CN107778198A - The processing method of the acrylonitrile of acrylamide is prepared suitable for bioanalysis - Google Patents
The processing method of the acrylonitrile of acrylamide is prepared suitable for bioanalysis Download PDFInfo
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- CN107778198A CN107778198A CN201610747666.2A CN201610747666A CN107778198A CN 107778198 A CN107778198 A CN 107778198A CN 201610747666 A CN201610747666 A CN 201610747666A CN 107778198 A CN107778198 A CN 107778198A
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- acrylonitrile
- acrylamide
- bioanalysis
- processing method
- molecular sieve
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/32—Separation; Purification; Stabilisation; Use of additives
- C07C253/34—Separation; Purification
Abstract
The present invention relates to the production of acrylonitrile, and in particular to a kind of processing method for the acrylonitrile that acrylamide is prepared suitable for bioanalysis.The described processing method for being applied to bioanalysis and preparing the acrylonitrile of acrylamide, is in the production process of acrylonitrile, first active oxidation aluminium ball, molecular sieve combination adsorbent is put into deperoxidation thing tower, then acrylonitrile is handled by deperoxidation thing tower.The present invention is by selecting suitable combination of adsorbents, adjust feeding temperature, drop temperature and the residence time of the acrylonitrile in deperoxidation thing tower, can be by caused 3 hydroxypropionitriles control during deperoxidation thing in a zone of reasonableness, so as to reduce, 3 hydroxypropionitriles are secondary on the poison of hydrase in hydro-combination process to be influenceed, hydrase is kept hydration activity in hydro-combination process, be advantageous to efficiently prepare the acrylamide of high-quality.
Description
Technical field
The present invention relates to the production of acrylonitrile, and in particular to a kind of acrylonitrile that acrylamide is prepared suitable for bioanalysis
Processing method.
Background technology
Acrylonitrile is the important monomer of synthetic fibers, synthetic rubber and synthetic resin.The polyacrylonitrile as made from acrylonitrile
Fiber, i.e. " acrylic fibers ", performance pole is like wool；Nitrile rubber made from acrylonitrile and butadiene copolymer, have good oil resistivity,
Cold resistance, wearability and electrical insulation capability；Acrylonitrile and butadiene, styrene copolymerized obtained ABS resin, have it is light, cold-resistant,
The advantages that shock resistance is good；Acrylamide and acrylicacidandesters class can be made in acrylonitrile hydrolysis, and they are important organic
Industrial chemicals；Acrylonitrile can also electrolytic hydrogenation coupling be made adiponitrile, by adipic dinitrile hydrogenation again can nylon66 fiber processed raw material oneself two
Amine.Recently as acrylonitrile downstream product Dralon, acrylonitrile-butadiene-styrene (ABS) plastics, nitrile rubber, butyronitrile
The development of latex, acrylamide and hexamethylene diamine etc., particularly downstream fine chemistry industry new product being continually developed and applying, generation
The demand of boundary's acrylonitrile is being continuously increased.
The acrylonitrile in the whole world more than 95% is all produced using Sohio methods now.The technique is with chemical grade propylene and fertilizer grade
Ammonia and air are sent into fluidized-bed catalytic reactor by the amount of material than 1.0: 1.15~1.25: 9.3~10.Catalyst uses two
Silica supported BiPMo.While acrylonitrile is generated, by-product hydrogen cyanide, acetonitrile, propionitrile, acetone, acetaldehyde, acetic acid are gone back
Deng accessory substance.The typical process flow of Sohio propylene ammmoxidation process is：Reaction product enters after being come out from reactor head to be neutralized
Tower, with ammonia not reacted in sulfuric acid and ammonium sulfate washed product；Product enters water scrubber after tower top is neutralized out,
Nitrogen, carbon monoxide, carbon dioxide and unreacted hydrocarbon are not soluble in water, are expelled directly out or burn from tower top as tail gas, acrylonitrile,
Acetonitrile and hydrogen cyanide are soluble in water from the outflow of water scrubber bottom；Water scrubber bottoms enters water extractive distillation column, by acrylonitrile, acetonitrile
Separated with hydrogen cyanide, each component separated respectively enters 3 rectifying columns and is subject to rectifying, and then obtains acrylonitrile product
With acetonitrile and hydrogen cyanide byproduct.
But the acrylonitrile of above method production is used nitrile hydratase work easily occur when bioanalysis prepares acrylamide
Property reduce, hydration reaction batch is reduced, the problems such as acrylamide quality fluctuation is larger.
Research is found, when progress acrylonitrile hydration reaction prepares acrylamide, if containing excessive 3- in acrylonitrile
Hydroxypropionitrile impurity, then great harmful effect can be produced to the catalytic activity of nitrile hydratase so that enzymatic activity reduces, and hydration is anti-
Batch is answered to reduce, the residual acrylonitrile eventually resulted in acrylamide is exceeded.And in acrylonitrile process, due in acrylonitrile
Peroxide impurity can influence acrylonitrile quality, it is necessary to acrylonitrile carry out deperoxidation thing processing, such as patent
Exactly peroxide is removed in CN103446801A using aluminum oxide as adsorbent.But acrylonitrile is in deperoxidation thing
During can inevitably produce 3- hydroxypropionitriles.
The content of the invention
It is an object of the invention to provide a kind of processing method for the acrylonitrile that acrylamide is prepared suitable for bioanalysis, improve
The nitrile hydratase activity that acrylonitrile occurs in use is reduced, and hydration reaction batch is reduced, and acrylamide quality fluctuation is larger
Problem.
The processing method of the acrylonitrile of the present invention that acrylamide is prepared suitable for bioanalysis, is the life in acrylonitrile
During production, first active oxidation aluminium ball, molecular sieve combination adsorbent are put into deperoxidation thing tower, then by acrylonitrile by de-
Peroxide tower is handled.
In the processing procedure of aforesaid propylene nitrile, in the active oxidation aluminium ball and molecular sieve combination adsorbent, active oxygen
The mass ratio for changing aluminium ball and molecular sieve is 1: 0.9~1.1, preferably 1: 1.
In the processing procedure of aforesaid propylene nitrile, a diameter of 3.0~3.5mm of the active oxidation aluminium ball, pore volume is
0.38~0.4cm3/ g, intensity are 50~80N/ grains, heap density >=0.75g/cm3.The pore volume of active oxidation aluminium ball is surveyed using BET
Examination method, intensity, the heap density of active oxidation aluminium ball are tested using national standard.
In the processing procedure of aforesaid propylene nitrile, a diameter of 3~5mm of the molecular sieve, compression strength is >=70N, point
The bulk density of son sieve is 0.68g/mL.The compression strength of molecular sieve, the bulk density of molecular sieve are tested using national standard.
In the processing procedure of aforesaid propylene nitrile, the feeding temperature that the acrylonitrile enters deperoxidation thing tower is 22~25
℃。
In the processing procedure of aforesaid propylene nitrile, the drop temperature that the acrylonitrile goes out deperoxidation thing tower is 20 DEG C.
In the processing procedure of aforesaid propylene nitrile, the acrylonitrile in deperoxidation thing tower the residence time be 0.5~
2.5min。
Beneficial effects of the present invention are as follows：
The present invention by selecting suitable combination of adsorbents, adjust acrylonitrile in deperoxidation thing tower feeding temperature,
Drop temperature and residence time, can be by caused 3- hydroxypropionitriles control during deperoxidation thing in≤50ppm such one
In individual rational scope, so as to reduce 3- hydroxypropionitriles in hydro-combination process to the secondary influence of the poison of nitrile hydratase, make nitrile hydratase
Hydration activity is kept in hydro-combination process, is advantageous to efficiently prepare the acrylamide of high-quality.
Embodiment
The present invention is described further with reference to embodiments.
Embodiment 1
By bulb diameter it is 3mm, pore volume 0.38cm by acrylonitrile that temperature is 22 DEG C3/ g, intensity are 50N/ grains, and heap is close
Spend 0.75g/cm3Activated alumina and heap density be 0.68g/mL, compression strength >=70N, a diameter of 3mm molecular sieve it is de-
The mass ratio of peroxide tower, active oxidation aluminium ball and molecular sieve mixture is 1: 1, passage time 0.5min, acrylonitrile
Drop temperature is 20 DEG C, and the content of the 3- hydroxypropionitriles in the acrylonitrile finally given is 50ppm.
Embodiment 2
By bulb diameter it is 3.5mm, pore volume 0.38cm by acrylonitrile that temperature is 25 DEG C3/ g, intensity are 50N/ grains, heap
Density 0.85g/cm3Activated alumina and heap density be 0.68g/mL, compression strength >=70N, a diameter of 3mm molecular sieve
The mass ratio of deperoxidation thing tower, active oxidation aluminium ball and molecular sieve mixture is 1: 1, passage time 0.5min, acrylonitrile
Drop temperature be 20 DEG C, the content of the 3- hydroxypropionitriles in the acrylonitrile finally given is 40ppm.
Embodiment 3
By bulb diameter it is 3.2mm, pore volume 0.4cm by acrylonitrile that temperature is 23 DEG C3/ g, intensity are 50N/ grains, heap
Density 0.81g/cm3Activated alumina and heap density be 0.68g/mL, compression strength >=70N, a diameter of 3mm molecular sieve
The mass ratio of deperoxidation thing tower, active oxidation aluminium ball and molecular sieve mixture is 1: 1, passage time 0.5min, acrylonitrile
Drop temperature be 20 DEG C, the content of the 3- hydroxypropionitriles in the acrylonitrile finally given is 35ppm.
Embodiment 4
By bulb diameter it is 3mm, pore volume 0.38cm by acrylonitrile that temperature is 22 DEG C3/ g, intensity are 80N/ grains, and heap is close
Spend 0.88g/cm3Activated alumina and heap density be 0.68g/mL, compression strength >=70N, a diameter of 5mm molecular sieve it is de-
The mass ratio of peroxide tower, active oxidation aluminium ball and molecular sieve mixture is 1: 1, passage time 2.5min, acrylonitrile
Drop temperature is 20 DEG C, and the content in the 3- hydroxypropionitriles of the acrylonitrile finally given is 45ppm.
Embodiment 5
By bulb diameter it is 3.4mm, pore volume 0.39cm by acrylonitrile that temperature is 24 DEG C3/ g, intensity are 70N/ grains, heap
Density 0.82g/cm3Activated alumina and heap density be 0.68g/mL, compression strength >=70N, a diameter of 4mm molecular sieve
The mass ratio of deperoxidation thing tower, active oxidation aluminium ball and molecular sieve mixture is 1: 0.9, passage time 2min, acrylonitrile
Drop temperature be 20 DEG C, the content in the 3- hydroxypropionitriles of the acrylonitrile finally given is 41ppm.
Embodiment 6
By bulb diameter it is 3.5mm, pore volume 0.38cm by acrylonitrile that temperature is 23 DEG C3/ g, intensity are 65N/ grains, heap
Density 0.77g/cm3Activated alumina and heap density be 0.68g/mL, compression strength >=70N, a diameter of 3mm molecular sieve
The mass ratio of deperoxidation thing tower, active oxidation aluminium ball and molecular sieve mixture is 1: 1, passage time 1.5min, acrylonitrile
Drop temperature be 20 DEG C, the content in the 3- hydroxypropionitriles of the acrylonitrile finally given is 33ppm.
Embodiment 7
By bulb diameter it is 3.1mm, pore volume 0.38cm by acrylonitrile that temperature is 22 DEG C3/ g, intensity are 75N/ grains, heap
Density 0.77g/cm3Activated alumina and heap density be 0.68g/mL, compression strength >=70N, a diameter of 3.5mm molecular sieve
Deperoxidation thing tower, the mass ratio of active oxidation aluminium ball and molecular sieve mixture is 1: 1.1, passage time 1.2min, third
The drop temperature of alkene nitrile is 20 DEG C, and the content of the 3- hydroxypropionitriles in the acrylonitrile finally given is 37ppm.
Embodiment 8
By bulb diameter it is 3mm, pore volume 0.4cm by acrylonitrile that temperature is 24 DEG C3/ g, intensity are 55N/ grains, and heap is close
Spend 0.86/cm3Activated alumina and heap density be 0.68g/mL, compression strength >=70N, a diameter of 3mm molecular sieve it is de-
The mass ratio of peroxide tower, active oxidation aluminium ball and molecular sieve mixture is 1: 0.9, passage time 1.2min, acrylonitrile
Drop temperature be 20 DEG C, the content in the 3- hydroxypropionitriles of the acrylonitrile finally given is 32ppm.
Comparative example 1
By bulb diameter it is 4mm, pore volume 0.38cm by acrylonitrile that temperature is 15 DEG C3/ g, intensity are 60N/ grains, and heap is close
Spend 0.75g/cm3Activated alumina deperoxidation thing tower, passage time 0.2min, the drop temperature of acrylonitrile is 20 DEG C,
Content in the 3- hydroxypropionitriles of the acrylonitrile finally given is 100ppm.
Comparative example 2
By bulb diameter it is 4mm, pore volume 0.38cm by acrylonitrile that temperature is 17 DEG C3/ g, intensity are 60N/ grains, and heap is close
Spend 0.75g/cm3Activated alumina deperoxidation thing tower, passage time 4min, the drop temperature of acrylonitrile is 20 DEG C, most
Content in the 3- hydroxypropionitriles of the acrylonitrile obtained eventually is 100ppm.
Claims (8)
- A kind of 1. processing method for the acrylonitrile that acrylamide is prepared suitable for bioanalysis, it is characterised in that：In the life of acrylonitrile During production, first active oxidation aluminium ball and molecular sieve combination adsorbent are put into deperoxidation thing tower, then by acrylonitrile through de- Peroxide tower is handled.
- 2. the processing method of the acrylonitrile according to claim 1 that acrylamide is prepared suitable for bioanalysis, its feature exist In：In the active oxidation aluminium ball and molecular sieve combination adsorbent, the mass ratio of active oxidation aluminium ball and molecular sieve for 1: 0.9~ 1.1。
- 3. the processing method of the acrylonitrile according to claim 2 that acrylamide is prepared suitable for bioanalysis, its feature exist In：In the active oxidation aluminium ball and molecular sieve combination adsorbent, the mass ratio of active oxidation aluminium ball and molecular sieve is 1: 1.
- 4. the processing method of the acrylonitrile according to claim 1 that acrylamide is prepared suitable for bioanalysis, its feature exist In：A diameter of 3.0~3.5mm of the active oxidation aluminium ball, pore volume are 0.38~0.4cm3/ g, intensity are 50~80N/ grains, Heap density >=0.75g/cm3。
- 5. the processing method of the acrylonitrile according to claim 1 that acrylamide is prepared suitable for bioanalysis, its feature exist In：A diameter of 3~5mm of the molecular sieve, compression strength are >=70N, and the bulk density of molecular sieve is 0.68g/mL.
- 6. the processing method of the acrylonitrile according to claim 1 that acrylamide is prepared suitable for bioanalysis, its feature exist In：The feeding temperature that the acrylonitrile enters deperoxidation thing tower is 22~25 DEG C.
- 7. the processing method of the acrylonitrile according to claim 1 that acrylamide is prepared suitable for bioanalysis, its feature exist In：The drop temperature that the acrylonitrile goes out deperoxidation thing tower is 20 DEG C.
- 8. the processing method for being applied to bioanalysis and preparing the acrylonitrile of acrylamide according to claim 1~7 is any, its It is characterised by：Acrylonitrile residence time in deperoxidation thing tower is 0.5~2.5min.
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Cited By (3)
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| CN108976149A (en) * | 2017-05-31 | 2018-12-11 | 中国石油化工股份有限公司 | The acrylonitrile and preparation method thereof of acrylamide is prepared suitable for bioanalysis |
| CN110511160A (en) * | 2019-08-06 | 2019-11-29 | 浙江中科恒泰新材料科技有限公司 | A kind of method that (methyl) acrylamide dehydration prepares (methyl) acrylonitrile |
| CN110724068A (en) * | 2018-07-16 | 2020-01-24 | 中国石油化工股份有限公司 | Process for producing high-purity acrylonitrile |
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| CN110724068A (en) * | 2018-07-16 | 2020-01-24 | 中国石油化工股份有限公司 | Process for producing high-purity acrylonitrile |
| CN110511160A (en) * | 2019-08-06 | 2019-11-29 | 浙江中科恒泰新材料科技有限公司 | A kind of method that (methyl) acrylamide dehydration prepares (methyl) acrylonitrile |
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Application publication date: 20180309 |