C are reacted 4 hours, are cooled to room temperature, and the halogenated hydrocarbons is analytically pure chloro-normal butane；
4th step, mixture in reaction vessel is filtered, and the ratio added into filtrate with the amount of hydroxy benzaldehyde material is 1：5 Alkyl phenol, stirs, that is, obtains methanol gasoline rubber swelling inhibitor, and the alkyl phenol is technical grade and its above purity Nonyl phenol.
5. a kind of preparation method of methanol gasoline rubber swelling inhibitor according to claim 1, it is characterised in that bag Include following steps：
Hydroxy benzaldehyde is dissolved in 15 times of mass solvents in reaction vessel under the first step, normal temperature, the hydroxy benzaldehyde is The amount of the material of technical grade purity compares 1:1 salicylaldhyde and parahydroxyben-zaldehyde, the solvent is technical grade purity Isopropanol；
Second step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 1.1 under stirring：1 fatty amine and with The ratio of the amount of hydroxy benzaldehyde material is 10：1 alkali, is heated to 82 DEG C, reacts 4 hours, and the fatty amine is technical grade purity Cetylamine, the alkali be technical grade purity saleratus；
3rd step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 1 under stirring：1 halogenated hydrocarbons, continues 82 DEG C are reacted 4 hours, are cooled to room temperature, and the halogenated hydrocarbons is technical grade purity bromination of n-butane；
4th step, mixture in reaction vessel is filtered, and the ratio added into filtrate with the amount of hydroxy benzaldehyde material is 1：3 Alkyl phenol, stirs, that is, obtains methanol gasoline rubber swelling inhibitor, and the alkyl phenol is the cashew nut of technical grade purity Phenol.
6. a kind of preparation method of methanol gasoline rubber swelling inhibitor according to claim 1, it is characterised in that bag Include following steps：
Hydroxy benzaldehyde is dissolved in 20 times of mass solvents in reaction vessel under the first step, normal temperature, the hydroxy benzaldehyde is The amount ratio of chemical pure material is 1:2 salicylaldhyde and parahydroxyben-zaldehyde, the solvent is the pure isobutanol of chemistry；
Second step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 1.1 under stirring：1 fatty amine and with The ratio of the amount of hydroxy benzaldehyde material is 8：1 alkali, is heated to 108 DEG C, reacts 2 hours, and the fatty amine is pure ten of chemistry Eight amine, the alkali is the pure sodium carbonate of chemistry；
3rd step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 1 under stirring：1 halogenated hydrocarbons, continues 108 DEG C are reacted 3 hours, are cooled to room temperature, and the halogenated hydrocarbons is analytically pure bromoethane；
4th step, mixture in reaction vessel is filtered, and the ratio added into filtrate with the amount of hydroxy benzaldehyde material is 1：2 Alkyl phenol, stirs, that is, obtains methanol gasoline rubber swelling inhibitor, and the alkyl phenol is the pure nonyl phenol of chemistry.
7. a kind of preparation method of methanol gasoline rubber swelling inhibitor according to claim 1, it is characterised in that bag Include following steps：
Hydroxy benzaldehyde is dissolved in 20 times of mass solvents in reaction vessel under the first step, normal temperature, the hydroxy benzaldehyde is The salicylaldhyde of technical grade purity, the solvent is the isoamyl alcohol of technical grade purity；
Second step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 1.1 under stirring：1 fatty amine and with The ratio of the amount of hydroxy benzaldehyde material is 8：1 alkali, is heated to 140 DEG C, reacts 2 hours, and the fatty amine is technical grade purity Lauryl amine, the alkali be technical grade purity potassium carbonate；
3rd step, into reaction vessel, the ratio of addition and the amount of hydroxy benzaldehyde material is 0.9 under stirring：1 halogenated hydrocarbons, continues Reacted 2 hours at 140 DEG C, be cooled to room temperature, the halogenated hydrocarbons is that the amount ratio of technical grade purity material is 1:The 2 positive fourth of chloro Alkane and chlorinated dodecane；
4th step, mixture in reaction vessel is filtered, and the ratio added into filtrate with the amount of hydroxy benzaldehyde material is 1：1 Alkyl phenol, stirs, that is, obtains methanol gasoline rubber swelling inhibitor, and the alkyl phenol is that technical grade purity mass ratio is 1:3 nonyl phenol and the composition of anacardol.
CN201610806942.8A 2016-09-07 2016-09-07 A kind of preparation method of methanol gasoline rubber swelling inhibitor Active CN106281501B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008024822A (en) * 2006-07-21 2008-02-07 Reiketsu Kichi Additive for alcohol-containing fuel oil, fuel oil containing the additive for alcohol-containing fuel oil, and method for producing fuel oil containing the additive for alcohol-containing fuel oil
CN102021053A (en) * 2010-12-31 2011-04-20 深圳市贝壳能源科技有限公司 Methanol gasoline denaturant and preparation method thereof
CN104357111A (en) * 2014-10-19 2015-02-18 青岛拓联信息技术有限公司 Methanol gasoline additive with stable performance
CN104711050A (en) * 2015-03-19 2015-06-17 黄河三角洲京博化工研究院有限公司 Compound gasoline antiknock and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008024822A (en) * 2006-07-21 2008-02-07 Reiketsu Kichi Additive for alcohol-containing fuel oil, fuel oil containing the additive for alcohol-containing fuel oil, and method for producing fuel oil containing the additive for alcohol-containing fuel oil
CN102021053A (en) * 2010-12-31 2011-04-20 深圳市贝壳能源科技有限公司 Methanol gasoline denaturant and preparation method thereof
CN104357111A (en) * 2014-10-19 2015-02-18 青岛拓联信息技术有限公司 Methanol gasoline additive with stable performance
CN104711050A (en) * 2015-03-19 2015-06-17 黄河三角洲京博化工研究院有限公司 Compound gasoline antiknock and preparation method thereof

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