CN107779482A - A kind of production technology of high concentration acrylamide - Google Patents
A kind of production technology of high concentration acrylamide Download PDFInfo
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- CN107779482A CN107779482A CN201711264021.4A CN201711264021A CN107779482A CN 107779482 A CN107779482 A CN 107779482A CN 201711264021 A CN201711264021 A CN 201711264021A CN 107779482 A CN107779482 A CN 107779482A
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Abstract
The present invention relates to a kind of production technology of high concentration acrylamide, by one-level membrane bioreactor, two level membrane bioreactor, three-level membrane bioreactor ... N level membrane bioreactors are connected by series system, wherein N is the natural number more than 1, two level membrane bioreactor, three-level membrane bioreactor ... N levels membrane bioreactor sets up the parallel way (N 1 of different numbers as needed, N 2, ... N X), any one (N 1) 1 of N levels membrane bioreactor and 1 grade of membrane bioreactor of N, (N 1) 2, ... (N 1) X is connected in a series arrangement, wherein N and X is the natural number more than 1.Efficiently, stably, continuous production, the efficiency of biocatalyst is taken full advantage of, acrylamide terminates AM concentration and is obviously improved, and utilization rate of equipment and installations, unit volume equipment capacity are substantially improved, production cost and energy consumption of unit product are reduced, unit product quantity of wastewater effluent is greatly reduced.
Description
Technical field
The invention belongs to biocatalytic reaction technology field, and in particular to a kind of production work of high concentration acrylamide
Skill.
Background technology
Acrylamide (AM) is a kind of widely used organic chemical industry's intermediate, and main production is with nitrile hydratase production
Thalline is biocatalyst, and substrate acrylonitrile (AN) and water are catalyzed in single reactor and carry out hydration reaction, generates product
Acrylamide (AM) solution.With technology of biological membrane by product propylene amide aqueous solution (small molecule) and mycetome reaction system
(macromolecular) separates, and obtains crude propylene amide solution, crude propylene amide solution obtains fine propylene after a series of refined means
Amide solution.
Nitrile hydratase is the leading enzyme that acrylamide produces bacterial strain, but a small amount of amidase, energy be present simultaneously in bacterial strain
It is enough that acrylamide product catalyst is produced into acrylic acid accessory substance, if there is the feelings for not having acrylonitrile and activity also affluence in system
Condition, it becomes possible to the acrylamide generated is continued into catalysis generation acrylic acid accessory substance, causes overall production efficiency to decline, after
Phase refines cost and increased.
Nitrile hydratase has significant product (i.e. acrylamide AM) inhibitory action simultaneously, enzymatic activity with production concentration rise
Inhibitory action is strengthened, so with the extension of catalytic cycle and the simultaneous AM aqueous solution being stepped up in reaction system
Dual-pressure under, catalytic activity declines very fast.
At present, bioanalysis acrylamide production technology mainly has free cell batch (-type) hydration reaction technique and continuous hydration
Reaction process.According to the demand of current produce reality, there are some technological deficiencies in both production technologies:
1st, the technological deficiency of free cell batch (-type) hydration reaction technique:
Free cell batch (-type) hydration reaction technique, the process for producing acrylamide are batch (-type)s, product generating process
Progress asynchronous with product separation process, with gradually raising and the extension of reaction time of production concentration in reaction solution, urge
After long-time immersion in highly concentrated product solution mass change occurs for agent catalytic efficiency, it is difficult to produce the third of higher concentration
Acrylamide solution and product quality fluctuate larger, production efficiency reduction, and product design is single.
2nd, the technical disadvantages of serialization hydration reaction production acrylamide technique:
Serialization hydration reaction technique is that one-pot is continuous or multi-floating bodies production technology at present, although can continuous output third
Acrylamide, especially multi-floating bodies are with the increase of the order of reaction, and output acrylamide concentration also gradually increases, by different
The height of the catalytic reaction efficiency of biocatalyst caused by production concentration inhibitory action in differential responses series is different, in order to
Reach the balance of W-response system liquid level concentration, catalytic activity occurs in the acrylonitrile dosage deficiency of the reaction system of lower level
It is significantly superfluous, generate acrylic acid accessory substance so as to be catalyzed the acrylamide generated.Most greatly nitrile amount by afterbody height
Biocatalyst efficiency under dense acrylamide solution high inhibition effect determines that W-response substrate acrylonitrile adding speed is not
Height, reaction time length, biocatalyst are influenceed by product inhibition for a long time, cause the generation of accessory substance acrylic acid to increase,
Product quality and production efficiency decline.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of new particularly with longer feelings reaction time
The production technology of high concentration acrylamide aqueous solution under condition, make full use of the living things catalysis in different series biological respinse systems
Agent efficiency, improve speed of production;Improve product and finally terminate concentration of aqueous solution, reduce the generation of accessory substance, reduce production cost.
The technical solution adopted for the present invention to solve the technical problems is:A kind of production technology of high concentration acrylamide,
Comprise the following steps:
1) by one-level membrane bioreactor, two level membrane bioreactor, three-level membrane bioreactor ... N level membrane bioreactions
Device is answered to be connected by series system, wherein N is the natural number more than 1;Two level membrane bioreactor, three-level membrane biological reaction
Device ... N levels membrane bioreactor sets up parallel way (N-1, N- of different numbers according to production requirement and catalyst activity
2nd ... N-X), any one (N-1) -1 of N levels membrane bioreactor and N-1 level membrane bioreactors, (N-1) -2 ...
(N-1)-X is connected in a series arrangement, and wherein N and X are the natural number more than 1;
2) biocatalyst is squeezed into the one-level film biology through over cleaning by the 10%-20% of reaction solution cumulative volume before reaction
In the reactor of reactor 1, stirring is opened, 17-20 DEG C of control hydration reaction temperature, starts to react to one-level membrane bioreactor 1
Current adding substrate acrylonitrile and water in kettle, by the catalytic action of nitrile hydratase, generate product propylene acid amides;When one-level membrane bioreaction
Device 1 is answered to react after acrylamide solution concentration reaches technological requirement in kettle liquid, by one-level membrane bioreactor membrane module system
Lock out operation be continuously available acrylamide permeate and the phegma containing biocatalyst, phegma returns by reflux pipeline
In one-level membrane bioreactor reactor, acrylamide permeate respectively enters the multiple in parallel of two level membrane bioreactor 2
In reactor;
3) when the reactor liquid level of two level membrane bioreactor 2 to regulation scale, the biocatalyst through over cleaning is pressed
The 20%-30% of reaction solution cumulative volume is separately added into multiple reactors in parallel of two level membrane bioreactor 2 before reaction, control
20-23 DEG C of temperature processed, then start the current adding substrate acrylonitrile into multiple reactors of two level membrane bioreactor 2, acrylonitrile
Hydration reaction generation acrylamide is carried out with the water in one-level membrane bioreactor acrylamide permeate;When two level membrane bioreaction
Answer after acrylamide solution concentration reaches technological requirement in device 2, carry out lock out operation by membrane module system, successively obtain
High concentration acrylamide permeate and the phegma containing biocatalyst, phegma return to two level membrane bioreaction by reflux pipeline
Answer in the reactor of device 2, acrylamide permeate enters in multiple reactors in parallel of three-level membrane bioreactor 3;
4) membrane bioreactors at different levels are after production concentration reaches technological standards requirement, the aqueous solution of the acid amides containing product propylene
Entering next stage membrane bioreactor through membrane module, the phegma containing biocatalyst is returned in this order reaction system, until
Acrylamide permeate enters N level membrane bioreactors;
5) N levels membrane bioreactor is after production concentration reaches technological standards requirement, the aqueous solution of the acid amides containing product propylene
Enter product storage tank through membrane module, phegma containing biocatalyst is returned in this order reaction system.
Specifically, highly concentrated link i.e. N levels membrane bioreactor can be arranged on according to production requirement product storage tank, can also set
Put after any level membrane bioreactor;Product propylene acid amides, water can be further separated into product through membrane module in highly concentrated link
Storage tank, can also voluntarily production requirement sets up shunting products pot in low dense link according to company.
Specifically, the biocatalyst selection in the step 2) can produce nitrile hydratase Nocard's bacillus or Rhodococcus sp and
Its mutagenic strain.
The invention has the advantages that:The present invention high concentration acrylamide production technology, efficiently, stably,
Continuous production, compared with prior art, the present invention take full advantage of the efficiency of biocatalyst, and acrylamide terminates AM concentration
It is obviously improved, utilization rate of equipment and installations, unit volume equipment capacity are substantially improved, and reduce production cost and energy consumption of unit product, single
Position product quantity of wastewater effluent is greatly reduced.
Brief description of the drawings
Fig. 1 is the production technological process of high concentration acrylamide of the present invention.
Fig. 2 is the production technological process of the acrylamide of the embodiment of the present invention 1.
Embodiment
It is the specific embodiment of the present invention below, technical scheme is described further, but the present invention
Protection domain is not limited to these embodiments.It is every to be included in the present invention without departing substantially from the change of present inventive concept or equivalent substitute
Protection domain within.
As shown in figure 1, a kind of production technology of high concentration acrylamide, comprises the following steps:
1) by one-level membrane bioreactor, two level membrane bioreactor, three-level membrane bioreactor ... N level membrane bioreactions
Device is answered to be connected by series system, wherein N is the natural number more than 1;Two level membrane bioreactor, three-level membrane biological reaction
Device ... N levels membrane bioreactor sets up parallel way (N-1, N- of different numbers according to production requirement and catalyst activity
2nd ... N-X), any one (N-1) -1 of N levels membrane bioreactor and N-1 level membrane bioreactors, (N-1) -2 ...
(N-1)-X is connected in a series arrangement, and wherein N and X are the natural number more than 1;
2) biocatalyst is squeezed into the one-level film biology through over cleaning by the 10%-20% of reaction solution cumulative volume before reaction
In reactor reaction kettle, stirring is opened, 17-20 DEG C of control hydration reaction temperature, is started to one-level membrane bioreactor reactor
Middle current adding substrate acrylonitrile and water, by the catalytic action of nitrile hydratase, generate product propylene acid amides;When one-level membrane biological reaction
After acrylamide solution concentration reaches technological requirement in device reaction kettle liquid, by point of one-level membrane bioreactor membrane module system
Acrylamide permeate and phegma containing biocatalyst are continuously available from operation, phegma returns to one-level by reflux pipeline
In membrane bioreactor reactor, acrylamide permeate respectively enters multiple reactors in parallel of two level membrane bioreactor
In;
3) when two level membrane bioreactor reactor liquid level to regulation scale, by the biocatalyst through over cleaning by anti-
The 20%-30% of reaction solution cumulative volume is separately added into multiple reactors in parallel of two level membrane bioreactor before answering, and is controlled
20-23 DEG C of temperature, then start the current adding substrate acrylonitrile into multiple reactors of two level membrane bioreactor, acrylonitrile and one
Water in level membrane bioreactor acrylamide permeate carries out hydration reaction generation acrylamide;When two level membrane bioreactor
After middle acrylamide solution concentration reaches technological requirement, lock out operation is carried out by membrane module system, is successively obtained highly concentrated
Acrylamide permeate and the phegma containing biocatalyst are spent, phegma returns to two level membrane bioreactor by reflux pipeline
In reactor, acrylamide permeate enters in multiple reactors in parallel of three-level membrane bioreactor;
4) membrane bioreactors at different levels are after production concentration reaches technological standards requirement, the aqueous solution of the acid amides containing product propylene
Entering next stage membrane bioreactor through membrane module, the phegma containing biocatalyst is returned in this order reaction system, until
Acrylamide permeate enters N level membrane bioreactors;
5) N levels membrane bioreactor is after production concentration reaches technological standards requirement, the aqueous solution of the acid amides containing product propylene
Enter product storage tank through membrane module, phegma containing biocatalyst is returned in this order reaction system.
Embodiment 1
By taking simplest connection in series-parallel production technology as an example, it is made up of 3 membrane bioreactors.Two level membrane bioreactor 2-
1 is connected in parallel with two level membrane bioreactor 2-2, after one-level membrane bioreactor 1, one-level membrane bioreactor 1 with
Two level membrane bioreactor 2-1, two level membrane bioreactor 2-2 reactors are connected in series respectively, as shown in Figure 2.
Urged from the Nocard's bacillus or Rhodococcus sp and its mutagenic strain that can produce nitrile hydratase as the biology of hydration reaction
Agent.
Qualified biocatalyst will be cultivated by the 10%-20% of reaction solution cumulative volume before reaction and squeezes into one through over cleaning
In the level reactor of membrane bioreactor 1, stirring is opened.17-20 DEG C of hydration reaction temperature is controlled, is started to one-level membrane biological reaction
Current adding substrate acrylonitrile and water in the reactor of device 1, by the catalytic action of nitrile hydratase, generate product propylene acid amides.
After acrylamide solution concentration reaches technological requirement 30% in the reaction kettle liquid of one-level membrane bioreactor 1, pass through
The lock out operation (aqueous solution containing acrylamide can pass through) of one-level membrane bioreactor membrane module system, is continuously available propylene
Acid amides permeate and the phegma containing biocatalyst.Phegma returns to one-level membrane bioreactor 1 by reflux pipeline and reacted
In kettle, the acrylamide aqueous solution permeate of 30% concentration enters in two level membrane bioreactor 2-1,2-2 reactor.
AM concentration is relatively low in one-level membrane bioreactor 1, so the Product inhibiton effect of catalyst is minimum, AN dosage
Larger, speed of production lifting can be controlled, the balance control for being diverted to two two levels can be met completely.
When two level membrane bioreactor reactor liquid level is to when providing scale, by the biocatalyst through over cleaning, by anti-
The 20%-30% of reaction solution cumulative volume is separately added into two level membrane bioreactor 2-1,2-2 reactor before answering, and controls temperature
20-23 DEG C, then start current adding substrate acrylonitrile and one-level membrane bioreactor acrylamide into two level membrane bioreactor
Water in permeate carries out hydration reaction generation acrylamide.When acrylamide solution concentration reaches in two level membrane bioreactor
After technological requirement 40%, by membrane module system carry out lock out operation, successively obtain high concentration acrylamide permeate and
Phegma.Phegma is returned in two level membrane bioreactor reactor by reflux pipeline, and 40% acrylamide aqueous solution passes through
Liquid enters in products pot.
The biocatalyst of two membrane bioreactors of two level is now due to Product inhibiton, and AN dosages are less than one-level film biology
The reactor of reactor.
The final liquid level equilibrium control for realizing three reactors, reaches the stabilization of the AM concentration in kettles at different levels and terminates level
The output of the high concentration AM aqueous solution, the charging cumulative volume and the discharging cumulative volume of two two levels of one-level remain basically stable.
The present invention is not limited to the above-described embodiments, and anyone should learn that the structure made under the enlightenment of the present invention becomes
Change, the technical schemes that are same or similar to the present invention, each fall within protection scope of the present invention.
The present invention be not described in detail technology, shape, construction part be known technology.
Claims (3)
1. a kind of production technology of high concentration acrylamide, it is characterised in that comprise the following steps:
1) by one-level membrane bioreactor, two level membrane bioreactor, three-level membrane bioreactor ... N level membrane bioreactors
Connected by series system, wherein N is the natural number more than 1;Two level membrane bioreactor, three-level membrane bioreactor ... N
Level membrane bioreactor according to production requirement and catalyst activity set up different numbers parallel way (N-1, N-2 ... N-
X), any one (N-1) -1 of N levels membrane bioreactor and N-1 level membrane bioreactors, (N-1) -2 ... (N-1)-X with
Series system connection, wherein N and X are the natural number more than 1;
2) biocatalyst is squeezed into the one-level membrane biological reaction through over cleaning by the 10%-20% of reaction solution cumulative volume before reaction
In device reactor, stirring is opened, 17-20 DEG C of control hydration reaction temperature, starts to flow into one-level membrane bioreactor reactor
Add substrate acrylonitrile and water, by the catalytic action of nitrile hydratase, generate product propylene acid amides;When one-level membrane bioreactor is anti-
Answer after acrylamide solution concentration reaches technological requirement in kettle liquid, the separation behaviour by one-level membrane bioreactor membrane module system
Acrylamide permeate and the phegma containing biocatalyst are continuously available, phegma returns to the life of one-level film by reflux pipeline
In thing reactor reaction kettle, acrylamide permeate is respectively enterd in multiple reactors in parallel of two level membrane bioreactor;
3) when two level membrane bioreactor reactor liquid level to regulation scale, before the biocatalyst through over cleaning is pressed into reaction
The 20%-30% of reaction solution cumulative volume is separately added into multiple reactors in parallel of two level membrane bioreactor, controls temperature
20-23 DEG C, then start the current adding substrate acrylonitrile into multiple reactors of two level membrane bioreactor, acrylonitrile and one-level film
Water in bioreactor acrylamide permeate carries out hydration reaction generation acrylamide;When third in two level membrane bioreactor
After acrylamide solution concentration reaches technological requirement, lock out operation is carried out by membrane module system, successively obtains high concentration third
Acrylamide permeate and the phegma containing biocatalyst, phegma return to the reaction of two level membrane bioreactor by reflux pipeline
In kettle, acrylamide permeate enters in multiple reactors in parallel of three-level membrane bioreactor;
4) after production concentration reaches technological standards requirement, the aqueous solution of the acid amides containing product propylene passes through membrane bioreactors at different levels
Membrane module enters next stage membrane bioreactor, and the phegma containing biocatalyst is returned in this order reaction system, until propylene
Acid amides permeate enters N level membrane bioreactors;
5) after production concentration reaches technological standards requirement, the aqueous solution of the acid amides containing product propylene passes through N levels membrane bioreactor
Membrane module enters product storage tank, and phegma containing biocatalyst is returned in this order reaction system.
2. the production technology of high concentration acrylamide as claimed in claim 1, it is characterised in that stored up according to production requirement product
After tank can be arranged on any level membrane bioreactor.
3. the production technology of high concentration acrylamide as claimed in claim 1, it is characterised in that the biology in the step 2)
Catalyst selection can produce the Nocard's bacillus or Rhodococcus sp and its mutagenic strain of nitrile hydratase.
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CN112522337A (en) * | 2020-11-16 | 2021-03-19 | 广东宝莫生物化工有限公司 | Continuous production method of acrylamide solution |
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