CN103044318A - Method for extracting pyridine from coked crude benzene - Google Patents
Method for extracting pyridine from coked crude benzene Download PDFInfo
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- CN103044318A CN103044318A CN2013100291464A CN201310029146A CN103044318A CN 103044318 A CN103044318 A CN 103044318A CN 2013100291464 A CN2013100291464 A CN 2013100291464A CN 201310029146 A CN201310029146 A CN 201310029146A CN 103044318 A CN103044318 A CN 103044318A
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Abstract
The invention discloses a method for extracting pyridine from coked crude benzene. With the coked crude benzene as raw material, the pyridine is extracted, and benzene, methylbenzene and dimethylbenzene are also obtained, so that utilization rate of the coked crude benzene raw material is increased, and yield is increased. The method disclosed by the invention has the advantages that a technological process is advanced, no waste is produced in the whole production process, and no environmental problem exists, so that the method disclosed by the invention is environment-friendly; material hardly corrods equipment, cost is low, and yield and efficiency are high; and the method disclosed by the invention adopts a continuous production mode, so that quality of products is stable and uniform as the pross is continuous and operation is smooth and stable.
Description
Technical field
The present invention relates to a kind of extracting method of pyridine, specifically, relate to a kind of method of being extracted pyridine by coking crude benzene.
Background technology
Pyridine is the 6-membered heterocyclic compound that contains a nitrogen-atoms, can regard a compound that (CH) replaced by N in the benzene molecular as, so claim again pyridine, colourless or little yellow liquid, foul smelling.Pyridine and homologue thereof are present in Dippel's oil, coal tar, coal gas, shale oil, the oil.Pyridine is industrial main as solvent, and except making solvent, pyridine is at industrial denaturing agent, the dyeing auxiliaries of also can be used as, and the raw material of synthetic a series of products (comprising medicine, sterilizing agent, dyestuff, food dressing, tackiness agent, explosive etc.); In addition, pyridine can also be used as catalyzer.
Many derivatives of pyridine are important medicines, and some is the important component part of VITAMIN or enzyme.The derivative vazadrine of pyridine is a kind of antituberculotic, and 2-methyl-5-vinylpyrine is elastomeric raw material, so the having many uses of pyridine.
Pyridine can obtain from crude coal tar, also can be made by acetaldehyde and ammonia.Pyridine and its derivatives also can be synthetic by several different methods, wherein most widely used is the strange pyridine synthesis method of the Chinese, this is with bimolecular β-carbonyl compound, such as methyl aceto acetate and a part acetaldehyde condensation, product forms dihydropyridine compound with the methyl aceto acetate of a part and ammonia condensation again, then use oxygenant (such as nitrous acid) dehydrogenation, hydrolysis is lost carboxylic and is namely got pyridine derivate again; Also available acetylene, ammonia and methyl alcohol prepare by catalyzer at 500 ℃.
Use first sulfuric acid scrubbing in the existing coal tar extraction process, use ammonia neutralization again, then make with extra care, the sour water that occurs in process engineering, Zhong Heshui are difficult to process; And synthesis technique is the ripe technique of a cover, but the shortcoming such as it exists temperature of reaction high, and reaction yield is low.
Summary of the invention
The technical problem to be solved in the present invention is to overcome defects, provides a kind of technical maturity, environmental protection and reaction yield the high method by coking crude benzene extraction pyridine.
For addressing the above problem, the technical solution adopted in the present invention is:
A kind of method by coking crude benzene extraction pyridine is characterized in that the method may further comprise the steps:
(1) coking crude benzene is put into the crude benzol weight-removing column, vacuum distillation removes restructuring minute heavy benzol and dimethylbenzene, and from high boiling material such as weight-removing column bottom extraction heavy benzol and dimethylbenzene, overhead extraction contains the pyridine component, and dimethylbenzene enters the dimethylbenzene refined unit and purifies;
(2) material with overhead extraction in the step (1) enters the crude benzol lightness-removing column, and air distillation removes light constituent, from overhead extraction crude benzol light constituent, and extraction pyridine, benzene and toluene mixture at the bottom of the tower;
(3) material with extraction at the bottom of the tower in the step (2) enters two benzene knockout towers, vacuum distillation, Separation of Benzene and pyridine, toluene,, overhead extraction benzene cut enters the benzene refining unit and reclaims, extraction pyridine, toluene at the bottom of the tower, the benzene cut enters the benzene refining unit and purifies;
(4) pyridine, the toluene that obtains in the step (3) is entered the water extraction tower, atmospheric extraction separates pyridine water extraction absorption with toluene, and toluene enters the toluene refined unit and purifies;
(5) pyridine solution that obtains in the step (4) is entered the benzene azeotropic distillation tower, cat head obtains the azeotrope of benzene and water and puts into water trap, extraction pyridine at the bottom of the tower, and benzene refluxes, and water enters the water extraction tower and recycles;
(6) step enters dehydration tower with the pyridine with micro-moisture that obtains in (5), removes a small amount of moisture and coloring material in the pyridine, obtains the pyridine finished product.
As a kind of improvement:
The crude benzol weight-removing column is vacuum distillation in the described step (1), and pressure is 40-50KPa, pushes up warm 50-60 ℃, and end temperature 140-150 ℃, reflux ratio is 8-10.
The crude benzol lightness-removing column is air distillation in the described step (2), and tower top temperature 50-60 ℃, column bottom temperature is 100-105 ℃, and reflux ratio is 13-15.
Two benzene knockout towers are vacuum distillation in the step (3), and pressure is 30-40 KPa, push up warm 40-50 ℃, and end temperature 70-80 ℃, reflux ratio is 3-4.
The water extraction tower is atmospheric operation in the described step (4), pyridine and toluene component are from water extraction tower extraction section underfeed, and extraction agent water is from the top charging of extraction tower extraction section, and water and pyridine are from extraction bottom extraction, toluene overflows from water extraction tower top, enters the toluene refined unit and reclaims.
The benzene azeotropic distillation tower is air distillation in the step (5), 80-90 ℃ of control tower top temperature, column bottom temperature 90-110 ℃, reflux ratio is 4-6, and cat head obtains the azeotrope of benzene and water-enter water trap, and the benzene after the separation refluxes, water enters the water extraction tower and recycles, extraction pyridine at the bottom of the tower.
As further improvement:
The water-retaining agent that is equipped with in the described dehydration tower is: Calcium Chloride Powder Anhydrous, anhydrous sodium carbonate, wherein one or more of calcium oxide.
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 problem of environmental pollution, environmental protection in whole production process;
2, technical process of the present invention is simple, and material is little to equipment corrosion, and cost is low, and Income is high;
3, the present invention can obtain benzene,toluene,xylene simultaneously by the extraction to pyridine in the coking crude benzene, has strengthened effective utilization of raw material;
4, the present invention since technique continuously and operate steadily the steady quality homogeneous of product.
6, because the present invention all adopts DCS automatically to control, reduce labour intensity, improved work situation.
Embodiment
Embodiment 1:
Coking crude benzene is entered the crude benzol weight-removing column, and vacuum distillation, control pressure are 40KPa, 50 ℃ of top temperature, and 140 ℃ of end temperature, reflux ratio are 8, from high boiling material such as weight-removing column bottom extraction heavy benzol and dimethylbenzene, overhead extraction contains the pyridine component.
The overhead extraction material of crude benzol weight-removing column is entered the crude benzol lightness-removing column, air distillation, 52 ℃ of tower top temperatures, column bottom temperature is 100 ℃, reflux ratio is 13, from overhead extraction crude benzol light constituent, extraction pyridine, benzene and toluene mixture at the bottom of the tower.
The materials at bottom of tower of crude benzol lightness-removing column is entered the crude benzol knockout tower, and vacuum distillation, control pressure are 30 KPa, 40 ℃ of top temperature, and 70 ℃ of end temperature, reflux ratio are 3, overhead extraction benzene component enters the benzene refining unit and reclaims, extraction pyridine, toluene at the bottom of the tower.
The pyridine, the toluene that obtain are entered the water extraction tower, atmospheric operation, pyridine and toluene component are from water extraction tower extraction section underfeed, extraction agent water is from the top charging of extraction tower extraction section, water and pyridine are from extraction bottom extraction, toluene overflows from water extraction tower top, enters the toluene refined unit and reclaims.
The pyridine solution that obtains is entered the benzene azeotropic distillation tower, air distillation, 80 ℃ of control tower top temperatures, 90 ℃ of column bottom temperatures, reflux ratio are 4, and cat head obtains the azeotrope of benzene and water-enter water trap, benzene after the separation refluxes, and water enters the water extraction tower and recycles, extraction pyridine at the bottom of the tower.
The pyridine with micro-moisture that obtains is entered dehydration tower, the Calcium Chloride Powder Anhydrous water-retaining agent is housed in the dehydration tower, remove a small amount of moisture and coloring material in the pyridine, obtain the pyridine finished product,
Embodiment 2
Coking crude benzene is entered the crude benzol weight-removing column, and vacuum distillation, control pressure are 45KPa, 55 ℃ of top temperature, and 145 ℃ of end temperature, reflux ratio are 9, from high boiling material such as weight-removing column bottom extraction heavy benzol and dimethylbenzene, overhead extraction contains the pyridine component.
The overhead extraction material of crude benzol weight-removing column is entered the crude benzol lightness-removing column, air distillation, 56 ℃ of tower top temperatures, column bottom temperature is 102 ℃, reflux ratio is 14, from overhead extraction crude benzol light constituent, extraction pyridine, benzene and toluene mixture at the bottom of the tower.
The materials at bottom of tower of crude benzol lightness-removing column is entered the crude benzol knockout tower, and vacuum distillation, control pressure are 35 KPa, 45 ℃ of top temperature, and 75 ℃ of end temperature, reflux ratio are 3, overhead extraction benzene component enters the benzene refining unit and reclaims, extraction pyridine, toluene at the bottom of the tower.
The pyridine, the toluene that obtain are entered the water extraction tower, atmospheric operation, pyridine and toluene component are from water extraction tower extraction section underfeed, extraction agent water is from the top charging of extraction tower extraction section, water and pyridine are from extraction bottom extraction, toluene overflows from water extraction tower top, enters the toluene refined unit and reclaims.
The pyridine solution that obtains is entered the benzene azeotropic distillation tower, air distillation, 85 ℃ of control tower top temperatures, 98 ℃ of column bottom temperatures, reflux ratio are 5, and cat head obtains the azeotrope of benzene and water-enter water trap, benzene after the separation refluxes, and water enters the water extraction tower and recycles, extraction pyridine at the bottom of the tower.
The pyridine with micro-moisture that obtains is entered dehydration tower, the anhydrous sodium carbonate water-retaining agent is housed in the dehydration tower, remove a small amount of moisture and coloring material in the pyridine, obtain the pyridine finished product.
Embodiment 3
Coking crude benzene is entered the crude benzol weight-removing column, and vacuum distillation, control pressure are 50KPa, 60 ℃ of top temperature, and 150 ℃ of end temperature, reflux ratio are 10, from high boiling material such as weight-removing column bottom extraction heavy benzol and dimethylbenzene, overhead extraction contains the pyridine component.
The overhead extraction material of crude benzol weight-removing column is entered the crude benzol lightness-removing column, air distillation, 59 ℃ of tower top temperatures, column bottom temperature is 109 ℃, reflux ratio is 15, from the overhead extraction crude benzol light constituent of crude benzol lightness-removing column, extraction pyridine, benzene and toluene mixture at the bottom of the tower.
The material of extraction at the bottom of the tower of crude benzol lightness-removing column is entered the crude benzol knockout tower, and vacuum distillation, control pressure are 40 KPa, 49 ℃ of top temperature, and 80 ℃ of end temperature, reflux ratio are 4, overhead extraction benzene component enters the benzene refining unit and reclaims, extraction pyridine, toluene at the bottom of the tower.
The pyridine, the toluene that obtain are entered the water extraction tower, atmospheric operation, pyridine and toluene component are from water extraction tower extraction section underfeed, extraction agent water is from the top charging of extraction tower extraction section, water and pyridine are from extraction bottom extraction, toluene overflows from water extraction tower top, enters the toluene refined unit and reclaims.
The pyridine solution that obtains is entered the benzene azeotropic distillation tower, air distillation, 90 ℃ of control tower top temperatures, 110 ℃ of column bottom temperatures, reflux ratio are 6, and cat head obtains the azeotrope of benzene and water-enter water trap, benzene after the separation refluxes, and water enters the water extraction tower and recycles, extraction pyridine at the bottom of the tower.
The pyridine with micro-moisture that obtains is entered dehydration tower, the calcium oxide water-retaining agent is housed in the dehydration tower, remove a small amount of moisture and coloring material in the pyridine, obtain the pyridine finished product.
Claims (7)
1. one kind is extracted the method for pyridine by coking crude benzene, it is characterized in that the method may further comprise the steps:
(1) coking crude benzene is put into the crude benzol weight-removing column, vacuum distillation removes restructuring minute heavy benzol and dimethylbenzene, and from high boiling material such as weight-removing column bottom extraction heavy benzol and dimethylbenzene, overhead extraction contains the pyridine component, and dimethylbenzene enters the dimethylbenzene refined unit and purifies;
(2) material with overhead extraction in the step (1) enters the crude benzol lightness-removing column, and air distillation removes light constituent, from overhead extraction crude benzol light constituent, and extraction pyridine, benzene and toluene mixture at the bottom of the tower;
(3) material with extraction at the bottom of the tower in the step (2) enters two benzene knockout towers, vacuum distillation, Separation of Benzene and pyridine, toluene,, overhead extraction benzene cut enters the benzene refining unit and reclaims, extraction pyridine, toluene at the bottom of the tower, the benzene cut enters the benzene refining unit and purifies;
(4) pyridine, the toluene that obtains in the step (3) is entered the water extraction tower, atmospheric extraction separates pyridine water extraction absorption with toluene, and toluene enters the toluene refined unit and purifies;
(5) pyridine solution that obtains in the step (4) is entered the benzene azeotropic distillation tower, cat head obtains the azeotrope of benzene and water and puts into water trap, extraction pyridine at the bottom of the tower, and benzene refluxes, and water enters the water extraction tower and recycles;
Step enters dehydration tower with the pyridine with micro-moisture that obtains in (5), removes a small amount of moisture and coloring material in the pyridine, obtains the pyridine finished product.
2. according to claim 1ly extract the method for pyridine by coking crude benzene, it is characterized in that: the crude benzol weight-removing column is vacuum distillation in the described step (1), and pressure is 40-50KPa, pushes up warm 50-60 ℃, and end temperature 140-150 ℃, reflux ratio is 8-10.
3. according to claim 1ly a kind ofly extract the method for pyridine by coking crude benzene, it is characterized in that: the crude benzol lightness-removing column is air distillation in the described step (2), and tower top temperature 50-60 ℃, column bottom temperature is 100-105 ℃, and reflux ratio is 13-15.
4. according to claim 1ly a kind ofly extract the method for pyridine by coking crude benzene, it is characterized in that: two benzene knockout towers are vacuum distillation in the step (3), and pressure is 30-40 KPa, push up warm 40-50 ℃, and end temperature 70-80 ℃, reflux ratio is 3-4.
5. a kind of method of being extracted pyridine by coking crude benzene according to claim 1, it is characterized in that: the water extraction tower is atmospheric operation in the described step (4), pyridine and toluene component are from water extraction tower extraction section underfeed, extraction agent water is from the top charging of extraction tower extraction section, water and pyridine are from extraction bottom extraction, toluene overflows from water extraction tower top, enters the toluene refined unit and reclaims.
6. a kind of method of being extracted pyridine by coking crude benzene according to claim 1, it is characterized in that: the benzene azeotropic distillation tower is air distillation in the step (5), 80-90 ℃ of control tower top temperature, column bottom temperature 90-110 ℃, reflux ratio is 4-6, and cat head obtains the azeotrope of benzene and water-enter water trap, and the benzene after the separation refluxes, water enters the water extraction tower and recycles, extraction pyridine at the bottom of the tower.
7. according to claim 1ly a kind ofly extract the method for pyridine by coking crude benzene, it is characterized in that: the water-retaining agent that is equipped with in the dehydration tower is: Calcium Chloride Powder Anhydrous, anhydrous sodium carbonate, wherein one or more of calcium oxide.
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Cited By (2)
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CN107382831A (en) * | 2017-09-22 | 2017-11-24 | 湖北竹溪人福药业有限责任公司 | A kind of processing method for reclaiming pyridine |
CN110818615A (en) * | 2019-11-25 | 2020-02-21 | 浙江大学 | Method for separating toluene and pyridine |
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CN110818615A (en) * | 2019-11-25 | 2020-02-21 | 浙江大学 | Method for separating toluene and pyridine |
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Application publication date: 20130417 |