CN107032969A - The technique that a kind of liquid-phase oxidation of toluene prepares benzaldehyde - Google Patents
The technique that a kind of liquid-phase oxidation of toluene prepares benzaldehyde Download PDFInfo
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- CN107032969A CN107032969A CN201710379040.5A CN201710379040A CN107032969A CN 107032969 A CN107032969 A CN 107032969A CN 201710379040 A CN201710379040 A CN 201710379040A CN 107032969 A CN107032969 A CN 107032969A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
- C07C45/32—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
- C07C45/33—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties
- C07C45/34—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties in unsaturated compounds
- C07C45/36—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties in unsaturated compounds in compounds containing six-membered aromatic rings
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C45/82—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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Abstract
The invention discloses the technique that a kind of liquid-phase oxidation of toluene prepares benzaldehyde, comprise the technical steps that：1) workshop section is reacted；2) centrifugal station；Final major product benzaldehyde is from the overhead extraction of rectifying column 3, and purity reaches more than 97%, and other a small amount of blending ingredients flow out from the tower reactor of rectifying column 3；3) vent gas treatment workshop section.
Description
Technical field
The invention belongs to technical field of fine, and in particular to the technique that a kind of liquid-phase oxidation of toluene prepares benzaldehyde.
Background technology
The molecular formula of benzaldehyde (Benzaldehyde) is C7H6O, color typically shows yellow or colourless, belongs to one
The liquid of oily is planted, its volatility is very strong, with high refractivity, the smell distributed is bitter benevolence apricot smell, is commonly referred to as
Almond oil, it is flammable, there is fragranced during burning.Benzaldehyde belongs to critically important aromatic aldehyde in the industry, with grape sugar form
It is present in nature.It can be with very many immiscible organic solvents such as ethanol, ether, benzene and chloroform etc..Benzaldehyde is nontoxic, its steaming
Vapour anaesthetizes to obtain function as mild as a dove.Benzaldehyde, which is easy to be oxidized by oxygen into atmosphere under benzoic acid, alkaline environment, to be added
Fast benzaldehyde autoxidation, phenols, a species of orchid, sulphur, iodine and the effect for playing suppression to the oxidation of benzaldehyde to inhibitor such as hydroquinones.Benzene first
There is an active group of base in aldehyde molecule, and the carbon-oxygen bond of group base polarizes because of II bonding electrons density toward the skew of oxygen direction is easy, therefore benzene
Formaldehyde can carry out many chemical reactions, and such as nucleophilic addition is condensed through aldehyde, nitrification, the serial reaction such as chlorination, can derive many chemical industry
Product, it is widely used in the industries such as medicine, spices, agricultural chemicals, dyestuff, it is resin, oils, some cellulose ethers, acetic acid and nitre
The solvent of acid cellulose.
With the extensive use of benzaldehyde, the production to benzaldehyde both at home and abroad is also increasingly paid attention to, thing followed system
The method of standby benzaldehyde is also more and more, and the also more and more higher of the requirement to the method for preparation, now production benzaldehyde
Method mainly has two major classes：Toluene oxidation method and chlorination toluene Hydrolyze method.Toluene oxidation method is divided into：Gas phase oxidation of toluene method and first
Benzene liquid phase oxidation；Chlorination toluene Hydrolyze method is divided into again：Benzyl alcohol oxidation method and benzyl chloride Hydrolyze method.
(1) benzyl alcohol oxidation producing benzaldehyde
Wu Xingan, Chen Shu cuts down the synthesis of benzoic acid and refined [J] modern chemical industries, 2000,20 (8):10-14. phenmethylols
Preparing benzaldehyde by oxidizing is by made from toluene and the mutual hydrolysis oxidation of monochlor(in)ate materialization benzyl.This method is industrially used
Oxidant is merely not only to use NaZCrZO, and can also use hydrogen peroxide and sodium hypochlorite, and these are also good selection.
But still required cost is too high quickly for this method speed of production so that the use value mistake for the benzaldehyde produced
It is low, so the utilization rate in industry greatly reduces.
(2) chlorination toluene Hydrolyze method
Beautiful temperate conditions Toluene selective oxidation prepares benzaldehyde [D] Nanjing University, 2014. and Qin H to face long
F.Research Progress of FluorobenzaldehydeSynthesis[J].Anhui Chemical
Industry, 2009. this method are toluene and chlorine reaction is obtained after some chlorides after the hydrolysis of acid-base property by essence
Evaporate purification and obtain benzaldehyde.After the completion of reaction, the benzaldehyde content that obtained product is obtained by rectification and purification can reach
95%-98%.The advantage for changing method is that the recovery content of benzaldehyde is very high, has the disadvantage that production line and process are very complicated,
The benzaldehyde produced contains chlorine, and purity is lowered by, and this causes the purposes for the benzaldehyde produced greatly reducing,
And equipment is by serious corrosion, cost is added, the accessory substance of production has very big pollution to environment, and institute is in this way by state
Family prohibits the use of.
(3) gas phase oxidation of toluene producing benzaldehyde
Research [J] the Heilungkiang scientific and technological information of Pan Ying duckweed toluene catalytic oxidation synthesizing benzaldehydes, 2016 (5):41-41.
And research [D] the Hunan Normal University of Li Yongqiang toluene liquid phase catalytic oxidations reaction, 2014. and Zhou W, Huang
K, Cao M, et al.Selective oxidation of toluene to benzaldehyde in liquid phase
over CoAl oxides prepared from hydrotalcite-like precursors[J].Reaction
Kinetics, Mechanisms and Catalysis, 2015,115 (1):1-13. formaldehyde be by toluene be reactant, oxygen
Gas generates benzaldehyde, the oxidation of this method as oxidant by the way that catalytic oxidation occurs under the catalyst and high temperature of solid
Agent except with oxygen or air and ozone, and catalyst generally from some activity and selectivities very high metal and
Based on metal oxide, it is main be this method except obtaining free from chloride benzaldehyde, phenmethylol and benzoic acid etc. can also be obtained
Many kinds of substance.It is most of in simulation process to use fixed bed and fluidized bed processes, and mainly have raw material cheap and
It is readily obtained, operating process is uncomplicated, relatively easy, course of reaction is also very fast, it is easy to multiple continuous and automatic, it is resulting
Product be very environmental protection without chlorine product, considerably increase the use approach of production thing, but course of reaction is more multiple
Miscellaneous, used reaction condition is also difficult to be met, and last product species excessively greatly improve the difficulty of separating-purifying, increase
Production cost, and be difficult to the conversion ratio that improves toluene, institute is difficult to operate and made in now industrial in this way
With.
(4) liquid-phase oxidation of toluene producing benzaldehyde
Liquid-phase oxidation of toluene producing benzaldehyde method refers to that reaction product is toluene, and air or oxygen are used as oxidant, acetic acid
Cobalt is catalyst, liquid-phase catalytic oxidation is carried out under certain temperature and pressure, reaction product is mainly by benzaldehyde, benzene first
Acid and phenmethylol, and different reaction product (Guo Fei toluene oxidation producing benzaldehydes can be obtained by controlling reaction condition
Bubble column slurry reactor is simulated and heat [D] East China University of Science, 2013. and Yao Yao toluene liquid-phases selectivity oxygen
Change research [D] the East China University of Science of producing benzaldehyde, 2013.).
Liquid-phase oxidation of toluene has the advantages that mild condition, easy controlled operation, pollutant be few, high income.Benzaldehyde is not chloride,
Use value and scope are very high, and production cost greatly reduces as oxidant in air, are a kind of in this way
The process of new green environment protection.The advantage that liquid-phase oxidation of toluene prepares benzaldehyde each side is all very big, is well suited as one
Plant the new process for meeting megatrend.
In the prior art, benzyl alcohol oxidation producing benzaldehyde, complex process, it is impossible to realize industrialization, expensive starting materials are rare, receive
Rate is low, and accessory substance is complicated, and principal product is chloride, purity is not high, and equipment investment is big；
Chlorination toluene hydrolyzes producing benzaldehyde, and technics comparing is ripe but complicated difficult is manipulated, and raw material is easy to get cheaply, and yield compares
Height, accessory substance is complicated, have pollution, and principal product is chloride, purity is not high, and equipment is easily corroded, and invests many；
Gas phase oxidation of toluene producing benzaldehyde, technique is simple to operation, and raw material is easy to get cheaply, and yield is than relatively low, and accessory substance is multiple
Miscellaneous, principal product is not chloride, and purity is high, and equipment is easily corroded, small investment.
In today's society, more and more using the demand of tolyl aldehyde in industry, pharmaceutical sector and foodstuff flavouring industry, quilt
The scope of application is also increasingly wider, is shown according to data survey, and China's benzaldehyde demand is increased with annual more than 7% speed
It is long, and also need a large amount of import benzaldehydes to meet domestic demands every year.Also having many plants in nature, there is also have benzene first
Aldehyde, so with the development of society, people are to high accuracy, the demand without chloride benzaldehyde is also gradually increased, but it
The process of preceding ancient production benzaldehyde is all the main method hydrolyzed by chlorination toluene to extract production, this method
But there are many weak points：Productivity ratio is low, and product contains a variety of byproducts such as chlorine, causes the pollution of environment and the corrosion ratio of equipment
More serious, the tolyl aldehyde of production does not simultaneously meet using for food and medicine industry.Institute is in this way substantially by social cleaning
, therefore a kind of pollution-free, high conversion rate of research, green technological process simple and easy to apply is necessary.Using air as oxygen
Agent, it is a kind of very advanced, environmental protection that cobalt prepares benzaldehyde for the liquid-phase oxidation of toluene of catalyst, operates uncomplicated, life
Produce the low process of cost.This method has development prospect very much, have to the production of benzaldehyde very big industrial utilization with
Researching value.
With the fast development of social economy, industry-by-industry is also run forward at full speed, particularly cosmetics, food
The development of the industry volcano eruption formula such as product, medicine, to more and more, the requirement in matter in the required benzaldehyde amount of being not only
More and more higher, the requirement of benzaldehyde matter is mainly reflected in：Purity requirement more and more higher, chlorinty is more and more lower, preferably chloride
Amount is zero.So the development prospect of benzaldehyde is immeasurable, it is impossible to can substitute it in industry-by-industry with anything else
Status.And liquid-phase oxidation of toluene prepares the technique side that benzaldehyde is a benzaldehyde for meeting every profession and trade demand that can have been produced
Method, so research of the people to it is also only more and more deep.
Initially, MnO2It is that liquid-phase oxidation of toluene prepares the most frequently used catalysis of benzaldehyde with the dilution heat of sulfuric acid that solvent is 65%
Agent, reaction temperature is is produced at 40 DEG C, but this method is eliminated due to falling behind very much.Because air is very easy
It is arriving and price is very low, so be typically now all intended for oxidant prepares benzene first to be used for liquid-phase oxidation of toluene
Aldehyde, can thus fall below cost minimum.Temperature is so transferred to 140-160 DEG C, pressure is adjusted to 0.446-0.618MPa,
Catalyst is used as using Co etc., although the mainly benzoic acid of generation but the also benzaldehyde containing 1-2%.
In nowadays fast-developing society, as research preparing benzaldehyde by oxidizing toluene is more and more deep, people also from
The research that the different factor of each in oxidizing process is deepened, such as：The influence of the factors such as temperature, time, catalyst, therefore
The research of many documents and patent in terms of these is occurred in that, the selection of wherein catalyst can have influence on the degree of reaction.
Most of benzaldehyde of current China's production is all the requirement for not meeting development, because being all the composition doped with chlorine, so that
Result in benzaldehyde can not come into operation in many industries, such as prepares medicine and fragrance industry also has cosmetic industry etc. all
Chloride benzaldehyde can not be used, is to have very big harm to human body because severe toxicity can be produced containing chlorobenzaldehyde, and with China
Production situation from the point of view of, all benzaldehyde is produced as accessory substance, so its yield and yield are all suitable low, reached
Less than the demand in market.So meeting the demand in market, it is to have to develop a production Technology without chlorobenzaldehyde very much
It is necessary.
The content of the invention
The present invention prior art it is prepared by toluene benzaldehyde process, technological process many comparisons, selection
A kind of environmental protection, clean and effective, new process route, using toluene, oxygen be oxidant and catalyst cobalt as raw material, use
Toluene air oxidation in liquid phase prepares benzaldehyde process route, obtains the technique that a kind of liquid-phase oxidation of toluene prepares benzaldehyde.
Liquid-phase oxidation of toluene reaction mechanism：Liquid-phase oxidation of toluene is the consecutive reaction of an autoxidation, is initially just started
When generation oxidation reaction, the product of production is phenmethylol and benzaldehyde, then benzaldehyde when reaction temperature is increased
Generation benzoic acid will be further oxidized, benzoic acid can also generate directly by toluene oxidation, last benzoic acid also can be by
The other products of oxidation generation, but amount is fewer, can be ignored.
A kind of liquid-phase oxidation of toluene prepares the technique of benzaldehyde, comprises the technical steps that：
1) workshop section is reacted：Raw material toluene enter oxidation reactor mode be directly put at the top of oxidation reaction tower into
Go, the fresh air after overcompression is directly injected into from the beneath entrance of oxidation reaction tower, and mixed reaction solution can not be complete
Reaction, some reaction solution flows back to oxidation reaction tower weight after the heat exchange of heat exchanger and newly reacted again；
2) centrifugal station：The material component for carrying out automatic oxidation reaction tower flows into flash tank, part light component from flash vessel tower
Top is flashed off, and the light component is the water and unreacted toluene and oxygen that partial reaction is generated；
Other components then exit into rectifying column 1 from the tower reactor of flash vessel and separated, and rectifying column 1, which is one, 17 pieces of towers
The rectifying column of plate, from the 7th piece of column plate charging, component phenmethylol and the toluene not flashed away that the tower top of rectifying column 1 is isolated
Produced with oxygen as byproduct；
Remaining component flowed out from the tower reactor of rectifying column 1 enters rectifying column 2 after pump, and rectifying column 2, which is one, 17 pieces of towers
The rectifying column of plate, from the 7th piece of pedal charging；
The tower reactor of rectifying column 2 mainly isolates benzoic acid, is produced as byproduct, and the tower top of rectifying column 2 isolates crude product benzene
Formaldehyde carries out accurate rectifying into rectifying column 3, and rectifying column 3, which is one, a rectifying column of 17 blocks of column plates, crude product benzaldehyde from
7th piece of column plate charging；
Final major product benzaldehyde is from the overhead extraction of rectifying column 3, and purity reaches more than 97%, other a small amount of blending ingredients
From the outflow of the tower reactor of rectifying column 3；
3) vent gas treatment workshop section：After tail gas cooling, purified treatment is carried out to pernicious gas and pollution environmental gas.
Step 1 of the present invention) described in reaction workshop section, the mode that raw material toluene enters oxidation reaction tower is directly anti-in oxidation
The top of tower is answered to put into, the fresh air after overcompression is directly injected into from the beneath entrance of oxidation reaction tower, after mixing
Reaction solution can not react completely, so some reaction solution by heat exchanger heat exchange after flow back to oxidation reaction again
Tower weight newly reacts, and thus enables the material in reactor have more fully stirring to strengthen the mixing between reactant
Effect and making the middle heat of oxidation reaction tower participate in reaction again makes it be fully utilized.
Liquid-phase oxidation of toluene of the present invention prepares the technique of benzaldehyde, the preferred cobalt of liquid-phase oxidation of toluene catalysts
Salt is used as catalyst.Most of catalyst needed for liquid-phase oxidation of toluene reaction is all the organic carboxylate of some transition metals,
And cobalt salt and manganese salt are most popular, because their effect is relatively good.Cobalt is by using potential during redox itself
Hydroperoxides in the effective decomposition reaction of high the characteristics of reach catalytic effect, and liquid-phase oxidation of toluene reaction is freely
Base chain reaction, so cobalt can allow it to produce the chain reaction that free radical participates in oxidation reaction, cobalt is exactly to be produced by separating
Positive trivalent Co ions with peroxide organic acid occur fast response generation free radical, so that radical initiator is obtained, here it is cobalt
Catalytic process, and the catalytic effect of cobalt salt do not disturbed by its anion, but its price is cheap, and is easy to
Obtain, there is good cost performance, so cobalt salt is the most frequently used catalyst.In order that cobalt salt catalytic performance bigizationner and reaction induced
Phase becomes shorter, and generally can all add some accelerator and enter in reaction, such as add the brominations such as sodium bromide, potassium, amine, manganese
Thing.
Compared with prior art, the present invention has advantages below：
1st, the inventive method liquid-phase oxidation of toluene producing benzaldehyde, technical maturity, environmental protection is new, and raw material is easy to get cheaply,
High income, accessory substance is few, pollution-free, and principal product is not chloride, and purity is high, and equipment investment is few.
2nd, rectifying column of the present invention selects 17 pieces of numbers of plates to be that applicant passes through the result that many experiments are obtained, if increase is more
Many numbers of plates, the yield of product can be reduced, and cost can be improved；If reducing the number of plates, the purity of product can be reduced, and not meet production
Product requirement.
Embodiment
With embodiment, the invention will be further described below, but the invention is not limited in these embodiments.
Embodiment：
A kind of liquid-phase oxidation of toluene prepares the technique of benzaldehyde, comprises the technical steps that：
1) workshop section is reacted：
Raw material toluene enters after heater carries out heat temperature raising by pump and enters oxidation reaction tower, and oxygen is then through overcompression
Enter oxidation reaction tower after the compression of machine, carry out toluene air oxidation in liquid phase reaction；
2) centrifugal station：The material component for carrying out automatic oxidation reaction tower flows into flash tank, part light component from flash vessel tower
Top is flashed off, and light component includes the water and unreacted toluene and oxygen that partial reaction is generated；
Other components then exit into rectifying column 1 from the tower reactor of flash vessel and separated, and rectifying column 1, which is one, 17 pieces of towers
The rectifying column of plate, from the 7th piece of column plate charging, component phenmethylol and the toluene not flashed away that the tower top of rectifying column 1 is isolated
Produced with oxygen as byproduct；
Remaining component flowed out from the tower reactor of rectifying column 1 enters rectifying column 2 after pump, and rectifying column 2, which is one, 17 pieces of towers
The rectifying column of plate, from the 7th piece of pedal charging；
The tower reactor of rectifying column 2 mainly isolates benzoic acid, is produced as byproduct, and the tower top of rectifying column 2 isolates crude product benzene
Formaldehyde carries out accurate rectifying into rectifying column 3, and rectifying column 3, which is one, a rectifying column of 17 blocks of column plates, crude product benzaldehyde from
7th piece of column plate charging；
Final major product benzaldehyde is from the overhead extraction of rectifying column 3, and purity reaches more than 97%, other a small amount of blending ingredients
From the outflow of the tower reactor of rectifying column 3；
3) vent gas treatment workshop section：After tail gas cooling, purified treatment is carried out to pernicious gas and pollution environmental gas.
Mass balance
1st, toluene is used for raw material, oxygen is oxidant, cobalt acetate is catalyst, 160 DEG C of reaction temperature, reaction pressure
600KPa, the annual production of benzaldehyde is 1.5 ten thousand tons, and accessory substance mainly includes benzoic acid and phenmethylol, and the time of work in 1 year is
8000h。
1.1 reaction workshop section technological process mass balances
React workshop section's flow mass balance table
The brief summary of 1.2 reaction workshop sections
React workshop section it is total it is co-feeding be 9110.55kg/hr, discharge as 9110.54kg/hr, material is in poised state, instead
The crude product benzaldehyde that workshop section is 51.69% by the reaction generation 4708.91kg/hr mass fractions of reactor is answered,
119.96kg/hr mass fractions are 1.32% byproduct phenmethylol；135.47kg/hr mass fractions are 1.49% benzoic acid,
Into next workshop section, the wherein conversion ratio of toluene is 80%.
2 centrifugal station mass balances
2.1 centrifugal station flow mass balance tables
2.2 centrifugal station brief summaries
In liquid-phase oxidation of toluene prepares benzaldehyde centrifugal station, total charging is 9110.53kg/hr, and discharging is
9110.51kg/hr, system is in material balance.In centrifugal station, the flash distillation of flash tank is have passed through, part 678kg/ is obtained
Hr mass fractions are 14.01% toluene, and this can carry out recycling by purification；By separating for rectifying column 1
To toluene be that 110.30kg/hr mass fractions are 43.93% and a small amount of byproduct phenmethylol, these can be carried out reclaim
Utilization is purified again；Then it is 6.75% by-product separating benzoic acid to have obtained 134.83kg/hr mass fractions by rectifying column 2
Product benzoic acid, and crude product benzaldehyde has also been obtained here for 1771.49kg/hr, mass fraction is 88.64%, this
Purification again can be carried out, purity is reached and higher is used as major product.Eventually pass through separating again for rectifying column 3
The major product benzaldehyde that 1875.01kg/hr mass fractions are 97.63% is arrived, the purity for realizing major product reaches 95%, and
And toluene is separated circulate in utilization, raw material have been saved well, have been increased economic efficiency.
3. whole process mass balance
3.1 whole mass balance tables
3.2 brief summary
Pass through mass balance, it is determined that the consumption of methylbenzene raw material, the purity of major product benzaldehyde, reaction tower, sudden strain of a muscle is determined
The column plate of the input and output flow of steaming pot and each rectifying column, mass fraction and mole fraction and component, also rectifying column
Number.
The consumption of toluene raw material：40884.4 ton/year, major product benzaldehyde annual production：15000 tons/year, mass fraction
For 97.63%, the number of plates of rectifying column is 17 pieces.
Comparative example：
In existing industrial processes, the technological process substantially step of liquid-phase oxidation of toluene method is as follows：
The mode that raw material toluene enters oxidation reactor is directly to enter in the top input of oxidation reactor, through overcompression
Fresh air afterwards is directly injected into from the beneath entrance of oxidation reactor；
Mixed reaction solution can not react completely, so some reaction solution is again heavy after the heat exchange of heat exchanger
Newly oxidation reactor is flowed back to react again；The preheating of raw material toluene is realized by the by-product low-pressure steam of heat exchanger, from reaction
The reacted gas-liquid mixture flowed out on device top, the gas-liquid separation that separator carries out mixture is flowed into by pipeline；
After separation is finished, it is injected into first rectifying column and carries out first step fractionation process, returned to after toluene is extracted
To oxidation reactor；The side line material that first rectifying column is fractionated then will also flow into Second distillation column by fractionation again,
Then purpose product benzaldehyde is flowed out from the tower top mouthful of Second distillation column, and kettle material then needs to extract back by catalyst
It could be come back to again in reactor after receipts；
Purified treatment is carried out to pernicious gas and pollution environmental gas after last tail gas cooling.
The consumption of toluene raw material：30000 tons/year, major product benzaldehyde annual production：9000 tons/year, mass fraction is
95.23%, the number of plates of rectifying column is 23 pieces.
Claims (3)
1. the technique that a kind of liquid-phase oxidation of toluene prepares benzaldehyde, it is characterised in that comprise the technical steps that：
1) workshop section is reacted：The mode that raw material toluene enters oxidation reactor is directly to enter in the top input of oxidation reaction tower,
Fresh air after overcompression is directly injected into from the beneath entrance of oxidation reaction tower, and mixed reaction solution can not be completely anti-
Should, some reaction solution flows back to oxidation reaction tower weight after the heat exchange of heat exchanger and newly reacted again；
2) centrifugal station：The material component for carrying out automatic oxidation reaction tower flows into flash tank, and part light component is dodged from flash vessel tower top
It is steamed out, the light component is the water and unreacted toluene and oxygen that partial reaction is generated；
Other components then exit into rectifying column 1 from the tower reactor of flash vessel and separated, and rectifying column 1, which is one, 17 blocks of column plates
Rectifying column, from the 7th piece of column plate charging, component phenmethylol and the toluene and oxygen not flashed away that the tower top of rectifying column 1 is isolated
Gas is produced as byproduct；
Remaining component flowed out from the tower reactor of rectifying column 1 enters rectifying column 2 after pump, and rectifying column 2, which is one, 17 blocks of column plates
Rectifying column, from the 7th piece of pedal charging；
The tower reactor of rectifying column 2 mainly isolates benzoic acid, is produced as byproduct, and the tower top of rectifying column 2 isolates crude product benzaldehyde
Accurate rectifying is carried out into rectifying column 3, rectifying column 3, which is one, the rectifying column of 17 blocks of column plates, and crude product benzaldehyde is from the 7th piece
Column plate is fed；
Final major product benzaldehyde is from the overhead extraction of rectifying column 3, and purity reaches more than 97%, and other a small amount of blending ingredients are from essence
Evaporate the outflow of the tower reactor of tower 3；
3) vent gas treatment workshop section：After tail gas cooling, purified treatment is carried out to pernicious gas and pollution environmental gas.
2. the technique that a kind of liquid-phase oxidation of toluene according to claim 1 prepares benzaldehyde, it is characterised in that：Step 1) institute
The reaction workshop section stated, the mode that raw material toluene enters oxidation reaction tower is directly to enter in the top input of oxidation reaction tower, is passed through
Fresh air after overcompression is directly injected into from the beneath entrance of oxidation reaction tower.
3. the technique that a kind of liquid-phase oxidation of toluene according to claim 1 prepares benzaldehyde, it is characterised in that：Described first
Benzene liquid phase oxidation prepares the technique of benzaldehyde, and liquid-phase oxidation of toluene catalysts are cobalt salt.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109772466A (en) * | 2019-01-23 | 2019-05-21 | 厦门中坤化学有限公司 | Cobalt acetate/bromination sodium catalyst recovery method in a kind of catalytic oxidation |
| CN114558532A (en) * | 2022-03-04 | 2022-05-31 | 连云港市工投集团利海化工有限公司 | Production method and equipment of environment-friendly benzaldehyde |
| CN114773170A (en) * | 2022-05-05 | 2022-07-22 | 上海予君生物科技发展有限公司 | Preparation process of m-phthalaldehyde |
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| CN109772466A (en) * | 2019-01-23 | 2019-05-21 | 厦门中坤化学有限公司 | Cobalt acetate/bromination sodium catalyst recovery method in a kind of catalytic oxidation |
| CN109772466B (en) * | 2019-01-23 | 2021-12-24 | 厦门中坤化学有限公司 | Method for recovering cobalt acetate/sodium bromide catalyst in catalytic oxidation reaction |
| CN114558532A (en) * | 2022-03-04 | 2022-05-31 | 连云港市工投集团利海化工有限公司 | Production method and equipment of environment-friendly benzaldehyde |
| CN114558532B (en) * | 2022-03-04 | 2023-02-17 | 连云港市工投集团利海化工有限公司 | Production method and equipment of environment-friendly benzaldehyde |
| CN114773170A (en) * | 2022-05-05 | 2022-07-22 | 上海予君生物科技发展有限公司 | Preparation process of m-phthalaldehyde |
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