CN107739300A - A kind of process for producing high-purity isobutene and ethylene glycol mono-tert-butyl ether - Google Patents
A kind of process for producing high-purity isobutene and ethylene glycol mono-tert-butyl ether Download PDFInfo
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- CN107739300A CN107739300A CN201710992691.1A CN201710992691A CN107739300A CN 107739300 A CN107739300 A CN 107739300A CN 201710992691 A CN201710992691 A CN 201710992691A CN 107739300 A CN107739300 A CN 107739300A
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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
- C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
- C07C1/20—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon starting from organic compounds containing only oxygen atoms as heteroatoms
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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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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/40—Ethylene production
Abstract
The invention discloses a kind of while produce the production technology of high-purity isobutene and ethylene glycol mono-tert-butyl ether, belong to chemical products technique productions field.The production technology is that ethylene glycol generates ethylene glycol mono-tert-butyl ether crude product with mixing the isobutene in carbon four in the presence of solid catalyst, and part ethylene glycol mono-tert-butyl ether crude product prepares ethylene glycol mono-tert-butyl ether product by rectification and purification；Remainder ethylene glycol mono-tert-butyl ether crude product cracking reaction under solid catalyst effect generates high-purity isobutene product.The technique prepares high-purity isobutene technique and has the advantages that technological process is simple, equipment investment is small, product is easily separated, energy consumption is low, superior product quality compared with traditional；Novel environment friendly solvent ethylene glycol list tertbutyl ether can also be produced simultaneously, increases the anti-market risk ability of device, reduce total cost of production；It is a kind of advanced process.
Description
Technical field
The present invention relates to chemical products technical field of producing, and in particular to one kind produces high-purity isobutene and ethylene glycol
The process of single tertbutyl ether
Background technology
High-purity isobutylene refers generally to the product that isobutene purity is more than 99.5%, and oil refinery is come to be different from
With Ethylene vapor cracker mixed fraction isobutene.High-purity isobutene can be applied to fine chemicals, such as butyl rubber, poly- different
A variety of Organic chemical products such as butylene, methacrylate (MMA), tert-butyl mercaptan, tertiary butyl phenol, antioxidant, tert-butylamine, it is contemplated that
2018, the aggregate demand of the high-purity isobutene in the world was up to 2,600,000 tons, and market demand is huge.
The main supplier of the high-purity isobutene in the world is Lyondell Basell, Exxon Mobil, Texas at present
Petrochemicals (TPC), Russian Nizhnekamskneftehim companies (NKNK), Evonik, SUMITOMO CHEMICAL etc..Its
In except Lyondell Basell three grown places in the whole world device and company of Songyuan City of South Korea device using tert-butyl alcohol hydrolysis work
The high-purity isobutene of skill system, other devices use the high-purity isobutene of MTBE cracking technology systems mostly.Although MTBE cracking technology techniques
Maturation, but complex process, long flow path, vapor-phase thermal cracking, temperature are high, and cracking process easily generates dimethyl ether, and separating-purifying difficulty is big；If
For more, investment greatly, high energy consumption, production cost are high.Though tert-butyl alcohol hydrolysis process technological process is simple, equipment investment is low, technique bar
Part is gentle；But tert-butyl alcohol dehydration conversion per pass is low, total energy consumption is big, and production cost is also higher.
The existing technological process letter of high-purity isobutene technique is made in ethylene glycol mono-tert-butyl ether disclosed in this patent (ETB) cracking
Singly, the advantages that equipment investment is small, product is easily separated, there are low conversion per pass height, energy consumption, isobutene superior product quality, production again
The advantages such as cost is low；It is that one kind preferably prepares high-purity isobutene new technology.
Ethylene glycol mono-tert-butyl ether (ETB) is used as a kind of low photo-chemically reactive product simultaneously, can make in some fields
It is a kind of new environment-friendly type solvent to substitute the substitution solvent of butyl glycol ether (EB).Compared with EB, ETB has water solubility
The advantages such as well, latex dispersion stability is good, aqueous solution volatility is good, gentle to skin irritation, photo-chemically reactive is low；Can be wide
It is general to be applied to the fields such as coating, ink, family expenses cleaning agent.Therefore, this technique also may be used while high-purity isobutene product is produced
According to market situation, ETB international sales, aggrandizement apparatus income and anti-market risk ability are produced.
The content of the invention
For the high-purity isobutene complex manufacturing in China, high energy consumption, product separation is difficult, production cost is bigger than normal etc. asks
Topic, the present invention substitute methanol using higher boiling dihydric alcohol ethylene glycol, and high-purity isobutene and new can be produced simultaneously by developing one kind
The process of environmentally friendly solvent ethylene glycol mono-tert-butyl ether.The process has simple technological process, energy-conserving and environment-protective, product matter
Measure, the advantage such as equipment investment is small, production cost is low, there is very high application value and economic benefit.
The present invention concrete technical scheme be：
A kind of process for producing isobutene and ethylene glycol mono-tert-butyl ether, the technological process of production include：Etherificate
Three reaction member, ethylene glycol mono-tert-butyl ether product unit, high-purity isobutene product unit parts.
Described etherification reaction cellular manufacture processing step is as follows：
(1) the mixing carbon four containing isobutene is sent into the surge tank of carbon four, enters after the blended feed pump of carbon four boosting static mixed
Clutch is sufficiently mixed with ethylene glycol；
(2) virgin ethylene glycol and circulation and stress ethylene glycol are sent into ethylene glycol surge tank, are boosted through ethylene glycol feed pump laggard
Enter ethylene glycol clarifier, remove the ethylene glycol after trace impurity and be partly into static mixer and be sufficiently mixed with mixing carbon four,
Another part enter catalytic distillation top of tower with methyltertiarvbutyl ether reactor unreacted isobutene continue to react；
(3) ethylene glycol and mixing four preheated device of carbon after being sufficiently mixed enter fixed bed etherification after being heated to certain temperature
Reactor, under catalyst for etherification effect, mix most of isobutene in carbon four and glycol reaction generation ethylene glycol list uncle
Butyl ether or ethylene glycol dual-tert-butyl ether；
(4) reaction product of methyltertiarvbutyl ether reactor enters catalytic rectifying tower, and mixing carbon four by light component after rectifying enters
Tower top be equipped with catalyst for etherification conversion zone, mix carbon four in unreacted isobutene catalyst for etherification effect under with second two
Alcohol continues to react, and residual carbon four steams from tower top, and catalytic rectifying tower return tank, condensate liquid warp are entered after cycle condenser condenses
A catalytic rectifying tower reflux pump part is sent into tower top as phegma, and part product of carbon four after ether is taken out；Heavy constituent second two
Alcohol list tertbutyl ether crude product is after heat exchanger heat exchange cooling, into ethylene glycol mono-tert-butyl ether crude product surge tank.
The step (1) is characterized in that：It is 1%-90% to mix isobutene content in carbon four.
The step (2) is characterized in that：
Filling molecular sieve catalyst in ethylene glycol clarifier, it is main to remove water micro in ethylene glycol, reduce accessory substance uncle
The growing amount of butanol.
The step (3)：Ethylene glycol is ethylene glycol with mixing rubbing for isobutene in carbon four with mixing the charge proportion of carbon four
That ratio 1:0.5-2；Preheater preheating temperature is 30-80 DEG C；Etherification reaction temperature is 40-100 DEG C；Ethylene glycol feedstock quality air speed
For 0.5-3.0h-1；Etherification reaction pressure is 0.5-5.0Mpa；Isobutene conversion 80-95%；Etherification reaction catalyst type is
Modified strong acidic ion resin class catalyst, solid heteropoly acid class catalyst, modified molecular screen class catalyst, solid super-strong acid
One kind in class catalyst.
The step (4)：Catalytic distillation pressure tower is 0.5-1.5Mpa, and catalytic rectifying tower conversion zone reaction temperature is 40-
100 DEG C, the mol ratio of catalytic rectifying tower conversion zone ethylene glycol and isobutene is 1:0.5-2.0.
Ethylene glycol mono-tert-butyl ether product unit production craft step is as follows：
(1) a part of ethylene glycol mono-tert-butyl ether crude product in ethylene glycol mono-tert-butyl ether crude product surge tank, into second two
Alcohol list tertbutyl ether lightness-removing column rectifying, light component isobutene dimer, the tert-butyl alcohol are steamed from tower top；Bottom of towe heavy constituent enters de- double
Ether tower；
(2) ethylene glycol mono-tert-butyl ether lightness-removing column bottom of towe heavy constituent is formed after entering de- bis ether tower with the water entered in tower
Water-ethylene glycol list tertbutyl ether-ethylene glycol dual-tert-butyl ether azeotropic system, water-ethylene glycol list tertbutyl ether-second is steamed in tower top
Glycol dual-tert-butyl ether azeotropic mixture, enter phase separation tank after condensed；Bottom of towe heavy constituent enters ethylene glycol mono-tert-butyl ether knockout tower；
(3) oil phase in phase separation tank is entered in oil phase receiving tank by overflow, and the oil phase in oil phase receiving tank passes through oil phase
Tank discharging is pumped into cracking reactor reaction；Aqueous phase enters aqueous phase receiving tank from split-phase pot bottom, the water one in aqueous phase receiving tank
Part enters bis ether rectifying column through aqueous-phase reflux pump from tower, and another part realizes the recycling of water out of overhead reflux tower；
(4) take off bis ether tower bottom of towe heavy constituent and enter de- monoether tower continuation rectifying, ethylene glycol mono-tert-butyl ether is adopted from tower side line
Go out, be sent into ethylene glycol list tert-butyl group product storage tank, taken out as product；The condensed rear portion of light component is steamed from tower top to be sent into
Reflux in tower, a part are sent into phase separation tank；Bottom of towe heavy constituent ethylene glycol is sent into recovery ethylene glycol storage tank, recycles.
The step (1)：Ethylene glycol mono-tert-butyl ether lightness-removing column rectifying tower top temperature is 40-80 DEG C, and rectifying pressure is 10-
200kpa。
The step (2)：The mass ratio of entrainer water and ethylene glycol dual-tert-butyl ether is：1:0.1-5.0；Tower top temperature is
40-80 DEG C, rectifying pressure is 10-100kpa.
The step (4)：De- monoether column overhead temperatures are 80-150 DEG C, and rectifying pressure is 10-100kpa；Ethylene glycol list uncle
Butyl ether product content ＞ 99%, ethylene glycol content ＞ 99%.
High-purity isobutene product unit production craft step is as follows：
(1) cracking reactor preheater is entered after ethylene glycol mono-tert-butyl ether crude product mixes with the oil phase in oil phase receiving tank
After being heated to certain temperature, cracking reactor is sent into；Under the catalytic action of catalyst for cracking, ethylene glycol mono-tert-butyl ether and second
Cracking reaction occurs for glycol dual-tert-butyl ether, generates ethylene glycol and isobutene mixture；
(2) cracking reactor product enters ethylene glycol flash column, by light component and heavy constituent initial gross separation；
(3 ethylene glycol flash column light component tower tops enter isobutene weight-removing column rectification and purification, high-purity isobutene product after steaming
Steamed from tower top, high-purity isobutene product storage tank is sent into after condensation；Bottom of towe restructuring is distributed into the circulation of ethylene glycol flash column；
(4) ethylene glycol flash column heavy constituent enters ethylene glycol lightness-removing column and continues rectifying, and light component is from ethylene glycol lightness-removing column top
Steam, accessory substance storage tank is sent into after condensation；Bottom of towe restructuring is distributed into ethylene glycol weight-removing column；
(5) ethylene glycol lightness-removing column heavy constituent enters the continuation rectifying of ethylene glycol weight-removing column, and it is condensed to steam light component from tower top
Rear portion is sent into reflux in tower, and another part is sent into ethylene glycol recycling can and recycled, and is sent into after bottom of towe heavy constituent is condensed
Diethylene glycol (DEG) product storage tank.
Step (1) the cracking reactor preheating temperature is 60-200 DEG C, and cracking reaction temperature is 70-150 DEG C, and cracking is former
Expect that feedstock quality air speed is 0.5-3.0h-1, cleavage reaction pressure 0-0.5MPa, cracking reaction catalyst type is modified strong acid
Property resin cation class catalyst, solid heteropoly acid class catalyst, modified molecular screen class catalyst, solid super strong acids catalyst
In one kind.
The step (1)：The cracking reactor type is shell and tube reactor.
Embodiment
The embodiment of form by the following examples, the above of the present invention is done further specifically
It is bright, but the scope that this should not be interpreted as to the above-mentioned theme of the present invention is only limitted to following example.It is all to be based on the above of the present invention
The technology realized belongs to the scope of the present invention.
Embodiment 1
By the mixing raw material of carbon four that isobutene content is 30% and the 99% ethylene glycol raw material by purification utensil, press
Ethylene glycol and isobutene mol ratio 1.5:After 1 is sufficiently mixed, then by preheater it is preheated to 75 DEG C；It is in reaction pressure
1.5MPa, reaction temperature are 80 DEG C, and quality of glycol air speed is 2.0h-1Reaction condition under, the raw material after preheating is by being loaded with
The fixed bed reactors of catalyst for etherification, isobutene and the glycol reaction generation ethylene glycol list tert-butyl group in catalytic mixing carbon four
Ether or ethylene glycol dual-tert-butyl ether.The isobutene content ＜ 4%, isobutene conversion ＞ in carbon four are mixed after this section reaction
90%.
Reaction product is sent into catalytic rectifying tower, mixing carbon four by light component after rectifying enters tower top equipped with etherificate
The conversion zone of catalyst, mix unreacted isobutene in carbon four and continue to react with ethylene glycol under catalyst for etherification effect, protect
Hold catalytic distillation pressure tower 1.0MPa, 80 DEG C of tower top conversion zone temperature, ethylene glycol and unreacted isobutene mol ratio 1.5:1, make
Isobutene in mixing carbon four fully reacts, isobutene content ＜ 0.4%, isobutene conversion ＞ in residue mixing carbon four
99%.The product of carbon four is taken out after residual carbon four is steamed from tower top again after condensing when ether.Heavy constituent ethylene glycol mono-tert-butyl ether is thick
Product, into ethylene glycol mono-tert-butyl ether crude product surge tank, obtain ethylene glycol mono-tert-butyl ether crude product after heat exchanger heat exchange cooling.
A part of ethylene glycol mono-tert-butyl ether crude product is sent into ethylene glycol mono-tert-butyl ether lightness-removing column, in rectifying pressure
100KPa, the accessory substances such as light component isobutene dimer, the tert-butyl alcohol are produced under the conditions of 70 DEG C of tower top temperature.Again by bottom of towe heavy constituent
De- bis ether tower is sent into, while it is 1 to add with ethylene glycol dual-tert-butyl ether mass ratio in heavy constituent:1 water is as entrainer, in essence
Evaporate pressure 50KPa, 50 DEG C of condition extraction ethylene glycol dual-tert-butyl ethers of tower top temperature and water, the azeotropic of ethylene glycol mono-tert-butyl ether
Thing.Bottom of towe restructuring is distributed into de- monoether tower again, under the conditions of rectifying pressure 20KPa, 100 DEG C of tower top temperature, the side line from tower
Produce content ＞ 99% ethylene glycol mono-tert-butyl ether product.Product index parameter is as shown in the table：
After a part of preheated device of ethylene glycol mono-tert-butyl ether crude product is preheated into 150 DEG C, in reaction pressure 0.1MPa, instead
It is 2.0h to answer 150 DEG C of temperature, cracking stock feedstock quality air speed-1Under the conditions of pass through the shell and tube reactor equipped with catalyst for cracking
Cracking reaction is carried out, generates isobutene and ethylene glycol mixture；Isobutene in mixture is separated by ethylene glycol flash column,
High-purity isobutene product is obtained after the purification of isobutene weight-removing column, high-purity isobutene product index is as shown in the table：
| Sequence number | Title | Testing index |
| 1 | Isobutene | 99.95% |
| 2 | Iso-butane | 150ppm |
| 3 | Butene-1 | 8ppm |
| 4 | Maleic -2 | 20ppm |
| 5 | The tert-butyl alcohol | 5ppm |
| 6 | Water | 5ppm |
| 7 | Ethylene glycol | 1ppm |
| 8 | Sulphur | 1mg/m3 |
| 9 | Dimer | 5ppm |
Embodiment 2
By the mixing raw material of carbon four that isobutene content is 50% and the 99% ethylene glycol raw material by purification utensil, press
Ethylene glycol and isobutene mol ratio 1.5:After 1 is sufficiently mixed, then by preheater it is preheated to 75 DEG C；It is in reaction pressure
1.5MPa, reaction temperature are 80 DEG C, and quality of glycol air speed is 2.0h-1Reaction condition under, the raw material after preheating is by being loaded with
The fixed bed reactors of catalyst for etherification, isobutene and the glycol reaction generation ethylene glycol list tert-butyl group in catalytic mixing carbon four
Ether or ethylene glycol dual-tert-butyl ether.The isobutene content ＜ 6%, isobutene conversion ＞ in carbon four are mixed after this section reaction
90%.
Reaction product is sent into catalytic rectifying tower, mixing carbon four by light component after rectifying enters tower top equipped with etherificate
The conversion zone of catalyst, mix unreacted isobutene in carbon four and continue to react with ethylene glycol under catalyst for etherification effect, protect
Hold catalytic distillation pressure tower 1.0MPa, 80 DEG C of tower top conversion zone temperature, ethylene glycol and unreacted isobutene mol ratio 1.5:1, make
Isobutene in mixing carbon four fully reacts, isobutene content ＜ 0.4%, isobutene conversion ＞ in residue mixing carbon four
99%.The product of carbon four is taken out after residual carbon four is steamed from tower top again after condensing when ether.Heavy constituent ethylene glycol mono-tert-butyl ether is thick
Product, into ethylene glycol mono-tert-butyl ether crude product surge tank, obtain ethylene glycol mono-tert-butyl ether crude product after heat exchanger heat exchange cooling.
A part of ethylene glycol mono-tert-butyl ether crude product is sent into ethylene glycol mono-tert-butyl ether lightness-removing column, in rectifying pressure
100KPa, the accessory substances such as light component isobutene dimer, the tert-butyl alcohol are produced under the conditions of 70 DEG C of tower top temperature.Again by bottom of towe heavy constituent
De- bis ether tower is sent into, while it is 1 to add with ethylene glycol dual-tert-butyl ether mass ratio in heavy constituent:1 water is as entrainer, in essence
Evaporate pressure 50KPa, 50 DEG C of condition extraction ethylene glycol dual-tert-butyl ethers of tower top temperature and water, the azeotropic of ethylene glycol mono-tert-butyl ether
Thing.Bottom of towe restructuring is distributed into de- monoether tower again, under the conditions of rectifying pressure 20KPa, 100 DEG C of tower top temperature, the side line from tower
Produce content ＞ 99% ethylene glycol mono-tert-butyl ether product.Product index parameter is as shown in the table：
After a part of preheated device of ethylene glycol mono-tert-butyl ether crude product is preheated into 150 DEG C, in reaction pressure 0.1MPa, instead
It is 2.0h to answer 150 DEG C of temperature, cracking stock feedstock quality air speed-1Under the conditions of pass through the shell and tube reactor equipped with catalyst for cracking
Cracking reaction is carried out, generates isobutene and ethylene glycol mixture；Isobutene in mixture is separated by ethylene glycol flash column,
High-purity isobutene product is obtained after the purification of isobutene weight-removing column, high-purity isobutene product index is as shown in the table：
| Sequence number | Title | Testing index |
| 1 | Isobutene | 99.92% |
| 2 | Iso-butane | 180ppm |
| 3 | Butene-1 | 8ppm |
| 4 | Maleic -2 | 20ppm |
| 5 | The tert-butyl alcohol | 5ppm |
| 6 | Water | 8ppm |
| 7 | Ethylene glycol | 1ppm |
| 8 | Sulphur | 1mg/m3 |
| 9 | Dimer | 6ppm |
Embodiment 3
By the mixing raw material of carbon four that isobutene content is 70% and the 99% ethylene glycol raw material by purification utensil, press
Ethylene glycol and isobutene mol ratio 1.5:After 1 is sufficiently mixed, then by preheater it is preheated to 75 DEG C；It is in reaction pressure
1.5MPa, reaction temperature are 80 DEG C, and quality of glycol air speed is 2.0h-1Reaction condition under, the raw material after preheating is by being loaded with
The fixed bed reactors of catalyst for etherification, isobutene and the glycol reaction generation ethylene glycol list tert-butyl group in catalytic mixing carbon four
Ether or ethylene glycol dual-tert-butyl ether.The isobutene content ＜ 8%, isobutene conversion ＞ in carbon four are mixed after this section reaction
90%.
Reaction product is sent into catalytic rectifying tower, mixing carbon four by light component after rectifying enters tower top equipped with etherificate
The conversion zone of catalyst, mix unreacted isobutene in carbon four and continue to react with ethylene glycol under catalyst for etherification effect, protect
Hold catalytic distillation pressure tower 1.0MPa, 80 DEG C of tower top conversion zone temperature, ethylene glycol and unreacted isobutene mol ratio 1.5:1, make
Isobutene in mixing carbon four fully reacts, isobutene content ＜ 0.4%, isobutene conversion ＞ in residue mixing carbon four
99%.The product of carbon four is taken out after residual carbon four is steamed from tower top again after condensing when ether.Heavy constituent ethylene glycol mono-tert-butyl ether is thick
Product, into ethylene glycol mono-tert-butyl ether crude product surge tank, obtain ethylene glycol mono-tert-butyl ether crude product after heat exchanger heat exchange cooling.
A part of ethylene glycol mono-tert-butyl ether crude product is sent into ethylene glycol mono-tert-butyl ether lightness-removing column, in rectifying pressure
100KPa, the accessory substances such as light component isobutene dimer, the tert-butyl alcohol are produced under the conditions of 70 DEG C of tower top temperature.Again by bottom of towe heavy constituent
De- bis ether tower is sent into, while it is 1 to add with ethylene glycol dual-tert-butyl ether mass ratio in heavy constituent:1 water is as entrainer, in essence
Evaporate pressure 50KPa, 50 DEG C of condition extraction ethylene glycol dual-tert-butyl ethers of tower top temperature and water, the azeotropic of ethylene glycol mono-tert-butyl ether
Thing.Bottom of towe restructuring is distributed into de- monoether tower again, under the conditions of rectifying pressure 20KPa, 100 DEG C of tower top temperature, the side line from tower
Produce content ＞ 99% ethylene glycol mono-tert-butyl ether product.Product index parameter is as shown in the table：
After a part of preheated device of ethylene glycol mono-tert-butyl ether crude product is preheated into 150 DEG C, in reaction pressure 0.1MPa, instead
It is 2.0h to answer 150 DEG C of temperature, cracking stock feedstock quality air speed-1Under the conditions of pass through the shell and tube reactor equipped with catalyst for cracking
Cracking reaction is carried out, generates isobutene and ethylene glycol mixture；Isobutene in mixture is separated by ethylene glycol flash column,
High-purity isobutene product is obtained after the purification of isobutene weight-removing column, high-purity isobutene product index is as shown in the table：
| Sequence number | Title | Testing index |
| 1 | Isobutene | 99.98% |
| 2 | Iso-butane | 120ppm |
| 3 | Butene-1 | 5ppm |
| 4 | Maleic -2 | 20ppm |
| 5 | The tert-butyl alcohol | 5ppm |
| 6 | Water | 6ppm |
| 7 | Ethylene glycol | 1ppm |
| 8 | Sulphur | 1mg/m3 |
| 9 | Dimer | 4ppm |
Embodiment 4
By the mixing raw material of carbon four that isobutene content is 30% and the 99% ethylene glycol raw material by purification utensil, press
Ethylene glycol and isobutene mol ratio 2.0:After 1 is sufficiently mixed, then by preheater it is preheated to 75 DEG C；It is in reaction pressure
1.5MPa, reaction temperature are 80 DEG C, and quality of glycol air speed is 2.0h-1Reaction condition under, the raw material after preheating is by being loaded with
The fixed bed reactors of catalyst for etherification, isobutene and the glycol reaction generation ethylene glycol list tert-butyl group in catalytic mixing carbon four
Ether or ethylene glycol dual-tert-butyl ether.The isobutene content ＜ 3%, isobutene conversion ＞ in carbon four are mixed after this section reaction
92%.
Reaction product is sent into catalytic rectifying tower, mixing carbon four by light component after rectifying enters tower top equipped with etherificate
The conversion zone of catalyst, mix unreacted isobutene in carbon four and continue to react with ethylene glycol under catalyst for etherification effect, protect
Hold catalytic distillation pressure tower 1.0MPa, 80 DEG C of tower top conversion zone temperature, ethylene glycol and unreacted isobutene mol ratio 1.5:1, make
Isobutene in mixing carbon four fully reacts, isobutene content ＜ 0.4%, isobutene conversion ＞ in residue mixing carbon four
99%.The product of carbon four is taken out after residual carbon four is steamed from tower top again after condensing when ether.Heavy constituent ethylene glycol mono-tert-butyl ether is thick
Product, into ethylene glycol mono-tert-butyl ether crude product surge tank, obtain ethylene glycol mono-tert-butyl ether crude product after heat exchanger heat exchange cooling.
A part of ethylene glycol mono-tert-butyl ether crude product is sent into ethylene glycol mono-tert-butyl ether lightness-removing column, in rectifying pressure
100KPa, the accessory substances such as light component isobutene dimer, the tert-butyl alcohol are produced under the conditions of 70 DEG C of tower top temperature.Again by bottom of towe heavy constituent
De- bis ether tower is sent into, while it is 1 to add with ethylene glycol dual-tert-butyl ether mass ratio in heavy constituent:1 water is as entrainer, in essence
Evaporate pressure 50KPa, 50 DEG C of condition extraction ethylene glycol dual-tert-butyl ethers of tower top temperature and water, the azeotropic of ethylene glycol mono-tert-butyl ether
Thing.Bottom of towe restructuring is distributed into de- monoether tower again, under the conditions of rectifying pressure 20KPa, 100 DEG C of tower top temperature, the side line from tower
Produce content ＞ 99% ethylene glycol mono-tert-butyl ether product.Product index parameter is as shown in the table：
After a part of preheated device of ethylene glycol mono-tert-butyl ether crude product is preheated into 150 DEG C, in reaction pressure 0.1MPa, instead
It is 2.0h to answer 150 DEG C of temperature, cracking stock feedstock quality air speed-1Under the conditions of pass through the shell and tube reactor equipped with catalyst for cracking
Cracking reaction is carried out, generates isobutene and ethylene glycol mixture；Isobutene in mixture is separated by ethylene glycol flash column,
High-purity isobutene product is obtained after the purification of isobutene weight-removing column, high-purity isobutene product index is as shown in the table：
| Sequence number | Title | Testing index |
| 1 | Isobutene | 99.94% |
| 2 | Iso-butane | 200ppm |
| 3 | Butene-1 | 5ppm |
| 4 | Maleic -2 | 30ppm |
| 5 | The tert-butyl alcohol | 6ppm |
| 6 | Water | 8ppm |
| 7 | Ethylene glycol | 1ppm |
| 8 | Sulphur | 1mg/m3 |
| 9 | Dimer | 9ppm |
Embodiment 5
By the mixing raw material of carbon four that isobutene content is 30% and the 99% ethylene glycol raw material by purification utensil, press
Ethylene glycol and isobutene mol ratio 1.5:After 1 is sufficiently mixed, then by preheater it is preheated to 75 DEG C；It is in reaction pressure
2.0MPa, reaction temperature are 80 DEG C, and quality of glycol air speed is 2.0h-1Reaction condition under, the raw material after preheating is by being loaded with
The fixed bed reactors of catalyst for etherification, isobutene and the glycol reaction generation ethylene glycol list tert-butyl group in catalytic mixing carbon four
Ether or ethylene glycol dual-tert-butyl ether.The isobutene content ＜ 4%, isobutene conversion ＞ in carbon four are mixed after this section reaction
90%.
Reaction product is sent into catalytic rectifying tower, mixing carbon four by light component after rectifying enters tower top equipped with etherificate
The conversion zone of catalyst, mix unreacted isobutene in carbon four and continue to react with ethylene glycol under catalyst for etherification effect, protect
Hold catalytic distillation pressure tower 1.0MPa, 80 DEG C of tower top conversion zone temperature, ethylene glycol and unreacted isobutene mol ratio 1.5:1, make
Isobutene in mixing carbon four fully reacts, isobutene content ＜ 0.4%, isobutene conversion ＞ in residue mixing carbon four
99%.The product of carbon four is taken out after residual carbon four is steamed from tower top again after condensing when ether.Heavy constituent ethylene glycol mono-tert-butyl ether is thick
Product, into ethylene glycol mono-tert-butyl ether crude product surge tank, obtain ethylene glycol mono-tert-butyl ether crude product after heat exchanger heat exchange cooling.
A part of ethylene glycol mono-tert-butyl ether crude product is sent into ethylene glycol mono-tert-butyl ether lightness-removing column, in rectifying pressure
100KPa, the accessory substances such as light component isobutene dimer, the tert-butyl alcohol are produced under the conditions of 70 DEG C of tower top temperature.Again by bottom of towe heavy constituent
De- bis ether tower is sent into, while it is 1 to add with ethylene glycol dual-tert-butyl ether mass ratio in heavy constituent:1 water is as entrainer, in essence
Evaporate pressure 50KPa, 50 DEG C of condition extraction ethylene glycol dual-tert-butyl ethers of tower top temperature and water, the azeotropic of ethylene glycol mono-tert-butyl ether
Thing.Bottom of towe restructuring is distributed into de- monoether tower again, under the conditions of rectifying pressure 20KPa, 100 DEG C of tower top temperature, the side line from tower
Produce content ＞ 99% ethylene glycol mono-tert-butyl ether product.Product index parameter is as shown in the table：
After a part of preheated device of ethylene glycol mono-tert-butyl ether crude product is preheated into 150 DEG C, in reaction pressure 0.1MPa, instead
It is 2.0h to answer 180 DEG C of temperature, cracking stock feedstock quality air speed-1Under the conditions of pass through the shell and tube reactor equipped with catalyst for cracking
Cracking reaction is carried out, generates isobutene and ethylene glycol mixture；Isobutene in mixture is separated by ethylene glycol flash column,
High-purity isobutene product is obtained after the purification of isobutene weight-removing column, high-purity isobutene product index is as shown in the table：
Claims (10)
- A kind of 1. process for producing isobutene and ethylene glycol mono-tert-butyl ether, it is characterised in that：The technological process of production Including：Three etherification reaction unit, ethylene glycol mono-tert-butyl ether product unit, high-purity isobutene product unit parts.
- 2. the process of production isobutene and ethylene glycol mono-tert-butyl ether as claimed in claim 1, it is characterised in that：Described Etherification reaction cellular manufacture processing step is as follows：(1) the mixing carbon four containing isobutene is sent into the surge tank of carbon four, enters static mixer after the blended feed pump of carbon four boosting It is sufficiently mixed with ethylene glycol；(2) virgin ethylene glycol and circulation and stress ethylene glycol are sent into ethylene glycol surge tank, enter second after the boosting of ethylene glycol feed pump Glycol clarifier, remove the ethylene glycol after trace impurity and be partly into static mixer and be sufficiently mixed with mixing carbon four, it is another Part enter catalytic distillation top of tower with methyltertiarvbutyl ether reactor unreacted isobutene continue to react；(3) ethylene glycol and mixing four preheated device of carbon after being sufficiently mixed enter fixed bed etherification reaction after being heated to certain temperature Device, under catalyst for etherification effect, mix most of isobutene and the glycol reaction generation ethylene glycol list tert-butyl group in carbon four Ether or ethylene glycol dual-tert-butyl ether；(4) reaction product of methyltertiarvbutyl ether reactor enters catalytic rectifying tower, and mixing carbon four by light component after rectifying enters on tower Portion be equipped with catalyst for etherification conversion zone, mix carbon four in unreacted isobutene catalyst for etherification effect under with ethylene glycol after Continuous reaction, residual carbon four steam from tower top, catalytic rectifying tower return tank are entered after cycle condenser condenses, condensate liquid is through catalysis A rectifier column reflux pump part is sent into tower top as phegma, and part product of carbon four after ether is taken out；Heavy constituent ethylene glycol list Tertbutyl ether crude product is after heat exchanger heat exchange cooling, into ethylene glycol mono-tert-butyl ether crude product surge tank.
- 3. the process of production isobutene and ethylene glycol mono-tert-butyl ether as claimed in claim 1 or 2, it is characterised in that：Second Glycol list tertbutyl ether product unit production craft step is as follows：(1) a part of ethylene glycol mono-tert-butyl ether crude product in ethylene glycol mono-tert-butyl ether crude product surge tank, into ethylene glycol list Tertbutyl ether lightness-removing column rectifying, light component isobutene dimer, the tert-butyl alcohol are steamed from tower top；Bottom of towe heavy constituent enters de- bis ether Tower；(2) ethylene glycol mono-tert-butyl ether lightness-removing column bottom of towe heavy constituent enters after de- bis ether tower forms water-second with the water entered in tower Glycol list tertbutyl ether-ethylene glycol dual-tert-butyl ether azeotropic system, water-ethylene glycol list tertbutyl ether-ethylene glycol is steamed in tower top Dual-tert-butyl ether azeotropic mixture, enter phase separation tank after condensed；Bottom of towe heavy constituent enters ethylene glycol mono-tert-butyl ether knockout tower；(3) oil phase in phase separation tank is entered in oil phase receiving tank by overflow, and the oil phase in oil phase receiving tank goes out by oil phase tank Material is pumped into cracking reactor reaction；Aqueous phase enters aqueous phase receiving tank from split-phase pot bottom, the water part in aqueous phase receiving tank Enter bis ether rectifying column from tower through aqueous-phase reflux pump, another part realizes the recycling of water out of overhead reflux tower；(4) take off bis ether tower bottom of towe heavy constituent and enter de- monoether tower continuation rectifying, ethylene glycol mono-tert-butyl ether is sent from tower side take-off Enter ethylene glycol list tert-butyl group product storage tank, taken out as product；The condensed rear portion of light component is steamed from tower top to be sent into tower Backflow, a part are sent into phase separation tank；Bottom of towe heavy constituent ethylene glycol is sent into recovery ethylene glycol storage tank, recycles.
- 4. the process of production isobutene and ethylene glycol mono-tert-butyl ether as claimed in claim 1 or 2, it is characterised in that：It is high Pure isobutene product unit production craft step is as follows：(1) enter cracking reactor preheater after ethylene glycol mono-tert-butyl ether crude product mixes with the oil phase in oil phase receiving tank to heat To certain temperature, cracking reactor is sent into；Under the catalytic action of catalyst for cracking, ethylene glycol mono-tert-butyl ether and ethylene glycol Cracking reaction occurs for dual-tert-butyl ether, generates ethylene glycol and isobutene mixture；(2) cracking reactor product enters ethylene glycol flash column, by light component and heavy constituent initial gross separation；(3 ethylene glycol flash column light component tower tops enter isobutene weight-removing column rectification and purification after steaming, high-purity isobutene product is from tower Top is steamed, and high-purity isobutene product storage tank is sent into after condensation；Bottom of towe restructuring is distributed into the circulation of ethylene glycol flash column；(4) ethylene glycol flash column heavy constituent enters the continuation rectifying of ethylene glycol lightness-removing column, and light component steams from ethylene glycol lightness-removing column top, Accessory substance storage tank is sent into after condensation；Bottom of towe restructuring is distributed into ethylene glycol weight-removing column；(5) ethylene glycol lightness-removing column heavy constituent enters the continuation rectifying of ethylene glycol weight-removing column, and it is condensed latter to steam light component from tower top Reflux in tower is sent into part, and another part is sent into ethylene glycol recycling can and recycled, and it is sweet to be sent into two after bottom of towe heavy constituent is condensed Alcohol product storage tank.
- 5. the process of production isobutene and ethylene glycol mono-tert-butyl ether as claimed in claim 2, described its feature of step (1) It is：It is 1%-90% to mix isobutene content in carbon four.
- 6. the process of the production isobutene and ethylene glycol mono-tert-butyl ether as claimed in claim 2, it is characterised in that institute State step (2)：Filling molecular sieve catalyst in ethylene glycol clarifier, it is main to remove water micro in ethylene glycol, reduce the accessory substance tert-butyl alcohol Growing amount；The step (3)：Ethylene glycol is mol ratio of the ethylene glycol with mixing isobutene in carbon four with the charge proportion for mixing carbon four 1:0.5-2；Preheater preheating temperature is 30-80 DEG C；Etherification reaction temperature is 40-100 DEG C；Ethylene glycol feedstock quality air speed is 0.5-3.0h-1；Etherification reaction pressure is 0.5-5.0Mpa；Isobutene conversion 80-95%；Etherification reaction catalyst type is to change Property strong acidic ion resin class catalyst, solid heteropoly acid class catalyst, modified molecular screen class catalyst, solid super strong acids One kind in catalyst；The step (4)：Catalytic distillation pressure tower is 0.5-1.5Mpa, and catalytic rectifying tower conversion zone reaction temperature is 40-100 DEG C, the mol ratio of catalytic rectifying tower conversion zone ethylene glycol and isobutene is 1:0.5-2.0.
- 7. the process of the production isobutene and ethylene glycol mono-tert-butyl ether as claimed in claim 3, it is characterised in that：Institute Step (1) ethylene glycol mono-tert-butyl ether lightness-removing column rectifying tower top temperature is stated as 40-80 DEG C, rectifying pressure is 10-200kpa；The mass ratio of step (2) the entrainer water and ethylene glycol dual-tert-butyl ether is：1:0.1-5.0；Tower top temperature is 40-80 DEG C, rectifying pressure is 10-100kpa.
- 8. as claimed in claim 3 it is described production isobutene and ethylene glycol mono-tert-butyl ether process, the step (4) its It is characterised by：De- monoether column overhead temperatures are 80-150 DEG C, and rectifying pressure is 10-100kpa；Ethylene glycol mono-tert-butyl ether product Content ＞ 99%, ethylene glycol content ＞ 99%.
- 9. as claimed in claim 4 it is described production isobutene and ethylene glycol mono-tert-butyl ether process, the step (1) its It is characterised by：Cracking reactor preheating temperature is 60-200 DEG C, and cracking reaction temperature is 70-150 DEG C, cracking stock feedstock quality Air speed is 0.5-3.0h-1, cleavage reaction pressure 0-0.5MPa, cracking reaction catalyst type is modified highly acidic cation tree One kind in lipid catalyst, solid heteropoly acid class catalyst, modified molecular screen class catalyst, solid super strong acids catalyst.
- 10. the process of the production isobutene and ethylene glycol mono-tert-butyl ether as claimed in claim 4, the step (1) It is characterized in that：The cracking reactor type is shell and tube reactor.
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| CN110759817A (en) * | 2018-07-27 | 2020-02-07 | 中国石油化工股份有限公司 | Preparation method of ethylene glycol mono-tert-butyl ether |
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| 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 |
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