CN104592055A - Refining technology of acetonitrile by-product in production of acrylonitrile - Google Patents
Refining technology of acetonitrile by-product in production of acrylonitrile Download PDFInfo
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Abstract
The invention discloses a refining technology of an acetonitrile by-product in production of acrylonitrile. In a traditional acetonitrile refining process, a pervaporation membrane device is additionally arranged between a pressure reduction distillation tower and a pressurized azeotropic tower, and a current three towers-reaction process is changed into an energy-saving three towers-reaction-membrane separation process by using a pervaporation membrane technology. The pervaporation membrane device is additionally arranged behind the pressure reduction distillation tower, so that a part of water contents in acetonitrile-water azeotropic mixture is removed, the product quantity on the top of the pressurized tower is reduced, and the vaporization quantity of two towers is reduced; thus, the energy consumption is reduced, and the aims of energy conservation and consumption reduction are fulfilled.
Description
Technical field
The present invention relates to a kind of acetonitrile refining process, particularly adopt the process for refining of pervaporation method by product acetonitrile in a kind of acrylonitrile process, belong to chemical production technical field.
Background technology
Acetonitrile (acetonitrile CH
3cN) also known as acetonitrile, be the simplest representative examples of saturated aliphatic nitrile.Acetonitrile has excellent solvent nature, can dissolve multiple inorganic, organic and gaseous compound, and except being used as solvent, acetonitrile can also as the cleaning solvent etc. of the extraction agent in petrochemical industry, electronic unit.In addition, acetonitrile also has application in textile dyeing and coating formulation, and it or effective stablizer of chlorinated solvent.The method of suitability for industrialized production acetonitrile has direct synthesis technique and indirect method, indirect method mainly refer to from ammoxidating propylene to produce acrylonitrile simultaneously by-product crude acetonitrile refining obtain.At present, ammoxidating propylene to produce acrylonitrile simultaneously by-product acetonitrile is the main source of industrial production acetonitrile, and therefore, the output of acetonitrile often depends on the production of vinyl cyanide.The crude acetonitrile obtained by ammoxidating propylene to produce acrylonitrile is the aqueous mixture that a kind of component is very complicated, its main component is water and acetonitrile, simultaneously also containing impurity such as prussic acid, vinyl cyanide, oxazole, propionitrile, vinyl carbinol, acetone, vinylformic acid and heavy organism.The downstream 70% of acetonitrile is for pharmaceutical industry, and world market is to the index request purity of pharmaceutical grade acetonitrile more than 99.9%, and the crude acetonitrile of production needs could meet pharmaceutical industries application through refining.Therefore, along with the expansion of acetonitrile of high purity Application Areas and the development of pharmaceutical industries, high, that energy consumption the is little acetonitrile refining process of exploitation production capacity seems particularly urgent.
The exquisite technique of traditional acetonitrile is " three towers one are anti-" technique, that is, by containing the feedstock transportation of 50% acetonitrile to decyanation tower, remove a small amount of prussic acid and lower-boiling impurity; De-nitrile tower tower bottoms is sent to reactor, add sodium hydroxide, the vinyl cyanide in crude acetonitrile and prussic acid are reacted, generate the heavy constituent solution such as succinonitrile, gained solution is entered distillation tower underpressure distillation, removes heavy constituent and obtain the azeotropic mixture of acetonitrile-water; The azeotropic mixture of acetonitrile-water distillates from underpressure distillation tower top, deliver to pressurization azeotropic distillation column, pressurization component distillation tower bottom obtains the commercial product acetonitrile of purity more than 99.5%, and the acetonitrile-water azeotropic mixture that tower top concentration is lower is returned to vacuum still circulation and stress.The exquisite technical maturity of above-mentioned acetonitrile is stablized, but its defect existed is that product purity is not high.In addition, because in crude acetonitrile, water ratio is higher, distillation and pressure distillation stage is caused to consume energy higher.Chinese patent 201310119890.3 provides a kind of technique of pervaporation method purified acetonitrile, concrete steps be first by crude acetonitrile through decyanation column distillation, remove most of light constituents such as prussic acid, obtain the azeotrope of acetonitrile-water; The azeotrope of acetonitrile-water is sent into chemical treatment still carry out adding alkali depickling process; The water-acetonitrile that contains after depickling enters vaporizer after preheater and acetonitrile of high purity steam heat-exchanging; What steam from vaporizer enters Pervaporation membrane separator in vapour form containing water-acetonitrile, and Pervaporation membrane separator feed side obtains acetonitrile of high purity.The present invention is called for short " the anti-film of two towers one " technique, namely instead of the pressure distillation tower in traditional technology with infiltration evaporation device, and its technological process is simple, and facility investment is few, and floor space is little, and capacity usage ratio is high.But because this processing method infiltrating and vaporizing membrane used is expensive, its application is restricted.
Summary of the invention
The object of this invention is to provide the process for refining of by product acetonitrile in a kind of acrylonitrile process, overcome the deficiency in existing crude acetonitrile process for refining.
The technical scheme that the present invention takes is such.A process for refining for by product acetonitrile in acrylonitrile process, comprises the following steps:
(1) the crude acetonitrile solution containing 50% acetonitrile in mass produced in ammoxidating propylene to produce acrylonitrile technique is delivered to decyanation tower and carries out rectifying, remove most prussic acid Yi Ji the lower-boiling impurity such as oxazole, vinylcarbinol, obtain the tower bottoms containing acetonitrile, water and a small amount of high boiling substance;
(2) tower bottoms that step (1) obtains is delivered to reactor, add strong oxidizer and alkali in reactor, prussic acid remaining in tower bottoms and cyanalcohol and alkali carry out neutralization reaction and generate sodium cyanide; Prussic acid and vinyl cyanide react generation succinonitrile in the presence of a base; Under strong oxidizer and alkali existent condition, the impurity reactions such as aldehyde ketone generate carboxylic acid and carboxylate salt high boiling material, obtain the mixture that main component is acetonitrile, water and heavy constituent;
(3) mixture that step (2) obtains is delivered to distillation tower, underpressure distillation removes heavy constituent and the part water such as sodium cyanide, succinonitrile, carboxylic acid, carboxylate salt and propionitrile, and overhead product is the azeotropic mixture of the acetonitrile-water of in mass moisture 10%;
(4) azeotropic mixture of acetonitrile-water step (3) obtained is warming up to 70 DEG C ~ 150 DEG C, infiltration evaporation film device is entered with gaseous state or liquid form, infiltration evaporation film device feed side absolute pressure is regulated to be 0.2 ~ 0.7MPa, the absolute pressure of per-meate side is 0.01 ~ 10KPa, after infiltrating and vaporizing membrane per-meate side vacuumizes cooling, obtain water discharge, obtain the mixture of the acetonitrile-water of in mass moisture 1% ~ 2% in infiltrating and vaporizing membrane feed side;
(5) mixture of the acetonitrile-water of step (4) obtained moisture in mass 1% ~ 2% delivers to distillation tower pressure distillation, obtain at tower bottom the commercial product acetonitrile that quality purity is more than 99.9%, overhead distillate returns delivers to step (3) vacuum still circulation and stress.
In step of the present invention (2), strong oxidizer used is KMnO
4, alkali is NaOH.
In step of the present invention (4), the separatory membrane that infiltration evaporation film device adopts is: molecular screen membrane, Al
2o
3film, SiO
2film, polyvinyl alcohol film, polysulfone membrane, acetyl cellulose film one wherein.
Content or the purity of material involved in the present invention are mass content.
The beneficial effect that the present invention obtains is as follows:
1, compared with traditional " three towers one are anti-" technique, the present invention is " the anti-film of three towers one " technique, infiltration evaporation film device is increased after vacuum still, portion of water in the azeotropic mixture of removing acetonitrile-water, save the energy consumption of the azeotropic mixture vaporization process 30% of the acetonitrile-water distillated from pressurization azeotropic distillation column, reach energy-saving and cost-reducing object.
2, compared with " the anti-film of two towers one " technique, save the consumption of infiltrating and vaporizing membrane, because infiltrating and vaporizing membrane used is expensive, present invention process saves one-time investment.
Accompanying drawing explanation
fig. 1 is process flow sheet of the present invention.
Label implication is wherein: 1-decyanation tower, 2-reactor, 3-vacuum still, 4-interchanger, 5-infiltration evaporation film device, and 6-pressurizes azeotropic distillation column; A-crude acetonitrile solution, B-prussic acid and lower-boiling impurity, C-strong oxidizer and alkali, D-water and heavy constituent, E-water, F-commercial product acetonitrile.
Embodiment
following examples are for illustration of the present invention.
Embodiment 1
(1) the crude acetonitrile solution containing 50% acetonitrile produced in ammoxidating propylene to produce acrylonitrile technique is delivered to decyanation tower and carries out rectifying, to remove most prussic acid Yi Ji the lower-boiling impurity such as oxazole, vinylcarbinol, obtain the tower bottoms that composition is acetonitrile, water and a small amount of high boiling substance;
(2) tower bottoms in (1) is delivered to chemical reaction kettle from the outflow of tower side lower, in chemical reaction kettle, add KMnO
4and NaOH, prussic acid remaining in tower bottoms and cyanalcohol and NaOH carry out neutralization reaction and generate sodium cyanide; Prussic acid and vinyl cyanide react and generate succinonitrile under NaOH exists; At strong oxidizer KMnO
4with under NaOH existent condition, the impurity reactions such as the aldehyde ketone in tower bottoms generate carboxylic acid and carboxylate salt high boiling material, obtain the mixture that main component is acetonitrile, water and heavy constituent;
(3) mixture obtained in (2) is delivered to vacuum still and remove heavy constituent and the part water such as sodium cyanide, succinonitrile and propionitrile, overhead product is the azeotropic mixture of the acetonitrile-water of moisture 10%;
(4) azeotropic mixture of the acetonitrile-water obtained in (3) is warming up to 70 DEG C through interchanger, enter infiltration evaporation film device in liquid form, regulating infiltration evaporation film device raw material to survey absolute pressure is 0.5MPa, the absolute pressure of per-meate side is 2KPa, after infiltrating and vaporizing membrane per-meate side vacuumizes cooling, obtain water discharge, obtain the mixture of the acetonitrile-water of moisture 1% in infiltrating and vaporizing membrane feed side;
(5) mixture of the crude acetonitrile-water of moisture 1% in (4) is delivered to pressurization azeotropic distillation column to distill, obtain at tower bottom the commercial product acetonitrile that purity is more than 99.9%, overhead distillate is returned to vacuum still circulation and stress.
The separatory membrane that the present embodiment infiltration evaporation film device used adopts is molecular screen membrane.
Embodiment 2
(1) the crude acetonitrile solution containing 50% acetonitrile produced in ammoxidating propylene to produce acrylonitrile technique is delivered to decyanation tower and carries out rectifying, to remove most prussic acid Yi Ji the lower-boiling impurity such as oxazole, vinylcarbinol, obtain the tower bottoms that composition is acetonitrile, water and a small amount of high boiling substance;
(2) tower bottoms in (1) is delivered to chemical reaction kettle from the outflow of tower side lower, in chemical reaction kettle, add KMnO
4and NaOH, prussic acid remaining in tower bottoms and cyanalcohol and NaOH carry out neutralization reaction and generate sodium cyanide; Prussic acid and vinyl cyanide react and generate succinonitrile under NaOH exists; At strong oxidizer KMnO
4with under NaOH existent condition, the impurity reactions such as the aldehyde ketone in tower bottoms generate carboxylic acid and carboxylate salt high boiling material, obtain the mixture that main component is acetonitrile, water and heavy constituent;
(3) mixture obtained in (2) is delivered to vacuum still and remove heavy constituent and the part water such as sodium cyanide, succinonitrile and propionitrile, overhead product is the azeotropic mixture of the acetonitrile-water of moisture 10%;
(4) azeotropic mixture of the acetonitrile-water obtained in (3) is warming up to 90 DEG C through interchanger, enter infiltration evaporation film device in liquid form, regulating infiltration evaporation film device raw material to survey absolute pressure is 0.6MPa, the absolute pressure of per-meate side is 1KPa, after infiltrating and vaporizing membrane per-meate side vacuumizes cooling, obtain water discharge, obtain the mixture of the acetonitrile-water of moisture 1.5% in infiltrating and vaporizing membrane feed side;
(5) mixture of the crude acetonitrile-water of moisture 1.5% in (4) is delivered to pressurization azeotropic distillation column to distill, obtain at tower bottom the commercial product acetonitrile that purity is more than 99.9%, overhead distillate is returned to vacuum still circulation and stress.
The separatory membrane that the present embodiment infiltration evaporation device used adopts is Al
2o
3film.
Embodiment 3
(1) the crude acetonitrile solution containing 50% acetonitrile produced in ammoxidating propylene to produce acrylonitrile technique is delivered to decyanation tower and carries out rectifying, to remove most prussic acid Yi Ji the lower-boiling impurity such as oxazole, vinylcarbinol, obtain the tower bottoms that composition is acetonitrile, water and a small amount of high boiling substance;
(2) flowed out from tower side lower by the tower bottoms in (1) and deliver to chemical reaction kettle, in chemical reaction kettle, add KMnO4 and NaOH, prussic acid remaining in tower bottoms and cyanalcohol and NaOH carry out neutralization reaction and generate sodium cyanide; Prussic acid and vinyl cyanide react and generate succinonitrile under NaOH exists; Under strong oxidizer KMnO4 and NaOH existent condition, the impurity reactions such as the aldehyde ketone in tower bottoms generate carboxylic acid and carboxylate salt high boiling material, obtain the mixture that main component is acetonitrile, water and heavy constituent;
(3) mixture obtained in (2) is delivered to vacuum still and remove heavy constituent and the part water such as sodium cyanide, succinonitrile and propionitrile, overhead product is the azeotropic mixture of the acetonitrile-water of moisture 10%;
(4) azeotropic mixture of the acetonitrile-water obtained in (3) is warming up to 130 DEG C through interchanger, enter infiltration evaporation film device in a gaseous form, regulating infiltration evaporation film device raw material to survey absolute pressure is 0.6MPa, the absolute pressure of per-meate side is 1KPa, after infiltrating and vaporizing membrane per-meate side vacuumizes cooling, obtain water discharge, obtain the mixture of the acetonitrile-water of moisture 1.6% in infiltrating and vaporizing membrane feed side;
(5) mixture of the crude acetonitrile-water of moisture 1.6% in (4) is delivered to pressurization azeotropic distillation column to distill, obtain at tower bottom the commercial product acetonitrile that purity is more than 99.9%, overhead distillate is returned to vacuum still circulation and stress.
The separatory membrane that the present embodiment infiltration evaporation device used adopts is SiO2 film.
Embodiment 4
(1) the crude acetonitrile solution containing 50% acetonitrile produced in ammoxidating propylene to produce acrylonitrile technique is delivered to decyanation tower and carries out rectifying, to remove most prussic acid Yi Ji the lower-boiling impurity such as oxazole, vinylcarbinol, obtain the tower bottoms that composition is acetonitrile, water and a small amount of high boiling substance;
(2) tower bottoms in (1) is delivered to chemical reaction kettle from the outflow of tower side lower, in chemical reaction kettle, add KMnO
4and NaOH, prussic acid remaining in tower bottoms and cyanalcohol and NaOH carry out neutralization reaction and generate sodium cyanide; Prussic acid and vinyl cyanide react and generate succinonitrile under NaOH exists; At strong oxidizer KMnO
4with under NaOH existent condition, the impurity reactions such as the aldehyde ketone in tower bottoms generate carboxylic acid and carboxylate salt high boiling material, obtain the mixture that main component is acetonitrile, water and heavy constituent;
(3) mixture obtained in (2) is delivered to vacuum still and remove heavy constituent and the part water such as sodium cyanide, succinonitrile and propionitrile, overhead product is the azeotropic mixture of the acetonitrile-water of moisture 10%;
(4) azeotropic mixture of the acetonitrile-water obtained in (3) is warming up to 150 DEG C through interchanger, enter infiltration evaporation film device in a gaseous form, regulating infiltration evaporation film device raw material to survey absolute pressure is 0.5MPa, the absolute pressure of per-meate side is 0.5KPa, after infiltrating and vaporizing membrane per-meate side vacuumizes cooling, obtain water discharge, obtain the mixture of the acetonitrile-water of moisture 1.2% in infiltrating and vaporizing membrane feed side;
(5) mixture of the crude acetonitrile-water of moisture 1.2% in (4) is delivered to pressurization azeotropic distillation column to distill, obtain at tower bottom the commercial product acetonitrile that purity is more than 99.9%, overhead distillate is returned to vacuum still circulation and stress.
The separatory membrane that the present embodiment infiltration evaporation device used adopts is polyvinyl alcohol film.
Embodiment 5
(1) the crude acetonitrile solution containing 50% acetonitrile produced in ammoxidating propylene to produce acrylonitrile technique is delivered to decyanation tower and carries out rectifying, to remove most prussic acid Yi Ji the lower-boiling impurity such as oxazole, vinylcarbinol, obtain the tower bottoms that composition is acetonitrile, water and a small amount of high boiling substance;
(2) tower bottoms in (1) is delivered to chemical reaction kettle from the outflow of tower side lower, in chemical reaction kettle, add KMnO
4and NaOH, prussic acid remaining in tower bottoms and cyanalcohol and NaOH carry out neutralization reaction and generate sodium cyanide; Prussic acid and vinyl cyanide react and generate succinonitrile under NaOH exists; At strong oxidizer KMnO
4with under NaOH existent condition, the impurity reactions such as the aldehyde ketone in tower bottoms generate carboxylic acid and carboxylate salt high boiling material, obtain the mixture that main component is acetonitrile, water and heavy constituent;
(3) mixture obtained in (2) is delivered to vacuum still and remove heavy constituent and the part water such as sodium cyanide, succinonitrile and propionitrile, overhead product is the azeotropic mixture of the acetonitrile-water of moisture 10%;
(4) azeotropic mixture of the acetonitrile-water obtained in (3) is warming up to 130 DEG C through interchanger, enter infiltration evaporation film device in a gaseous form, regulating infiltration evaporation film device raw material to survey absolute pressure is 0.6MPa, the absolute pressure of per-meate side is 0.5KPa, after infiltrating and vaporizing membrane per-meate side vacuumizes cooling, obtain water discharge, obtain the mixture of the acetonitrile-water of moisture 2% in infiltrating and vaporizing membrane feed side;
(5) mixture of the crude acetonitrile-water of moisture 2% in (4) is delivered to pressurization azeotropic distillation column to distill, obtain at tower bottom the commercial product acetonitrile that purity is more than 99.9%, overhead distillate is returned to vacuum still circulation and stress.
The separatory membrane that the present embodiment infiltration evaporation device used adopts is polysulfone membrane.
Embodiment 6
(1) the crude acetonitrile solution containing 50% acetonitrile produced in ammoxidating propylene to produce acrylonitrile technique is delivered to decyanation tower and carries out rectifying, to remove most prussic acid Yi Ji the lower-boiling impurity such as oxazole, vinylcarbinol, obtain the tower bottoms that composition is acetonitrile, water and a small amount of high boiling substance;
(2) tower bottoms in (1) is delivered to chemical reaction kettle from the outflow of tower side lower, in chemical reaction kettle, add KMnO
4and NaOH, prussic acid remaining in tower bottoms and cyanalcohol and NaOH carry out neutralization reaction and generate sodium cyanide; Prussic acid and vinyl cyanide react and generate succinonitrile under NaOH exists; At strong oxidizer KMnO
4with under NaOH existent condition, the impurity reactions such as the aldehyde ketone in tower bottoms generate carboxylic acid and carboxylate salt high boiling material, obtain the mixture that main component is acetonitrile, water and heavy constituent;
(3) mixture obtained in (2) is delivered to vacuum still and remove heavy constituent and the part water such as sodium cyanide, succinonitrile and propionitrile, overhead product is the azeotropic mixture of the acetonitrile-water of moisture 10%;
(4) azeotropic mixture of the acetonitrile-water obtained in (3) is warming up to 150 DEG C through interchanger, enter infiltration evaporation film device in a gaseous form, regulating infiltration evaporation film device raw material to survey absolute pressure is 0.5MPa, the absolute pressure of per-meate side is 0.5KPa, after infiltrating and vaporizing membrane per-meate side vacuumizes cooling, obtain water discharge, obtain the mixture of the acetonitrile-water of moisture 1.8% in infiltrating and vaporizing membrane feed side;
(5) mixture of the crude acetonitrile-water of moisture 1.8% in (4) is delivered to pressurization azeotropic distillation column to distill, obtain at tower bottom the commercial product acetonitrile that purity is more than 99.9%, overhead distillate is returned to vacuum still circulation and stress.
The separatory membrane that the present embodiment infiltration evaporation device used adopts is acetyl cellulose film.
Content or the purity of the involved material in above-described embodiment are mass content or quality purity.
Claims (3)
1. the process for refining of by product acetonitrile in acrylonitrile process, is characterized in that comprising the following steps:
(1) the crude acetonitrile solution containing 50% acetonitrile in mass produced in ammoxidating propylene to produce acrylonitrile technique is delivered to decyanation tower and carries out rectifying, to remove most prussic acid Yi Ji the lower-boiling impurity such as oxazole, vinylcarbinol, obtain the tower bottoms of acetonitrile, water and a small amount of high boiling substance;
(2) tower bottoms that step (1) obtains is delivered to reactor, add strong oxidizer and alkali in reactor, prussic acid remaining in tower bottoms and cyanalcohol and alkali carry out neutralization reaction and generate sodium cyanide; Prussic acid and vinyl cyanide react generation succinonitrile in the presence of a base; Under strong oxidizer and alkali existent condition, the impurity reactions such as aldehyde ketone generate carboxylic acid and carboxylate salt high boiling material, obtain the mixture that main component is acetonitrile, water and heavy constituent;
(3) mixture that step (2) obtains is delivered to distillation tower, underpressure distillation removes heavy constituent and the part water such as sodium cyanide, succinonitrile, carboxylic acid, carboxylate salt and propionitrile, and overhead product is the azeotropic mixture of the acetonitrile-water of in mass moisture 10%;
(4) azeotropic mixture of acetonitrile-water step (3) obtained is warming up to 70 DEG C ~ 150 DEG C, infiltration evaporation film device is entered with gaseous state or liquid form, infiltration evaporation film device feed side absolute pressure is regulated to be 0.2 ~ 0.7MPa, the absolute pressure of per-meate side is 0.01 ~ 10KPa, after infiltrating and vaporizing membrane per-meate side vacuumizes cooling, obtain water discharge, obtain the mixture of the acetonitrile-water of in mass moisture 1% ~ 2% in infiltrating and vaporizing membrane feed side;
(5) mixture of the acetonitrile-water of step (4) obtained moisture in mass 1% ~ 2% delivers to distillation tower pressure distillation, obtain at tower bottom the commercial product acetonitrile that quality purity is more than 99.9%, overhead distillate returns delivers to step (3) vacuum still circulation and stress.
2. technique according to claim 1, it is characterized in that in step (2), said strong oxidizer is KMnO4, alkali is NaOH.
3. technique according to claim 1, is characterized in that the separatory membrane that in step (4), infiltration evaporation film device adopts is: molecular screen membrane, Al
2o
3film, SiO
2film, polyvinyl alcohol film, polysulfone membrane, acetyl cellulose film one wherein.
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| CN106631890A (en) * | 2016-12-27 | 2017-05-10 | 南京九思高科技有限公司 | Acetonitrile refining technology and device |
| CN109133268A (en) * | 2017-06-16 | 2019-01-04 | 南京大学 | The processing of the industrial wastewater containing acetonitrile and recovery method |
| CN111087530A (en) * | 2018-10-23 | 2020-05-01 | 中国石油化工股份有限公司 | Acrylonitrile composition and process for producing acrylonitrile composition |
| CN112812038A (en) * | 2020-12-30 | 2021-05-18 | 西安瑞联新材料股份有限公司 | Refining process of industrial acetonitrile-containing wastewater |
| CN113501770A (en) * | 2021-08-13 | 2021-10-15 | 中国天辰工程有限公司 | Acetonitrile refining method |
| CN114315641A (en) * | 2022-01-04 | 2022-04-12 | 丽珠集团福州福兴医药有限公司 | Purification and recovery method of acetonitrile waste liquid |
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| CN106631890A (en) * | 2016-12-27 | 2017-05-10 | 南京九思高科技有限公司 | Acetonitrile refining technology and device |
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| CN114315641A (en) * | 2022-01-04 | 2022-04-12 | 丽珠集团福州福兴医药有限公司 | Purification and recovery method of acetonitrile waste liquid |
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Application publication date: 20150506 |