CN110526814A - The method that serialization prepares butyric acid - Google Patents
The method that serialization prepares butyric acid Download PDFInfo
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- CN110526814A CN110526814A CN201910685126.XA CN201910685126A CN110526814A CN 110526814 A CN110526814 A CN 110526814A CN 201910685126 A CN201910685126 A CN 201910685126A CN 110526814 A CN110526814 A CN 110526814A
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
- C07C51/21—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen
- C07C51/23—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of oxygen-containing groups to carboxyl groups
- C07C51/235—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of oxygen-containing groups to carboxyl groups of —CHO groups or primary alcohol groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
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Abstract
The invention discloses a kind of methods that serialization prepares butyric acid, comprising the following steps: 1. butyraldehyde is added in oxidizing tower, adds to the 1/4~1/3 of oxidation tower height degree, air is added from oxidation tower bottom, and control tower interior reaction temperature is at 30 DEG C~40 DEG C in reaction process；2. bottom starts continuous feed when butyraldehyde conversion ratio reaches 80%~90% in the oxidizing tower of step 1., top is continuously produced；3. the mixture that top produces is introduced into condenser condensation, liquid is sent into rectifying column；Liquid is heated in rectifying column, and the reaction was continued in overhead extraction butyraldehyde return oxidizing tower；Tower bottom produces n-butyric acie and is sent into storage tank.Preparation method of the invention is excessive without catalyst, low temperature, aldehyde, and control butyraldehyde conversion ratio is 80%~90% in oxidizing tower；Due to inhibiting side reaction, the mixed material after reaction is made of butyric acid and butyraldehyde, and by the butyric acid of the isolated high-purity of rectifying, isolated butyraldehyde returns to oxidizing tower and participates in reaction again.
Description
Technical field
The present invention relates to a kind of preparation methods of butyric acid, and in particular to a kind of method of serialization preparation high-purity butyric acid.
Background technique
Butyric acid is a kind of important fine chemical material, mainly for the manufacture of cellulose butyrate and Synthesis of Butyric Esters, ester
Class is widely used in fragrance, instrument additive, medicine and other fields.
The industrial method of butyric acid is mainly fermentation method and butyraldehyde/butanol oxidizing process.Fermentation method is with starch or sugar
For raw material, fermented to obtain butyric acid with butyric.Butyraldehyde oxidizing process is using manganese acetate or cobalt acetate as catalyst, with air or oxygen oxygen
Change butyraldehyde, after reaction, is fractionated to obtain butyric acid.Concentrated nitric acid oxidation method is to be oxidized using n-amyl alcohol as raw material with concentrated nitric acid
At n-butyric acie.
" Preparation of Butyric Acid by Oxidation of Butyraldehyde research " (Li Xingcun etc., Chemical Reaction Engineering and technique, 2002
June, the 2nd phase of volume 18) one text oxidation technology is optimized, with tower oxidation reactor oxidation n-butanal prepare positive fourth
Acid, the pilot process condition of optimization are as follows: catalyst is 0.1%~0.2% to the mass fraction of n-butanal, and reaction temperature is 50~60
DEG C, the reaction time is about 3h or so, and oxygen aldehyde molar ratio is 0.75~0.875；The conversion ratio of n-butanal is greater than with this condition
99.5%, the selectivity of n-butyric acie has been more than 95%.
" technical study of n-butanal oxidation preparing high-purity n-butyric acie " (Lv Zhiguo, fragrance flavor and cosmetic, 2002 12
Month, the 6th phase) disclose following synthesis technology: oxidation is added to after raw material n-butanal and catalyst CMC are mixed according to a certain ratio
In reactor, oxygen enters after the metering of gas mass flow meter from reactor bottom, carries out oxidation reaction, tail gas with n-butanal
It is condensed and is vented after gas-liquid separation.N-butanal oxidation is carried out using the tower oxidation reactor with extracorporal circulatory system cooling system
N-butyric acie processed can effectively remove oxidation reaction heat, reduce side reaction.At 60 DEG C of reaction temperature or so, reaction time 3h, oxygen
Aldehyde is than under the preferable reaction condition for 0.875 or so, the conversion ratio of n-butanal is 99.5% or more, and the selectivity of n-butyric acie is 95%
More than.
Chinese patent CN 201610983534.X discloses a kind of device and method that butyraldehyde oxidation prepares butyric acid, device
First reactor, second reactor, the first butyric acid rectifying including being connected with oxygen input tube line and butyraldehyde raw material intake pipeline
Tower, the second butyric acid rectifying column.
Butyraldehyde oxidation prepares the method for butyric acid the following steps are included: step 1, by butyraldehyde head tank butyraldehyde and
The first unoxidized butyraldehyde in butyric acid the top of the distillation column is delivered to first reactor, carries out aoxidizing under the action of catalyst with oxygen anti-
It answers, for the mixing gaseous phase materials that tower top obtains after the first cooling water heat exchanger is cooling, condensate liquid is back to first reactor, does not coagulate
Exhaust gas enters emptying after tail gas absorber absorbed；The blended liquid phase material that tower reactor obtains is cold through the second cooling water heat exchanger
But after, a part is back to first reactor, and another part enters second reactor；Step 2, into the mixed of second reactor
It closes liquid phase material and oxygen continues oxidation reaction；The mixing gaseous phase materials that tower top obtains are cooling through third cooling water heat exchanger
Afterwards, condensate liquid is back to second reactor, and not solidifying exhaust gas enters emptying after tail gas absorber absorbed；Tower reactor obtains thick
Butyric acid mixed liquor is sent pump outside and pumped out through first is divided into two parts, and a part is back to second after the cooling of the 4th cooling water heat exchanger
Reactor, another part enter the first butyric acid rectifying column；Step 3, into the cymogene acid mixed liquor warp in the first butyric acid rectifying column
Low-pressure steam heater heating evaporation, the unoxidized butyraldehyde and water vapour of overhead extraction through the 5th cooling water heat exchanger condense into
Enter the first submerged soil and carry out sedimentation separation, send wherein unoxidized butyraldehyde pumps a part by the second outer circulation to the first reaction
Device, another part are back to the first butyric acid rectifying column, and organic wastewater is conveyed by export pipeline and collected；The butyric acid of tower reactor extraction is mixed
Conjunction liquid sends pump outside through third and is pumped into the second butyric acid rectifying column；Step 4, into the butyric acid mixed liquor warp in the second butyric acid rectifying column
Middle pressure steam heater heating evaporation, the n-butyric acie that the second butyric acid rectifying column top produces are cooling through the 6th cooling water heat exchanger
Afterwards, a part is back to the second butyric acid rectifying column, and another part is sent to finished product tank field；The catalyst mother liquor and fourth of tower reactor extraction
Heavy constituent in aldehyde raw material, a part are back to first reactor, and another part is delivered to heavy constituent tank field.
Foregoing invention is to be made up using butyraldehyde as raw material of dioxygen oxidation reaction, and reaction process belongs to continuous operation, production
Process uses mutually equal catalyst, and post catalyst reaction is recycled, and fourth is made by distillation system in the cymogene acid after oxidation reaction
Acid product；The present invention is simple with process route, production is easy to control, using butyraldehyde direct oxidation, is deviate from by distillation technology
Unoxidized butyraldehyde and butyraldehyde raw material bring heavy constituent improve the purity of product, butyraldehyde oxidation compared with biological fermentation process
In the process, not oxidized butyraldehyde returns re-oxidation in reactor by reflux pump, improves product yield.
Summary of the invention
Technical problem to be solved by the invention is to provide the high serializations of a kind of simple process, product purity to prepare butyric acid
Method.
The technical solution for realizing the object of the invention is a kind of method that serialization prepares butyric acid, comprising the following steps:
1. by butyraldehyde be added oxidizing tower in, add to oxidation tower height degree 1/4~1/3, air from oxidation tower bottom be added, butyraldehyde with
The molar ratio of oxygen is 2:0.8~0.9 in air；Oxygen and butyraldehyde in air start oxidation reaction, control in reaction process
Tower interior reaction temperature is at 30 DEG C~40 DEG C；
2. bottom starts continuous feed when butyraldehyde conversion ratio reaches 80%~90% in the oxidizing tower of step 1., top is continuously adopted
Contain butyraldehyde and butyric acid mixture out；When the continuous feed of bottom, the molar ratio of butyraldehyde and oxygen in air in reaction mass is controlled
For 2:0.8~0.9, reactor temperature reaction temperature is at 30 DEG C~40 DEG C；
3. the mixture that top produces is introduced into condenser condensation, gas emptying, liquid is sent into rectifying column；Liquid is in rectifying column
It is heated, the butyraldehyde of overhead extraction returns in oxidizing tower after condenser condenses, and tower bottom produces n-butyric acie and is sent into storage tank.
By using above scheme, the specific steps that a kind of serialization prepares butyric acid are provided, it is continuous from starting to be reacted to
Charging controls reaction conversion ratio by molar ratio of the control feed reactants between air and feed reactants, and passes through essence
It evaporates tower the excessive butyraldehyde for having neither part nor lot in reaction to be returned to reaction kettle the reaction was continued, has reached safety, green, efficient butyric acid
Preparation.
1. middle butyraldehyde is n-butanal or isobutylaldehyde to step.
By using above scheme, the serialization provided prepares butyric acid process and can be used for preparing isobutyric acid.
1. middle butyraldehyde feeds to the 1/4 of oxidation tower height degree step.
By using above scheme, control starting reaction response object mole, the reactant that complex reaction tower can bear
Volume reaches reaction optimal conversion, and is conducive to subsequent continuous preparation.
1. the molar ratio of middle butyraldehyde and oxygen in air is 2:0.9 to step.
By using above scheme, turning for control reactant butyraldehyde is reached by formoxy- molar ratio in control reaction system
Rate effectively inhibits side reaction.
Step 2. in the butyraldehyde butyraldehyde isolated from butyraldehyde storage tank and rectifying column.
By using above scheme, unreacted butyraldehyde is participated in reacting again, has reached what Green Chemistry was reacted completely
Effect.
For step 2. when butyraldehyde conversion ratio reaches 85%~90% in step oxidizing tower 1., bottom starts continuous feed.
By using above scheme, controls optimum response conversion ratio and just start continuous feed, can guarantee to react lasting, steady
Fixed progress.
Step 3. in, separate n-butanal and when n-butyric acie, 76~81 DEG C of the bottom temperature of rectifying column, tower top temperature 75~77
℃。
Suitable vapo(u)rizing temperature is taken according to the boiling point of n-butanal by using above scheme, just by extra unreacted
Butyraldehyde evaporating completely.
Step 3. in, separate isobutylaldehyde and when isobutyric acid, 65~70 DEG C of the bottom temperature of rectifying column, tower top temperature 63~65
℃。
Suitable vapo(u)rizing temperature is taken according to the boiling point of isobutylaldehyde by using above scheme, extra unreacted is different
Butyraldehyde evaporating completely.
Step 3. in, the butyraldehyde of extraction after condenser is condensed to 30 DEG C~35 DEG C, return oxidizing tower in.
By using above scheme, extra unreacted butyraldehyde is condensed back and participates in reaction again to reaction kettle, is made
Reactant reacts completely.
The present invention has the effect of positive:
(1) preparation method of the invention carries out the oxidation reaction of butyraldehyde under conditions of low temperature, control oxygen, and reaction temperature is 30~40
DEG C, it can effectively inhibit side reaction under low temperature, improve product purity, low energy consumption for low-temp reaction safety.
(2) without using catalyst in preparation method of the invention, using air oxidation butyraldehyde, relative to pure oxygen, air
Cheaply, production cost is reduced, simultaneously because pure oxygen is not used to improve the safety of reaction system instead, reducing may hair
Raw danger.
(3) preparation method of the invention is excessive without catalyst, low temperature, aldehyde, does not pursue a period of time butyraldehyde in the stage of reaction and converts
Rate, for control butyraldehyde conversion ratio 80%~90%, the extra butyraldehyde having neither part nor lot in enters rectifying column together with butyric acid in oxidizing tower, warp
The butyric acid of the isolated high-purity of rectifying is crossed, and distills the butyraldehyde first come out and participates in reaction again by condensation return oxidizing tower,
Improve the conversion ratio of final butyraldehyde.
Specific embodiment
It includes oxidizing tower, rectifying column and condensation that the serialization of following embodiment, which prepares device used in the method for butyric acid,
Device.Tower height 20m is aoxidized, the lower part of reaction tower is equipped with one section of collet, and lower part collet is connected with recirculated water.
(method that embodiment 1, serialization prepare n-butyric acie)
The serialization of the present embodiment prepare the method for n-butyric acie the following steps are included:
1. n-butanal is added in oxidizing tower, the 1/4 of oxidation tower height degree is added to；Air is after flowmeter measures from oxidation tower bottom
It is added, the molar ratio for controlling n-butanal and oxygen is 2:0.9；Oxygen and n-butanal in air start oxidation reaction.It reacted
Control tower interior reaction temperature is at 30 DEG C in journey；
2. when n-butanal conversion ratio reaches 80% in the oxidizing tower of step 1., bottom starts continuous feed (n-butanal and air),
Top, which continuously produces, contains n-butanal and n-butyric acie mixture.When the continuous feed of bottom, n-butanal and oxygen in reaction mass are controlled
The molar ratio of gas is 2:0.9, and reactor temperature reaction temperature is at 30 DEG C；
N-butanal in the reaction mass n-butanal isolated from n-butanal storage tank and rectifying column.
3. the mixture that top produces is introduced into condenser condensation, gas emptying, liquid is sent into rectifying column.
Liquid is heated in rectifying column, 78 DEG C of the bottom temperature of rectifying column, and 76 DEG C of tower top temperature.
Overhead extraction n-butanal, the n-butanal of extraction return in oxidizing tower after condenser is condensed to 30 DEG C.
Tower bottom produces n-butyric acie and is sent into storage tank, and the n-butyric acie purity of extraction reaches 99.2%.
(method that embodiment 2, serialization prepare n-butyric acie)
The serialization of the present embodiment prepare the method for n-butyric acie the following steps are included:
1. n-butanal is added in oxidizing tower, the 3/10 of oxidation tower height degree is added to；Air is after flowmeter measures from oxidizing tower bottom
Portion is added, and the molar ratio for controlling n-butanal and oxygen is 2:0.85；Oxygen and n-butanal in air start oxidation reaction.Reaction
Control tower interior reaction temperature is at 35 DEG C in the process；
2. when n-butanal conversion ratio reaches 85% in the oxidizing tower of step 1., bottom starts continuous feed (n-butanal and air),
Top, which continuously produces, contains n-butanal and n-butyric acie mixture.When the continuous feed of bottom, n-butanal and oxygen in reaction mass are controlled
The molar ratio of gas is 2:0.85, and reactor temperature reaction temperature is at 35 DEG C；
N-butanal in the reaction mass n-butanal isolated from n-butanal storage tank and rectifying column.
3. the mixture that top produces is introduced into condenser condensation, gas emptying, liquid is sent into rectifying column.
Liquid is heated in rectifying column, 80 DEG C of the bottom temperature of rectifying column, and 76 DEG C of tower top temperature.
Overhead extraction n-butanal, the n-butanal of extraction return in oxidizing tower after condenser is condensed to 30 DEG C.
Tower bottom produces n-butyric acie and is sent into storage tank, and the n-butyric acie purity of extraction reaches 99.5%.
(method that embodiment 3, serialization prepare n-butyric acie)
The serialization of the present embodiment prepare the method for n-butyric acie the following steps are included:
1. n-butanal is added in oxidizing tower, the 1/4 of oxidation tower height degree is added to；Air is after flowmeter measures from oxidation tower bottom
It is added, the molar ratio for controlling n-butanal and oxygen is 2:0.9；Oxygen and n-butanal in air start oxidation reaction.It reacted
Control tower interior reaction temperature is at 35 DEG C in journey；
2. when n-butanal conversion ratio reaches 90% in the oxidizing tower of step 1., bottom starts continuous feed (n-butanal and air),
Top, which continuously produces, contains n-butanal and n-butyric acie mixture.When the continuous feed of bottom, n-butanal and oxygen in reaction mass are controlled
The molar ratio of gas is 2:0.9, and reactor temperature reaction temperature is at 35 DEG C；
N-butanal in the reaction mass n-butanal isolated from n-butanal storage tank and rectifying column.
3. the mixture that top produces is introduced into condenser condensation, gas emptying, liquid is sent into rectifying column.
Liquid is heated in rectifying column, 80 DEG C of the bottom temperature of rectifying column, and 76 DEG C of tower top temperature.
Overhead extraction n-butanal, the n-butanal of extraction return in oxidizing tower after condenser is condensed to 30 DEG C.
Tower bottom produces n-butyric acie and is sent into storage tank, and the n-butyric acie purity of extraction reaches 99.6%.
(method that embodiment 4, serialization prepare n-butyric acie)
The serialization of the present embodiment prepare the method for n-butyric acie the following steps are included:
1. n-butanal is added in oxidizing tower, the 1/4 of oxidation tower height degree is added to；Air is after flowmeter measures from oxidation tower bottom
It is added, the molar ratio for controlling n-butanal and oxygen is 2:0.9；Oxygen and n-butanal in air start oxidation reaction.It reacted
Control tower interior reaction temperature is at 40 DEG C in journey；
2. when n-butanal conversion ratio reaches 90% in the oxidizing tower of step 1., bottom starts continuous feed (n-butanal and air),
Top, which continuously produces, contains n-butanal and n-butyric acie mixture.When the continuous feed of bottom, n-butanal and oxygen in reaction mass are controlled
The molar ratio of gas is 2:0.9, and reactor temperature reaction temperature is at 40 DEG C；
N-butanal in the reaction mass n-butanal isolated from n-butanal storage tank and rectifying column.
3. the mixture that top produces is introduced into condenser condensation, gas emptying, liquid is sent into rectifying column.
Liquid is heated in rectifying column, 79 DEG C of the bottom temperature of rectifying column, and 76 DEG C of tower top temperature.
Overhead extraction n-butanal, the n-butanal of extraction return in oxidizing tower after condenser is condensed to 30 DEG C.
Tower bottom produces n-butyric acie and is sent into storage tank, and the n-butyric acie purity of extraction reaches 99.3%.
(embodiment 5, serialization prepare isobutyric method)
The serialization of the present embodiment prepare isobutyric method the following steps are included:
1. isobutylaldehyde is added in oxidizing tower, the 1/4 of oxidation tower height degree is added to；Air is after flowmeter measures from oxidation tower bottom
It is added, the molar ratio for controlling isobutylaldehyde and oxygen is 2:0.9；Oxygen and isobutylaldehyde in air start oxidation reaction.It reacted
Control tower interior reaction temperature is at 30 DEG C in journey；
2. when isobutylaldehyde conversion rate reaches 90% in the oxidizing tower of step 1., bottom starts continuous feed (isobutylaldehyde and air),
Top, which continuously produces, contains isobutylaldehyde and isobutyl acid blend.When the continuous feed of bottom, isobutylaldehyde and oxygen in reaction mass are controlled
The molar ratio of gas is 2:0.9, and reactor temperature reaction temperature is at 30 DEG C；
Isobutylaldehyde in the reaction mass isobutylaldehyde isolated from isobutylaldehyde storage tank and rectifying column.
3. the mixture that top produces is introduced into condenser condensation, gas emptying, liquid is sent into rectifying column.
Liquid is heated in rectifying column, 67 DEG C of the bottom temperature of rectifying column, and 65 DEG C of tower top temperature.
Overhead extraction isobutylaldehyde, the isobutylaldehyde of extraction return in oxidizing tower after condenser is condensed to 30 DEG C.
Tower bottom produces isobutyric acid and is sent into storage tank, and the isobutyric acid purity of extraction reaches 99.2%.
(embodiment 6, serialization prepare isobutyric method)
The serialization of the present embodiment prepare isobutyric method the following steps are included:
1. isobutylaldehyde is added in oxidizing tower, the 1/3 of oxidation tower height degree is added to；Air is after flowmeter measures from oxidation tower bottom
It is added, the molar ratio for controlling isobutylaldehyde and oxygen is 2:0.85；Oxygen and isobutylaldehyde in air start oxidation reaction.It reacted
Control tower interior reaction temperature is at 35 DEG C in journey；
2. when isobutylaldehyde conversion rate reaches 85% in the oxidizing tower of step 1., bottom starts continuous feed (isobutylaldehyde and air),
Top, which continuously produces, contains isobutylaldehyde and isobutyl acid blend.When the continuous feed of bottom, isobutylaldehyde and oxygen in reaction mass are controlled
The molar ratio of gas is 2:0.85, and reactor temperature reaction temperature is at 35 DEG C；
N-butanal in the reaction mass isobutylaldehyde isolated from isobutylaldehyde storage tank and rectifying column.
3. the mixture that top produces is introduced into condenser condensation, gas emptying, liquid is sent into rectifying column.
Liquid is heated in rectifying column, 68 DEG C of the bottom temperature of rectifying column, and 64 DEG C of tower top temperature.
Overhead extraction isobutylaldehyde, the isobutylaldehyde of extraction return in oxidizing tower after condenser is condensed to 30 DEG C.
Tower bottom produces isobutyric acid and is sent into storage tank, and the isobutyric acid purity of extraction reaches 99.4%.
(embodiment 7, serialization prepare isobutyric method)
The serialization of the present embodiment prepare isobutyric method the following steps are included:
1. isobutylaldehyde is added in oxidizing tower, the 1/4 of oxidation tower height degree is added to；Air is after flowmeter measures from oxidation tower bottom
It is added, the molar ratio for controlling isobutylaldehyde and oxygen is 2:0.8；Oxygen and isobutylaldehyde in air start oxidation reaction.It reacted
Control tower interior reaction temperature is at 40 DEG C in journey；
2. when isobutylaldehyde conversion rate reaches 80% in the oxidizing tower of step 1., bottom starts continuous feed (isobutylaldehyde and air),
Top, which continuously produces, contains isobutylaldehyde and isobutyl acid blend.When the continuous feed of bottom, isobutylaldehyde and oxygen in reaction mass are controlled
The molar ratio of gas is 2:0.8, and reactor temperature reaction temperature is at 40 DEG C；
Isobutylaldehyde in the reaction mass isobutylaldehyde isolated from isobutylaldehyde storage tank and rectifying column.
3. the mixture that top produces is introduced into condenser condensation, gas emptying, liquid is sent into rectifying column.
Liquid is heated in rectifying column, 67 DEG C of the bottom temperature of rectifying column, and 64 DEG C of tower top temperature.
Overhead extraction isobutylaldehyde, the isobutylaldehyde of extraction return in oxidizing tower after condenser is condensed to 30 DEG C.
Tower bottom produces isobutyric acid and is sent into storage tank, and the isobutyric acid purity of extraction reaches 99.3%.
Claims (9)
1. a kind of method that serialization prepares butyric acid, it is characterised in that the following steps are included:
1. by butyraldehyde be added oxidizing tower in, add to oxidation tower height degree 1/4~1/3, air from oxidation tower bottom be added, butyraldehyde with
The molar ratio of oxygen is 2:0.8~0.9 in air；Oxygen and butyraldehyde in air start oxidation reaction, control in reaction process
Tower interior reaction temperature is at 30 DEG C~40 DEG C；
2. bottom starts continuous feed when butyraldehyde conversion ratio reaches 80%~90% in the oxidizing tower of step 1., top is continuously adopted
Contain butyraldehyde and butyric acid mixture out；When the continuous feed of bottom, the molar ratio of butyraldehyde and oxygen in air in reaction mass is controlled
For 2:0.8~0.9, reactor temperature reaction temperature is at 30 DEG C~40 DEG C；
3. the mixture that top produces is introduced into condenser condensation, gas emptying, liquid is sent into rectifying column；Liquid is in rectifying column
It is heated, the butyraldehyde of overhead extraction returns in oxidizing tower after condenser condenses, and tower bottom produces n-butyric acie and is sent into storage tank.
2. the method that serialization according to claim 1 prepares butyric acid, it is characterised in that: 1. middle butyraldehyde is n-butanal to step
Or isobutylaldehyde.
3. the method that serialization according to claim 1 prepares butyric acid, it is characterised in that: 1. middle butyraldehyde feeds to oxygen step
Change the 1/4 of tower height degree.
4. the method that serialization according to claim 1 prepares butyric acid, it is characterised in that: step is 1. in middle butyraldehyde and air
The molar ratio of oxygen is 2:0.9.
5. the method that serialization according to claim 1 prepares butyric acid, it is characterised in that: 2. middle butyraldehyde comes from butyraldehyde to step
Storage tank and the isolated butyraldehyde of rectifying column.
6. the method that serialization according to claim 1 prepares butyric acid, it is characterised in that: the step 2. oxidation when step 1.
When butyraldehyde conversion ratio reaches 85%~90% in tower, bottom starts continuous feed.
7. the method that serialization according to claim 1 prepares butyric acid, it is characterised in that: step 3. in, separate n-butanal
When with n-butyric acie, 78~85 DEG C of the bottom temperature of rectifying column, 75~77 DEG C of tower top temperature.
8. the method that serialization according to claim 1 prepares butyric acid, it is characterised in that: step 3. in, separate isobutylaldehyde
When with isobutyric acid, 65~70 DEG C of the bottom temperature of rectifying column, 63~65 DEG C of tower top temperature.
9. the method that serialization according to claim 1 prepares butyric acid, it is characterised in that: the butyraldehyde of extraction is cold through condenser
It coagulates to after 30 DEG C~35 DEG C and returns in oxidizing tower.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113185395A (en) * | 2021-04-09 | 2021-07-30 | 润泰新材料股份有限公司 | Process for the production of isobutyric acid |
| CN116354809A (en) * | 2023-04-04 | 2023-06-30 | 聊城鲁西多元醇新材料科技有限公司 | Method for treating and reutilizing tail gas from butyric acid production |
| EP4087834B1 (en) * | 2020-01-09 | 2023-11-22 | Basf Se | Process for the preparation of c3-5 saturated aliphatic carboxylic acids |
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| CN116354809A (en) * | 2023-04-04 | 2023-06-30 | 聊城鲁西多元醇新材料科技有限公司 | Method for treating and reutilizing tail gas from butyric acid production |
| CN116354809B (en) * | 2023-04-04 | 2024-01-26 | 聊城鲁西多元醇新材料科技有限公司 | Method for treating and reutilizing tail gas from butyric acid production |
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