CN106748668A - Ethylene glycol tertbutyl ether and its production technology - Google Patents
Ethylene glycol tertbutyl ether and its production technology Download PDFInfo
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- CN106748668A CN106748668A CN201611030003.5A CN201611030003A CN106748668A CN 106748668 A CN106748668 A CN 106748668A CN 201611030003 A CN201611030003 A CN 201611030003A CN 106748668 A CN106748668 A CN 106748668A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/05—Preparation of ethers by addition of compounds to unsaturated compounds
- C07C41/06—Preparation of ethers by addition of compounds to unsaturated compounds by addition of organic compounds only
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
- C07C41/42—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
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Abstract
The present invention relates to a kind of ethylene glycol tertbutyl ether and its production technology, belong to chemical products technique productions field.The ethylene glycol tertbutyl ether, generation is reacted by the isobutene in mixing carbon four and ethylene glycol in the presence of solid catalyst；Its technological process includes reaction member and separative element.The ethylene glycol tertbutyl ether prepared using technique of the present invention has the advantages that extremely low smell, hypotoxicity, low photo-chemically reactive, and gentle to skin irritation, property compatible with water is good, it is good to latex paint dispersion stabilization, mixed with most resins, organic solvent, and good hydrophilic property, can be widely applied to coating, ink, cleaning agent, fiber wetting agent, plasticizer, many fields such as organic synthesis intermediate, paint stripper.
Description
Technical field
The present invention relates to a kind of ethylene glycol tertbutyl ether and its production technology, belong to chemical products technique productions field.
Background technology
Gylcol ether is the important derivatives of oxirane, the history for having nearly 90 years so far of being gone into operation from nineteen twenty-six,
Because its intramolecular contains ehter bond and hydroxyl, with its excellent performance, it is widely used as solvent, jet fuel anti-freezing agent, brake
Liquid, chemical intermediate.
In China, up to 85% alcohol ether and alcohol ether ester solvent are used in coating (resinous), wherein, with ethylene glycol first
Ether, ethylene glycol ethyl ether, butyl glycol ether are that the consumption of representative occupy the first.But in recent years, with people's health consciousness strengthen and
Environmental regulation it is increasingly strict, the safety and environmental protection aspect of conventional glycol ether start to expose increasing problem.Grind
Study carefully and show, glycol ether (methyl ether, ether) can cause dysemia and fetal anomaly, developed countries and area have been opened
Begin to limit production and use.From 2001, the Ministry of Public Health of China dispatch regulation prohibits the use of ethylene glycol in dispensing used by indoor coating
Ether and its esters, in May, 2009, the state environment protecting standard of Environmental Protection in China portion issue《Environmental labelling product technical requirements-anti-
Water paint》Middle clear stipulaties, must not artificially add glycol ether and esters in water-repellent paint.Glycol butyl once always by
It is considered safe, but European Union in 2009 issues new instruction, limits it and is used in the articles for use such as hair dye.In March, 2015,
EPA announces a final rule, and seven classes may be led to the ethylene glycol of the health problems such as birth defect and septicemia
Ether implements import restriction, relevant enterprise import, produces or processes this seven classes glycol ether, it is necessary to notify U.S. ring within least 90 days in advance
Guarantor office is audited.With the continuous atrophy in consumption field of conventional glycol ether (methyl ether, ether, butyl ether) series of products, seek
Novel environment friendly field has been forced to turn into manufacturing enterprise and downstream field issues that need special attention.
Development of the market demand of glycol ether and its esters substantially with coating industry is synchronous.China's coating industry is in recent years
Fast development, yield increases to 1303.35 ten thousand tons/year, wherein solvent based coating in 2013 from 241.5 ten thousand tons/year of 2000
Account for 50%, about 3,000,000 tons/year of the demand of solvent, accounting of the butyl glycol ether in paint solvent about 4%, i.e., 140,000 tons/
Year.Butyl glycol ether in recent years domestic apparent demand amount at 16~180,000 tons/year, nearly 80% Dependent Demand import, but overall supply
Situation is answered to show superfluous.Domestic enterprise with moral receive a day sound, Jiangsu is happy reach based on, imported goods source is so that South Korea is carefree, LG-DOW,
Based on Yi Shiman, Li Ande, Petronas's chemical industry.Therewith coating, paint industry " oil changes water " progress faster and safety
Environmental regulation it is increasingly strict, butyl glycol ether demand will atrophy be progressively that the development of substitute is reserved until withdraw from the market
Space.
Ethylene glycol tertbutyl ether, English name：Ethylene glycol tertiary butyl ether (abbreviation ETB),
No. CAS：7580-85-0；Molecular formula：C6H14O2；Molecular weight：118.18.
The physicochemical property of ethylene glycol tertbutyl ether：Water white transparency has mint flavored flammable liquid.Can be organic with majority
Solvent dissolves each other, and can dissolve the resins such as amino, nitro, alkyd, acrylic acid.Miscible with water, low toxicity, low thorn under room temperature (25 DEG C)
Swash property.Design parameter is as shown in the table：
| Performance | Parameter | Performance | Parameter |
| Relative density (water=1) | 0.903 | Initial boiling point | 150.5℃ |
| Freezing point | ＜ -120 DEG C | 5% distillates | 151.0℃ |
| Ignition point (is closed) | 55℃ | 10% distillates | 151.5℃ |
| Firing temperature | 417℃ | 50% distillates | 152.0℃ |
| Surface tension (20 DEG C) | 2.63Pa | 95% distillates | 152.0℃ |
| Vapour pressure (20 DEG C) | 213.3Pa | Quantity of distillate (Vol) | 99.9% |
| Solubility parameter | 9.35 | Do | 152.5℃ |
Ethylene glycol tertbutyl ether mainly substitutes butyl glycol ether, in contrast, there is extremely low smell, hypotoxicity, low photochemistry
Reactive the advantages of, gentle to skin irritation, property compatible with water is good, good to latex paint dispersion stabilization, with most resins,
Organic solvent mixes, and good hydrophilic property, can be widely applied to coating, ink, cleaning agent, fiber wetting agent, plasticizer, You Jihe
Into intermediate, many fields such as paint stripper.Its main application is as follows：
1st, aqueous coating solvent
It is mainly used in the solvent of water-based system, latex Water-dispersing coatings in coatings industry.Because the HLB value of ETB is close to 9.0,
Its function in dispersion plays a part of dispersant, emulsifying agent, rheological agent, cosolvent, to latex oil in water paint
Paint, colloidal dispersions coating and lysotype aqueous solution cold coating performance are good, for building coating for internal and external wall, vehicle paint base, coloured silk
The fields such as color tinplate.
2nd, paint solvent
2.1 make dispersant.When producing goth black amino paint and goth black acrylic paint, it usually needs the plenty of time grinds pigment high
Carbon black is to reach certain fineness, and the high-carbon black pigment soaked using ETB, and its milling time can shorten more than half, and
And cover with paint, lacquer, colour wash, etc. after paint outward appearance it is more smooth, smooth.
2.2 make levelling agent and defoamer, improve rate of drying, flatness, glossiness, the attachment fastness of Water-dispersing coatings.
Due to its tertiary-butyl structure, make it have photochemical stability and security higher, can eliminate the pin hole of paint film, little particle and
Bubble.The Water-dispersing coatings being made of ET, under conditions of having good storage stability, particularly a winter low temperature.
2.3 improve glossiness.ETB is applied in amino paint, nitrate paint, can prevent " tangerine peel " shape speckle, paint film light
Damp degree improves 2%~6%.
3rd, ink dispersant
The ink being made as solvent with ETB, or be used in printing-ink as dilution dispersant, it is greatly improved ink
Rheological characteristic, improve high speed printing quality and glossiness, adhesive force.
4th, fibre abstraction agent
Alied-Signal companies of the U.S. extract the polyethylene fiber Wesy ETB containing 76% mineral oil, the fiber after extraction
Mineral oil in fluid content reduction by 0.15%.
5th, titanium oxide phthalocyanine dye
Japanese Canon companies add Ti (OBu) 4 in the ETB solution of 1,3- diaminourea isoindolines, are stirred at 130 DEG C
3h is mixed, the titanium oxide phthalocyanine dye of 87% purity is obtained.And the crystalline titanium oxide phthalein being made up of porous oxidation titanium phthalocyanines and ETB
Cyanines, can be used as the quick device of light sensation of taking a picture, and it has hypersensitivity to the glistening light of waves long.
6th, high effective household cleaning agent
Japanese rising sun electrician company expoxy propane and the KOH post-reaction treatments containing ETB, obtain the polyoxy propane list tert-butyl group
Ether, this is a kind of preferable high effective household cleaning agent.
7th, anticorrosive water-soluble shellac varnish
Nippon Paint company is made of dimethyl ether, acrylic resin, ETB, butanol, TiO2, cyclohexyl amine carbonate, defoamer
A kind of sprayable anticorrosive water-soluble shellac varnish.
8th, radio component fixed carbon resister
Make the fixed carbon resister of resistor fluid with ETB, surface is smooth, the bad phenomenon of pin hole and webbing can be eliminated, improve
The performance of electric elements.
9th, fuel adjunct
ETB can not only improve efficiency of combustion as the cosolvent of New-type boiler fuel, modifying agent, and can the row of reduction
Put, as boiler and the novel energy of big marine diesel engine, there is the advantage in terms of environmentally friendly rigid demand and policy bonus.
The content of the invention
It is an object of the present invention to provide a kind of ethylene glycol tertbutyl ether and its production technology, to solve above-mentioned technology
Problem.
The present invention is achieved through the following technical solutions：
A kind of ethylene glycol tertbutyl ether, it is characterised in that：By the isobutene in mixing carbon four and ethylene glycol in solid catalysis
Generation is reacted in the presence of agent, wherein, isobutene is 3-4 with the reaction ratio of ethylene glycol：0.8-1.2；The reaction is individual reversible
Balance exothermic process, its reaction equation is as follows：
Further say, the isobutene is 3.7 with the reaction ratio of ethylene glycol：1.
Further say, the technological process of the ethylene glycol tertbutyl ether production technology includes：
A, reaction member, comprise the following steps：
A1, the raw material of the carbon four feeding surge tank of carbon four rich in isobutene, exchange heat through the boosting of the feed pump of carbon four, the stabilizer of carbon four
After device heat exchange, into the stabilizer of carbon four, the operating pressure of the stabilizer of the carbon four is 1.73MPa；
It is steady into carbon four after A2, the overhead product of the stabilizer of the carbon four are cooled to 40 DEG C through the stabilizer condenser of carbon four
Determine tower return tank；, through the stabilizer of carbon four backflow pumped, used as backflow feeding tower top, another part is used as light for a part for condensate liquid
The product of carbon four is sent out；
A3, the tower bottom product of the stabilizer of the carbon four are attached most importance to carbon four, and weight carbon four is changed through the stabilizer heat exchanger of carbon four with charging
Enter reaction member after heat；
A4, virgin ethylene glycol and circulation ethylene glycol feeding ethylene glycol surge tank, after being boosted through ethylene glycol feed pump, with weight carbon
4th, after etherification reaction product circulation logistics, circulation ethylene glycol dual-tert-butyl ether mix in the reaction feed blender, into mixed
Close preheater；
A5, be preheated to 55 DEG C after, into fixed bed etherification reactor；The fixed bed etherification reactor includes etherification reaction
Protector, one section of methyltertiarvbutyl ether reactor and two sections of methyltertiarvbutyl ether reactors, wherein, filling etherification protection agent, one in etherification reaction protector
Catalyst for etherification is loaded in section methyltertiarvbutyl ether reactor and two sections of methyltertiarvbutyl ether reactors；
A6, under catalyst for etherification effect, isobutene and glycol reaction generate the product based on ethylene glycol tertbutyl ether
Thing；
B, separative element, comprise the following steps：
B1, exchanged heat to after 135 DEG C through butane removing tower heat exchanger from two sections of reaction products of methyltertiarvbutyl ether reactor, into de-
The tower of carbon four, the operating pressure of the butane removing tower is 0.33MPa；
B2, the unreacted carbon four, tert-butyl alcohol and isobutylene oligome product are steamed from the tower top of butane removing tower, through butane removing tower
After condenser is cooled to 36 DEG C, into butane removing tower return tank；, through the backflow pumped of decarburization four, a part is used as backflow for condensate liquid
Feeding tower top, another part is sent out as the product of carbon four；
B3, the tower bottom product of butane removing tower first exchange heat to 140 DEG C through butane removing tower heat exchanger with charging, then through butane removing tower
After the cooler of bottom of towe is cooled to 99 DEG C, into azeotrope column；
After B4, the tower bottom product of butane removing tower mix with the overhead product of circulation ethylene glycol dual-tert-butyl ether knockout tower, enter
Enter azeotrope column, the azeotropic mixture of ethylene glycol tertbutyl ether-circulation ethylene glycol dual-tert-butyl ether-water is formed in the tower top of azeotrope column；
After B5, the azeotropic mixture are cooled to 99 DEG C through azeotrope column condenser, into azeotropic column separator, separated in azeotrope column
There is hydrocarbon water two-phase laminated flow in device；The hydrocarbon phase of tertbutyl ether containing ethylene glycol and circulation ethylene glycol dual-tert-butyl ether, through azeotrope column oil
Mutually it is pumped to circulation ethylene glycol dual-tert-butyl ether knockout tower；Aqueous and ethylene glycol tertbutyl ether the water in azeotropic column separator bottom
Phase, azeotropic tower top is returned to after being boosted through azeotrope column aqueous-phase reflux pump as backflow；The bottom of towe of azeotrope column is containing ethylene glycol and second two
The mixture of alcohol tertbutyl ether, after being boosted through azeotropic column bottoms pump, sends into ethylene glycol tertbutyl ether purifying column；
B6, the overhead product of the circulation ethylene glycol dual-tert-butyl ether knockout tower are separated through circulating ethylene glycol dual-tert-butyl ether
After tower condenser is cooled to 99 DEG C, into circulation ethylene glycol dual-tert-butyl ether knockout tower return tank；The double uncles of circulation ethylene glycol
, through circulating ethylene glycol dual-tert-butyl ether knockout tower backflow pumped, a part is used as backflow for liquid phase in butyl ether knockout tower return tank
The tower top of feeding circulation ethylene glycol dual-tert-butyl ether knockout tower, another part then sends azeotrope column back to as circulation fluid；Circulation second two
The tower bottom product of alcohol dual-tert-butyl ether knockout tower is mainly circulation ethylene glycol dual-tert-butyl ether, through circulating ethylene glycol dual-tert-butyl ether
After the bottom of towe cooler cooling of knockout tower, reaction member is pumped to by the bottom of towe of circulation ethylene glycol dual-tert-butyl ether knockout tower；
B7, the overhead product of the ethylene glycol tertbutyl ether purifying column are cooled down through ethylene glycol tertbutyl ether purifying column condenser
To after 40 DEG C, into ethylene glycol tertbutyl ether purifying column return tank；Condensate liquid in ethylene glycol tertbutyl ether purifying column return tank
Through ethylene glycol tertbutyl ether purifying column return tank backflow pumped, a part is used as backflow feeding ethylene glycol tertbutyl ether purifying column
Tower top, another part is then sent as ethylene glycol tertbutyl ether product.
Furtherly, in the step B7, the tower bottom product of ethylene glycol tertbutyl ether purifying column is ethylene glycol mixture；
Ethylene glycol mixture is delivered into ethylene glycol flash column, is flashed under the pressure of 20kPa (A), the tower top of ethylene glycol flash column
After product is cooled to 40 DEG C through ethylene glycol flash column condenser, into ethylene glycol flash column lime set tank；Ethylene glycol flash column lime set
Condensate liquid in tank is delivered to ethylene glycol surge tank and is recycled after being boosted through glycol circulation pump.
Beneficial effect：Compared with prior art, the ethylene glycol tertbutyl ether for being prepared using technique of the present invention has pole
The advantages of low smell, hypotoxicity, low photo-chemically reactive, gentle to skin irritation, property compatible with water is good, to latex paint point
Good stability is dissipated, is mixed with most resins, organic solvent, and good hydrophilic property, coating is can be widely applied to, ink, cleaning agent is fine
Many fields such as dimension wetting agent, plasticizer, organic synthesis intermediate, paint stripper.
Specific embodiment
Below with reference to specific embodiment, the present invention is described further.
Ethylene glycol tertbutyl ether of the present invention, by the isobutene in mixing carbon four and ethylene glycol in solid catalyst
The lower reaction generation of effect, wherein, isobutene is 3-4 with the reaction ratio of ethylene glycol：0.8-1.2, as preferred scheme, isobutyl
Alkene is 3.7 with the reaction ratio of ethylene glycol：1；The reaction is a reversible balance exothermic process, and its reaction equation is as follows：
With height, other components of carbon four hardly participate in reaction to the selectivity of reaction, but occur simultaneously in main reaction following secondary
Reaction：
The technological process of ethylene glycol tertbutyl ether production technology of the present invention includes：
A, reaction member, comprise the following steps：
A1, the raw material of the carbon four feeding surge tank of carbon four rich in isobutene, exchange heat through the boosting of the feed pump of carbon four, the stabilizer of carbon four
After device heat exchange, into the stabilizer of carbon four, the operating pressure of the stabilizer of the carbon four is 1.73MPa；
It is steady into carbon four after A2, the overhead product of the stabilizer of the carbon four are cooled to 40 DEG C through the stabilizer condenser of carbon four
Determine tower return tank；, through the stabilizer of carbon four backflow pumped, used as backflow feeding tower top, another part is used as light for a part for condensate liquid
The product of carbon four is sent out；
A3, the tower bottom product of the stabilizer of the carbon four are attached most importance to carbon four, and weight carbon four is changed through the stabilizer heat exchanger of carbon four with charging
Enter reaction member after heat；
A4, virgin ethylene glycol and circulation ethylene glycol feeding ethylene glycol surge tank, after being boosted through ethylene glycol feed pump, with weight carbon
4th, after etherification reaction product circulation logistics, circulation ethylene glycol dual-tert-butyl ether mix in the reaction feed blender, into mixed
Close preheater；
A5, be preheated to 55 DEG C after, into fixed bed etherification reactor；The fixed bed etherification reactor includes etherification reaction
Protector, one section of methyltertiarvbutyl ether reactor and two sections of methyltertiarvbutyl ether reactors, wherein, filling etherification protection agent, one in etherification reaction protector
Catalyst for etherification is loaded in section methyltertiarvbutyl ether reactor and two sections of methyltertiarvbutyl ether reactors；
A6, under catalyst for etherification effect, isobutene and glycol reaction generate the product based on ethylene glycol tertbutyl ether
Thing；
B, separative element, comprise the following steps：
B1, exchanged heat to after 135 DEG C through butane removing tower heat exchanger from two sections of reaction products of methyltertiarvbutyl ether reactor, into de-
The tower of carbon four, the operating pressure of the butane removing tower is 0.33MPa；
B2, the unreacted carbon four, tert-butyl alcohol and isobutylene oligome product are steamed from the tower top of butane removing tower, through butane removing tower
After condenser is cooled to 36 DEG C, into butane removing tower return tank；, through the backflow pumped of decarburization four, a part is used as backflow for condensate liquid
Feeding tower top, another part is sent out as the product of carbon four；
B3, the tower bottom product of butane removing tower first exchange heat to 140 DEG C through butane removing tower heat exchanger with charging, then through butane removing tower
After the cooler of bottom of towe is cooled to 99 DEG C, into azeotrope column；
After B4, the tower bottom product of butane removing tower mix with the overhead product of circulation ethylene glycol dual-tert-butyl ether knockout tower, enter
Enter azeotrope column, the azeotropic mixture of ethylene glycol tertbutyl ether-circulation ethylene glycol dual-tert-butyl ether-water is formed in the tower top of azeotrope column；
After B5, the azeotropic mixture are cooled to 99 DEG C through azeotrope column condenser, into azeotropic column separator, separated in azeotrope column
There is hydrocarbon water two-phase laminated flow in device；The hydrocarbon phase of tertbutyl ether containing ethylene glycol and circulation ethylene glycol dual-tert-butyl ether, through azeotrope column oil
Mutually it is pumped to circulation ethylene glycol dual-tert-butyl ether knockout tower；Aqueous and ethylene glycol tertbutyl ether the water in azeotropic column separator bottom
Phase, azeotropic tower top is returned to after being boosted through azeotrope column aqueous-phase reflux pump as backflow；The bottom of towe of azeotrope column is containing ethylene glycol and second two
The mixture of alcohol tertbutyl ether, after being boosted through azeotropic column bottoms pump, sends into ethylene glycol tertbutyl ether purifying column；
B6, the overhead product of the circulation ethylene glycol dual-tert-butyl ether knockout tower are separated through circulating ethylene glycol dual-tert-butyl ether
After tower condenser is cooled to 99 DEG C, into circulation ethylene glycol dual-tert-butyl ether knockout tower return tank；The double uncles of circulation ethylene glycol
, through circulating ethylene glycol dual-tert-butyl ether knockout tower backflow pumped, a part is used as backflow for liquid phase in butyl ether knockout tower return tank
The tower top of feeding circulation ethylene glycol dual-tert-butyl ether knockout tower, another part then sends azeotrope column back to as circulation fluid；Circulation second two
The tower bottom product of alcohol dual-tert-butyl ether knockout tower is mainly circulation ethylene glycol dual-tert-butyl ether, through circulating ethylene glycol dual-tert-butyl ether
After the bottom of towe cooler cooling of knockout tower, reaction member is pumped to by the bottom of towe of circulation ethylene glycol dual-tert-butyl ether knockout tower；
B7, the overhead product of the ethylene glycol tertbutyl ether purifying column are cooled down through ethylene glycol tertbutyl ether purifying column condenser
To after 40 DEG C, into ethylene glycol tertbutyl ether purifying column return tank；Condensate liquid in ethylene glycol tertbutyl ether purifying column return tank
Through ethylene glycol tertbutyl ether purifying column return tank backflow pumped, a part is used as backflow feeding ethylene glycol tertbutyl ether purifying column
Tower top, another part is sent as ethylene glycol tertbutyl ether product.
In the step B7, the bottom of towe of ethylene glycol tertbutyl ether purifying column is ethylene glycol mixture；By ethylene glycol mixture
Ethylene glycol flash column is delivered to, is flashed under the pressure of 20kPa (A), the overhead product of ethylene glycol flash column dodges through ethylene glycol
After steaming tower condenser is cooled to 40 DEG C, into ethylene glycol flash column lime set tank；Condensate liquid warp in ethylene glycol flash column lime set tank
The recycling of ethylene glycol surge tank is delivered in the boosting of glycol circulation pump.
The various equipment used in production technology of the present invention are the common apparatus of chemical industry, their structure with
And installation, application method are prior art, it is no longer repeated herein.
The basic principles, principal features and advantages of the present invention have been shown and described above.The technical staff of the industry should
Understand, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these change and change
Enter all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by appending claims and its equivalent
Define.
Claims (4)
1. a kind of ethylene glycol tertbutyl ether, it is characterised in that：By the isobutene in mixing carbon four and ethylene glycol in solid catalyst
In the presence of react generation, wherein, the reaction ratio of isobutene and ethylene glycol is 3-4：0.8-1.2；The reaction is individual reversible flat
Weighing apparatus exothermic process, its reaction equation is as follows：
2. ethylene glycol tertbutyl ether according to claim 1, it is characterised in that：The reaction ratio of the isobutene and ethylene glycol
Example is 3.7:1.
3. the production technology of ethylene glycol tertbutyl ether as claimed in claim 1 or 2, it is characterised in that：The work of the production technology
Skill flow includes：
(A) reaction member, comprises the following steps：
(A1) raw material of the carbon four feeding surge tank of carbon four rich in isobutene, through the boosting of the feed pump of carbon four, the stabilizer heat exchanger of carbon four
After heat exchange, into the stabilizer of carbon four, the operating pressure of the stabilizer of the carbon four is 1.73MPa；
(A2) after the overhead product of the stabilizer of the carbon four is cooled to 40 DEG C through the stabilizer condenser of carbon four, into the stabilizer of carbon four
Return tank；, through the stabilizer of carbon four backflow pumped, used as backflow feeding tower top, another part is used as light carbon four for a part for condensate liquid
Product is sent out；
(A3) tower bottom product of the stabilizer of the carbon four is attached most importance to carbon four, and weight carbon four is through after the stabilizer heat exchanger of carbon four and charging heat exchange
Into reaction member；
(A4) virgin ethylene glycol with circulation ethylene glycol feeding ethylene glycol surge tank, through ethylene glycol feed pump boost after, with weight carbon four,
After etherification reaction product circulation logistics, circulation ethylene glycol dual-tert-butyl ether mix in reaction feed blender, into mixing
Preheater；
(A5) after being preheated to 55 DEG C, into fixed bed etherification reactor；The fixed bed etherification reactor is protected including etherification reaction
Shield device, one section of methyltertiarvbutyl ether reactor and two sections of methyltertiarvbutyl ether reactors, wherein, filling etherification protection agent, one section in etherification reaction protector
Catalyst for etherification is loaded in methyltertiarvbutyl ether reactor and two sections of methyltertiarvbutyl ether reactors；
(A6) under catalyst for etherification effect, isobutene and glycol reaction generate the product based on ethylene glycol tertbutyl ether；
(B) separative element, comprises the following steps：
(B1) exchanged heat to after 135 DEG C through butane removing tower heat exchanger from two sections of reaction products of methyltertiarvbutyl ether reactor, into decarburization
Four towers, the operating pressure of the butane removing tower is 0.33MPa；
(B2) the unreacted carbon four, tert-butyl alcohol and isobutylene oligome product are steamed from the tower top of butane removing tower, cold through butane removing tower
After condenser is cooled to 36 DEG C, into butane removing tower return tank；Condensate liquid send through the backflow pumped of decarburization four, a part as backflow
Enter tower top, another part is sent out as the product of carbon four；
(B3) tower bottom product of butane removing tower first exchanges heat to 140 DEG C through butane removing tower heat exchanger with charging, then through butane removing tower tower
After the cooler at bottom is cooled to 99 DEG C, into azeotrope column；
(B4) after the tower bottom product of butane removing tower mixes with the overhead product of circulation ethylene glycol dual-tert-butyl ether knockout tower, into altogether
Boiling tower, the azeotropic mixture of ethylene glycol tertbutyl ether-circulation ethylene glycol dual-tert-butyl ether-water is formed in the tower top of azeotrope column；
(B5) after the azeotropic mixture is cooled to 99 DEG C through azeotrope column condenser, into azeotropic column separator, in azeotropic column separator
Middle generation hydrocarbon water two-phase laminated flow；The hydrocarbon phase of tertbutyl ether containing ethylene glycol and circulation ethylene glycol dual-tert-butyl ether, through azeotrope column oil phase
It is pumped to circulation ethylene glycol dual-tert-butyl ether knockout tower；Aqueous and ethylene glycol tertbutyl ether the water phase in azeotropic column separator bottom,
After being boosted through azeotrope column aqueous-phase reflux pump azeotropic tower top is returned to as backflow；The bottom of towe of azeotrope column is containing ethylene glycol and ethylene glycol uncle
The mixture of butyl ether, after being boosted through azeotropic column bottoms pump, sends into ethylene glycol tertbutyl ether purifying column；
(B6) overhead product of the circulation ethylene glycol dual-tert-butyl ether knockout tower is through circulating ethylene glycol dual-tert-butyl ether knockout tower
After condenser is cooled to 99 DEG C, into circulation ethylene glycol dual-tert-butyl ether knockout tower return tank；The double tertiary fourths of circulation ethylene glycol
Liquid phase is sent through circulating ethylene glycol dual-tert-butyl ether knockout tower backflow pumped, a part as backflow in base ether knockout tower return tank
Enter to circulate the tower top of ethylene glycol dual-tert-butyl ether knockout tower, another part then sends azeotrope column back to as circulation fluid；Circulation ethylene glycol
The tower bottom product of dual-tert-butyl ether knockout tower is mainly circulation ethylene glycol dual-tert-butyl ether, through circulating ethylene glycol dual-tert-butyl ether point
After the bottom of towe cooler cooling of tower, reaction member is pumped to by the bottom of towe of circulation ethylene glycol dual-tert-butyl ether knockout tower；
(B7) overhead product of the ethylene glycol tertbutyl ether purifying column is cooled to through ethylene glycol tertbutyl ether purifying column condenser
After 40 DEG C, into ethylene glycol tertbutyl ether purifying column return tank；Condensate liquid warp in ethylene glycol tertbutyl ether purifying column return tank
Ethylene glycol tertbutyl ether purifying column return tank backflow pumped, a part is used as backflow feeding ethylene glycol tertbutyl ether purifying column tower
Top, another part is then sent as ethylene glycol tertbutyl ether product.
4. the production technology of ethylene glycol tertbutyl ether according to claim 3, it is characterised in that：In the step (B7), second
The tower bottom product of glycol tertbutyl ether purifying column is ethylene glycol mixture；Ethylene glycol mixture is delivered into ethylene glycol flash column,
Flashed under the pressure of 20kPa (A), the overhead product of ethylene glycol flash column is cooled to 40 DEG C through ethylene glycol flash column condenser
Afterwards, into ethylene glycol flash column lime set tank；Condensate liquid in ethylene glycol flash column lime set tank send after being boosted through glycol circulation pump
Recycled to ethylene glycol surge tank.
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| CN107739300A (en) * | 2017-10-23 | 2018-02-27 | 黄河三角洲京博化工研究院有限公司 | A kind of process for producing high-purity isobutene and ethylene glycol mono-tert-butyl ether |
| CN107794143A (en) * | 2017-08-31 | 2018-03-13 | 深圳市港联化工有限公司 | It is a kind of to remove the dirty agent for carbon hydrogen detergent in gap |
| CN109704930A (en) * | 2018-12-27 | 2019-05-03 | 深圳市前海博扬研究院有限公司 | The method and fuel oil additive of high selectivity dihydric alcohol di-tert-butyl ether |
| CN109852445A (en) * | 2018-12-25 | 2019-06-07 | 中国标准化研究院 | A kind of environment-friendly type motor petrol component substituting MTBE |
| CN111269095A (en) * | 2018-12-04 | 2020-06-12 | 湖南中创化工股份有限公司 | Method and system for refining ethylene glycol tert-butyl ether |
| CN111793380A (en) * | 2020-08-25 | 2020-10-20 | 江苏冠军科技集团股份有限公司 | Paint diluent containing solvent not participating in photochemical reaction and preparation method and application thereof |
| CN113461496A (en) * | 2020-03-30 | 2021-10-01 | 中国石油化工股份有限公司 | Synthesis method and synthesis system of dihydric alcohol mono-tert-butyl ether |
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| CN107794143A (en) * | 2017-08-31 | 2018-03-13 | 深圳市港联化工有限公司 | It is a kind of to remove the dirty agent for carbon hydrogen detergent in gap |
| CN107739300A (en) * | 2017-10-23 | 2018-02-27 | 黄河三角洲京博化工研究院有限公司 | A kind of process for producing high-purity isobutene and ethylene glycol mono-tert-butyl ether |
| CN107739300B (en) * | 2017-10-23 | 2021-02-09 | 黄河三角洲京博化工研究院有限公司 | Process method for producing high-purity isobutene and ethylene glycol mono-tert-butyl ether |
| CN111269095A (en) * | 2018-12-04 | 2020-06-12 | 湖南中创化工股份有限公司 | Method and system for refining ethylene glycol tert-butyl ether |
| CN111269095B (en) * | 2018-12-04 | 2022-08-12 | 湖南中创化工股份有限公司 | Method and system for refining ethylene glycol tert-butyl ether |
| CN109852445A (en) * | 2018-12-25 | 2019-06-07 | 中国标准化研究院 | A kind of environment-friendly type motor petrol component substituting MTBE |
| CN109852445B (en) * | 2018-12-25 | 2021-10-08 | 中国标准化研究院 | Environment-friendly vehicle gasoline component for replacing MTBE |
| CN109704930A (en) * | 2018-12-27 | 2019-05-03 | 深圳市前海博扬研究院有限公司 | The method and fuel oil additive of high selectivity dihydric alcohol di-tert-butyl ether |
| CN113461496A (en) * | 2020-03-30 | 2021-10-01 | 中国石油化工股份有限公司 | Synthesis method and synthesis system of dihydric alcohol mono-tert-butyl ether |
| CN111793380A (en) * | 2020-08-25 | 2020-10-20 | 江苏冠军科技集团股份有限公司 | Paint diluent containing solvent not participating in photochemical reaction and preparation method and application thereof |
| WO2022041939A1 (en) * | 2020-08-25 | 2022-03-03 | 江苏冠军科技集团股份有限公司 | Coating material diluent comprising solvent not participating in photochemical reaction, preparation method therefor and use thereof |
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