CN103058964A - Method for preparing maleic anhydride by continuous dehydration method - Google Patents
Method for preparing maleic anhydride by continuous dehydration method Download PDFInfo
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- CN103058964A CN103058964A CN2013100294138A CN201310029413A CN103058964A CN 103058964 A CN103058964 A CN 103058964A CN 2013100294138 A CN2013100294138 A CN 2013100294138A CN 201310029413 A CN201310029413 A CN 201310029413A CN 103058964 A CN103058964 A CN 103058964A
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- butenedioic anhydride
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Abstract
The invention discloses a method for preparing maleic anhydride by a continuous dehydration method. The method comprises a benzene catalytic oxidation step, a water absorption step, a continuous dehydration step, a coarse maleic anhydride dimethylbenzene stripping step, a coarse maleic anhydride lightening step and a coarse maleic anhydride weight reduction step. The method disclosed by the invention adopts continuous dehydration production, so that a technique is continuous and stable in operation, the product is stable and uniform in quality, and a public engineering energy is stable in use.
Description
Technical field
The present invention relates to a kind of method of industrial producing cis-butenedioic anhydride, specifically, relate to a kind of method of getting cis-butenedioic anhydride with the continuously dehydrating legal system.
Background technology
MALEIC ANHYDRIDE is called for short cis-butenedioic anhydride (MA), has another name called 2,5-furandione, and translated name is maleic anhydride or apple anhydride dehydration.Its molecular formula C4H2O3, these product are colourless acicular crystals under the normal temperature, and irritating smell and tart flavour are arranged, and are inflammable, distillation, generation maleic acid soluble in water (toxilic acid) also is dissolved in the organic solvents such as benzene and acetone, ethanol.
Cis-butenedioic anhydride is broad-spectrum basic organic chemical industry raw material as one of three large organic acid anhydrides, the production history in existing more than 70 years.Be widely used in the industries such as production, coating, paint, printing ink, engineering plastics, medicine, agricultural chemicals, food, feed, oil dope, papermaking, weaving.
The maleic anhydride production method has by-product cis-butenedioic anhydride in benzene oxidation style, n butane oxidation method, oxygenizement of butene and the phthalic anhydride production.
Wherein the benzene oxidation style is the conventional production methods of producing cis-butenedioic anhydride, the Technology mature and reliable, and most these class methods of using of the production of China Maleic Anhydrite are produced.
An important production stage maleic acid producing cis-butenedioic anhydride as the benzene oxidation style crude maleic anhydride that dewaters to get, traditional technology generally adopts intermittently azeotropic dehydration method, being about to dimethylbenzene squeezes in the sequence of constant boiling and rectification still by pump, heat with the rectifying still p-Xylol, in the tower to be drained off refluxing xylene normal after, enter in the tower with the maleic acid of the water middle and upper part from tower, xylene steam in the tower brings to overhead extraction with the free-water in the maleic acid and intermolecular water, the dimethylbenzene that minute the anhydrates use that refluxes again, crude maleic anhydride falls into rectifying still, after crude maleic anhydride in rectifying still and dimethylbenzene reach certain liquid level, stop the charging with the maleic acid of water, rectifying still is continued heating, make the moisture in the dehydration tower, dimethylbenzene in the rectifying still steams successively, and then steam cis-butenedioic anhydride or cis-butenedioic anhydride is squeezed into the continuous treating tower make with extra care, obtain the cis-butenedioic anhydride finished product.
There is following shortcoming in this technique: one, because rectifying still need stop charging after reaching certain liquid level, material in the still is distilled clear still, so power consumption is larger, and it is unstable to consume energy; Two, the cis-butenedioic anhydride that falls into rectifying still needs enrichment, in still the residence time long, high temperature easily generates fumaric acid and other impurity, reduces yield; Three, long because of the residence time in the cis-butenedioic anhydride rectifying still, easily generate fumaric acid and other impurity, be attached to the inwall of rectifying still, need behind the 2-3 batch materials to boil cleaning with hot water, to guarantee the heats of refining kettle, cause the heats of sequence of constant boiling and rectification still to reduce, so need frequently rectifying still to be cleaned, both cause large amount of sewage, increased again energy consumption.
Summary of the invention
The technical problem to be solved in the present invention is to overcome defects, provide a kind of consume energy low, yield is high and the method for getting cis-butenedioic anhydride with the continuously dehydrating legal system of environmental protection.
For addressing the above problem, the technical solution adopted in the present invention is:
A kind of method of getting cis-butenedioic anhydride with the continuously dehydrating legal system is characterized in that the method may further comprise the steps:
(1) benzene is entered the catalyst oxidation reactor that catalyzer is housed continuously with gas phase and carry out oxidizing reaction, obtain the gas phase cis-butenedioic anhydride;
(2) resulting gas phase cis-butenedioic anhydride and air mixture are entered the water absorption tower continuously, the cis-butenedioic anhydride in the water absorbing air generates maleic acid;
(3) maleic acid that obtains after water is absorbed enters in the tower from the middle and upper part of continuously dehydrating tower, dimethylbenzene gas after the reboiler heating enters in the continuously dehydrating tower from the bottom, moisture maleic acid and dimethylbenzene gas are done counter current contact and are absorbed in tower, the crude maleic anhydride that obtains after dehydration is from the extraction of continuously dehydrating tower bottom, the dimethylbenzene that the top extraction is moisture, moisture dimethylbenzene enter and recycle after water-and-oil separator divides water;
(4) will dewater after the gained crude maleic anhydride enter and take off benzenol hydrorefining, remove excessive dimethylbenzene, dimethylbenzene enters dehydration tower and recycles;
(5) gained crude maleic anhydride in the step (4) is entered the cis-butenedioic anhydride lightness-removing column, remove light constituent, then the materials at bottom of tower with lightness-removing column enters the cis-butenedioic anhydride treating tower, removes restructuring and divides, and obtains the target product cis-butenedioic anhydride.
Wherein, the catalyzer in the step (1) is the V-Mo-P series catalysts, can certainly be for satisfying other catalyzer of requirement of the present invention.
As a kind of improvement:
Described step (2) Zhong Shui absorption tower is atmospheric operation, pushes up warm 30-40 ℃, end temperature 60-70 ℃.
The continuously dehydrating tower is column plate tower in the described step (3), and stage number is 23, and the tower tail band has reboiler.
The continuously dehydrating tower is atmospheric operation in the described step (3), pushes up warm 95-110 ℃, and end temperature 145-165 ℃, reflux ratio is 8-10;
Taking off benzenol hydrorefining in the described step (4) is negative-pressure operation, and the control tower pressure on top surface is 20-30KPa, and tower bottom pressure is 30-40KPa, and tower top temperature is 80-100 ℃, and column bottom temperature is 130-150 ℃;
The cis-butenedioic anhydride lightness-removing column is negative-pressure operation in the described step (5), and the control tower pressure on top surface is 10-15KPa, and tower bottom pressure is 15-20KPa, and tower top temperature is 100-120 ℃, and column bottom temperature is 130-150 ℃;
The cis-butenedioic anhydride treating tower is negative-pressure operation in the described step (5), and the control tower pressure on top surface is 5-10KPa, and tower bottom pressure is 10-15KPa, and tower top temperature 120-130 ℃, column bottom temperature is 140-160 ℃.
As further improvement:
The temperature of described dimethylbenzene gas after the reboiler heating is 145-165 ℃.
As further improving:
In the described step (3), moisture dimethylbenzene enters the front first condensation of water-and-oil separator, and condensed temperature is 70 ℃.
Owing to adopted technique scheme, advantage of the present invention and beneficial effect are:
1, technical process of the present invention is advanced, without generation of waste materials, does not have environmental problem, environmental protection in whole production process;
2, the present invention adopts continuously dehydrating, and carrying out that can maximum load produces continuously, has strengthened the continuity that goes into operation of device, has namely reduced the energy dissipation that frequent washing device causes, and has reduced again the generation of sewage, reduces cost;
3, dewatering agent dimethylbenzene of the present invention and the water taken out of thereof dimethylbenzene after water-and-oil separator separates can recycle, and the water of telling can continue to loop water and absorb, and produces environmental protection and increase the utilization ratio of raw material without sewage;
4, the cis-butenedioic anhydride that generates among the present invention is short at dwell time in the tower, has greatly reduced the probability that generates trans fumaric acid and other impurity, has improved yield;
5, the present invention adopts continuously dehydrating to produce cis-butenedioic anhydride, because technique is continuously and operate steadily, and the steady quality homogeneous of product, and the energy of general facilities uses stable.
Embodiment
Embodiment 1:
Benzene feedstock entered continuously with gas phase V-Mo-P series catalysts fixed-bed reactor are housed, through oxidizing reaction
Obtain the gas phase cis-butenedioic anhydride; Resulting gas phase cis-butenedioic anhydride and air mixture are entered the water absorption tower continuously, and the cis-butenedioic anhydride in the water absorbing air generates maleic acid;
The maleic acid that obtains after the water absorption is entered the continuously dehydrating tower from the middle and upper part, dewatering agent dimethylbenzene is preheated to 100 ℃ through preheater, be heated to 145 ℃ through reboiler again, obtain overheated dimethylbenzene gas and enter the continuously dehydrating tower from the bottom, 95 ℃ of control continuously dehydrating column overhead temperature, 145 ℃ of column bottom temperatures, reflux ratio is 8, moisture maleic acid and dimethylbenzene gas are done counter current contact and are absorbed in tower, the crude maleic anhydride that obtains after dehydration is from the extraction of continuously dehydrating tower bottom, the dimethylbenzene that the top extraction is moisture, moisture dimethylbenzene enter and recycle after water-and-oil separator divides water;
The gained crude maleic anhydride enters and takes off benzenol hydrorefining after will dewatering, and taking off benzenol hydrorefining is negative-pressure operation, and the control cat head is pressed
Power is 20KPa, and tower bottom pressure is 30KPa, and tower top temperature is 80 ℃, and column bottom temperature is 130 ℃, removes excessive dimethylbenzene, and dimethylbenzene enters dehydration tower and recycles;
The gained crude maleic anhydride is entered the cis-butenedioic anhydride lightness-removing column, and the cis-butenedioic anhydride lightness-removing column is negative-pressure operation, and the control tower pressure on top surface is 10KPa, tower bottom pressure is 15KPa, and tower top temperature is 100 ℃, and column bottom temperature is 130 ℃, remove light constituent, then the materials at bottom of tower with lightness-removing column enters the cis-butenedioic anhydride treating tower, and the cis-butenedioic anhydride treating tower is negative-pressure operation, the control tower pressure on top surface is 5KPa, tower bottom pressure is 10KPa, 120 ℃ of tower top temperatures, and column bottom temperature is 140 ℃, remove restructuring and divide, obtain the target product cis-butenedioic anhydride.
Embodiment 2:
Benzene feedstock entered continuously with gas phase V-Mo-P series catalysts fixed-bed reactor are housed, obtain the gas phase cis-butenedioic anhydride through oxidizing reaction;
Resulting gas phase cis-butenedioic anhydride and air mixture are entered the water absorption tower continuously, in the water absorbing air
Cis-butenedioic anhydride generates maleic acid;
The maleic acid that obtains after the water absorption is entered the continuously dehydrating tower, dewatering agent dimethylbenzene warp from the middle and upper part
Preheater is preheated to 110 ℃, be heated to 150 ℃ through reboiler again, obtain overheated dimethylbenzene gas and enter the continuously dehydrating tower from the bottom, 105 ℃ of control continuously dehydrating column overhead temperature, 155 ℃ of column bottom temperatures, reflux ratio is 9, moisture maleic acid and dimethylbenzene gas are done counter current contact and are absorbed in tower, the crude maleic anhydride that obtains after dehydration is from the extraction of continuously dehydrating tower bottom, and the dimethylbenzene that the top extraction is moisture, moisture dimethylbenzene enter and recycles after water-and-oil separator divides water;
The gained crude maleic anhydride enters and takes off benzenol hydrorefining after will dewatering, and taking off benzenol hydrorefining is negative-pressure operation, the control cat head
Pressure is 25KPa, and tower bottom pressure is 35KPa, and tower top temperature is 89 ℃, and column bottom temperature is 141 ℃ and removes excessive dimethylbenzene that dimethylbenzene enters dehydration tower and recycles;
The gained crude maleic anhydride is entered the cis-butenedioic anhydride lightness-removing column, and the cis-butenedioic anhydride lightness-removing column is negative-pressure operation, and the control tower pressure on top surface is 12KPa, tower bottom pressure is 18KPa, and tower top temperature is 109 ℃, and column bottom temperature is 142 ℃ and removes light constituent, then the lightness-removing column materials at bottom of tower is entered the cis-butenedioic anhydride treating tower, the cis-butenedioic anhydride treating tower is negative-pressure operation, and the control tower pressure on top surface is 7KPa, and tower bottom pressure is 13KPa, 125 ℃ of tower top temperatures, column bottom temperature is 151 ℃, removes restructuring and divides, and obtains the target product cis-butenedioic anhydride.
Embodiment 3:
Benzene feedstock entered continuously with gas phase V-Mo-P series catalysts fixed-bed reactor are housed, obtain the gas phase cis-butenedioic anhydride through oxidizing reaction;
Resulting gas phase cis-butenedioic anhydride and air mixture are entered the water absorption tower continuously, suitable in the water absorbing air
Acid anhydride generates maleic acid;
The maleic acid that obtains after the water absorption is entered the continuously dehydrating tower from middle and upper part section, dewatering agent dimethylbenzene warp
Preheater is preheated to 120 ℃, be heated to 165 ℃ through reboiler again, obtain overheated dimethylbenzene gas and enter the continuously dehydrating tower from the bottom, 110 ℃ of control continuously dehydrating column overhead temperature, 165 ℃ of column bottom temperatures, reflux ratio is 10, moisture maleic acid and dimethylbenzene gas are done counter current contact and are absorbed in tower, the crude maleic anhydride that obtains after dehydration is from the extraction of continuously dehydrating tower bottom, and the dimethylbenzene that the top extraction is moisture, moisture dimethylbenzene enter and recycles after water-and-oil separator divides water;
The gained crude maleic anhydride enters and takes off benzenol hydrorefining after will dewatering, and taking off benzenol hydrorefining is negative-pressure operation, and the control cat head is pressed
Power is 30KPa, and tower bottom pressure is 40KPa, and tower top temperature is 100 ℃, and column bottom temperature is 150 ℃, removes excessive dimethylbenzene, and dimethylbenzene enters dehydration tower and recycles;
The gained crude maleic anhydride is entered the cis-butenedioic anhydride lightness-removing column, and the cis-butenedioic anhydride lightness-removing column is negative-pressure operation, and the control tower pressure on top surface is 15KPa, tower bottom pressure is 20KPa, and tower top temperature is 120 ℃, and column bottom temperature is 150 ℃, remove light constituent, then the materials at bottom of tower with lightness-removing column enters the cis-butenedioic anhydride treating tower, and the cis-butenedioic anhydride treating tower is negative-pressure operation, the control tower pressure on top surface is 10KPa, tower bottom pressure is 15KPa, 130 ℃ of tower top temperatures, and column bottom temperature is 160 ℃, remove restructuring and divide, obtain the target product cis-butenedioic anhydride.
Catalyst fixed bed reactor in above-described embodiment, water absorption tower, continuously dehydrating tower, reboiler, water-and-oil separator, take off benzenol hydrorefining, cis-butenedioic anhydride lightness-removing column, cis-butenedioic anhydride treating tower and be the commercially available prod, all there is sale in corresponding manufacturer.
Claims (5)
1. method of getting cis-butenedioic anhydride with the continuously dehydrating legal system is characterized in that the method may further comprise the steps:
Benzene is entered the catalyst oxidation reactor that catalyzer is housed continuously with gas phase carry out oxidizing reaction, obtain the gas phase cis-butenedioic anhydride;
Resulting gas phase cis-butenedioic anhydride and air mixture are entered the water absorption tower continuously, and the cis-butenedioic anhydride in the water absorbing air generates maleic acid;
The maleic acid that obtains after water absorbed enters in the tower from the middle and upper part of continuously dehydrating tower, dimethylbenzene gas after the reboiler heating enters in the continuously dehydrating tower from the bottom, moisture maleic acid and dimethylbenzene gas are done counter current contact and are absorbed in tower, the crude maleic anhydride that obtains after dehydration is from the extraction of continuously dehydrating tower bottom, the dimethylbenzene that the top extraction is moisture, moisture dimethylbenzene enter and recycle after water-and-oil separator divides water;
The gained crude maleic anhydride enters and takes off benzenol hydrorefining after will dewatering, and removes excessive dimethylbenzene, and dimethylbenzene enters dehydration tower and recycles;
Gained crude maleic anhydride in the step (4) is entered the cis-butenedioic anhydride lightness-removing column, remove light constituent, then the materials at bottom of tower with lightness-removing column enters the cis-butenedioic anhydride treating tower, removes restructuring and divides, and obtains the target product cis-butenedioic anhydride.
2. a kind of method of getting cis-butenedioic anhydride with the continuously dehydrating legal system according to claim 1 is characterized in that: the continuously dehydrating tower is column plate tower in the described step (3), and stage number is 23, and the tower tail band has reboiler.
3. a kind of method of getting cis-butenedioic anhydride with the continuously dehydrating legal system according to claim 1 and 2 is characterized in that: the continuously dehydrating tower is atmospheric operation in the described step (3), pushes up warm 95-110 ℃, and end temperature 145-165 ℃, reflux ratio is 8-10.
4. a kind of method of getting cis-butenedioic anhydride with the continuously dehydrating legal system according to claim 1 is characterized in that: the temperature of described dimethylbenzene gas after the reboiler heating is 145-165 ℃.
5. a kind of method of getting cis-butenedioic anhydride with the continuously dehydrating legal system according to claim 1 is characterized in that: in the described step (3), moisture dimethylbenzene enters first condensation before the water-and-oil separator.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107011300A (en) * | 2017-05-27 | 2017-08-04 | 天津科林泰克科技有限公司 | A kind of method for preparing cis-butenedioic anhydride along sour continuous dehydration |
| CN113999195A (en) * | 2021-11-26 | 2022-02-01 | 郑朝生 | High-yield maleic anhydride water absorption continuous refining process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107011300A (en) * | 2017-05-27 | 2017-08-04 | 天津科林泰克科技有限公司 | A kind of method for preparing cis-butenedioic anhydride along sour continuous dehydration |
| CN107011300B (en) * | 2017-05-27 | 2020-04-24 | 天津科林泰克科技有限公司 | Method for preparing maleic anhydride by maleic acid continuous dehydration |
| CN113999195A (en) * | 2021-11-26 | 2022-02-01 | 郑朝生 | High-yield maleic anhydride water absorption continuous refining process |
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Application publication date: 20130424 |