CN102286560A - Method for continuously producing acrylamide solution by using multi-level membrane bioreactors - Google Patents
Method for continuously producing acrylamide solution by using multi-level membrane bioreactors Download PDFInfo
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- CN102286560A CN102286560A CN201110165460A CN201110165460A CN102286560A CN 102286560 A CN102286560 A CN 102286560A CN 201110165460 A CN201110165460 A CN 201110165460A CN 201110165460 A CN201110165460 A CN 201110165460A CN 102286560 A CN102286560 A CN 102286560A
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Abstract
The invention discloses a method for continuously producing acrylamide solution by using multi-level membrane bioreactors. The multi-level membrane bioreactors are connected with one another in series. A membrane bioreactor device is formed by coupling a membrane component and a reaction kettle, wherein the membrane component is one of a hollow fibrous membrane, a ceramic membrane and a rolled membrane; a biological catalyst of each level membrane bioreactor is only circulated in the membrane bioreactor of the same level and cannot penetrate the membrane component to flow into the membrane bioreactor of the next level; and in membrane bioreactors of all levels, after the product concentration reaches the process standard requirement, the products of acrylamide, water and acrylonitrile and the byproduct of acrylic acid can penetrate the membrane component to enter the membrane bioreactor of the next level and are separated from the biological catalyst.
Description
Technical field
The present invention relates to biocatalytic reaction Technology field, the thalline that utilization produces Nitrile hydratase is a biological catalyst, the method that acrylamide soln is produced in three to ten grades of membrane bioreactor series connection of especially a kind of utilization serialization.
Background technology
Acrylamide (AM) is a kind of broad-spectrum organic chemical industry's intermediate, its main production is to be substrate with vinyl cyanide (AN) and water, the thalline that produces Nitrile hydratase is a biological catalyst, carries out hydration reaction in retort, generates product acrylamide (AM).The utilization technology of biological membrane is separated the product acrylamide with reaction system (mycetome), obtain the crude propylene amide solution, and the crude propylene amide solution finally obtains the fine propylene amide solution through a series of filtering membranes, ion exchange bed.
At present, the acrylamide production technique mainly contains free cell intermittent type hydration reaction technology and single-stage serialization hydration reaction technology.According to the demand of present production reality, there are some technological deficiencies in these two kinds of production technique.
1, the technological deficiency of free cell intermittent type hydration reaction technology:
(1) free cell intermittent type hydration reaction technology, the process of producing acrylamide is step.The product generative process is asynchronous with the product sepn process carries out, and biological catalyst is not brought into play biocatalytic Activity at the acrylamide separation phase.Biological catalyst is to be subjected to substrate and product to suppress the biological enzyme that influences, and is subjected to restraining effect, service efficiency and the decline of Nitrile hydratase activity of high density product at product separation phase biological catalyst.
(2) free cell intermittent type hydration reaction technology, acrylamide soln that can only output 250g/L to 300g/L scope is difficult to produce the acrylamide soln of high density.
(3) free cell intermittent type hydration reaction technology, owing to be subjected to the influence of factors such as vinyl cyanide flow acceleration, enzymic activity, temperature control, the acrylic acid generation of by product, the acrylamide quality fluctuation of generation is bigger.
2, single-stage serialization hydration reaction is produced the technical disadvantages of acrylamide technology:
(1) single-stage serialization hydration reaction technology, though the continuous output acrylamide of energy, biological catalyst was immersed in the reaction solution in the hydration reaction process midium or long term, the substrate restraining effect is bigger to the Nitrile hydratase activity influence.
(2) single-stage serialization hydration reaction technology, though substrate adding speed is relatively stable, flow acceleration is not high, the reaction times is longer.Biological catalyst is subjected to the influence of product acrylamide restraining effect for a long time, causes the acrylic acid generation of by product to increase, and quality product and production efficiency descend.
(3) single-stage serialization hydration reaction technology, in the production process of acrylamide, the acrylamide of output 250g/L to 300g/L scope is difficult to satisfy the requirement of producing reality continuously.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of multistage membrane bioreactor serialization to produce the method for acrylamide soln at the deficiencies in the prior art.
The method that acrylamide soln is produced in multistage membrane bioreactor series connection serialization, multistage membrane bioreactor connects by series system; Described film bioreactor device is formed by membrane module and reactor coupling; Described membrane module is one of hollow-fibre membrane, ceramic membrane, rolled film; Biological catalyst in the membrane bioreactors at different levels only circulates in membrane bioreactor at the corresponding levels, can not see through membrane module and flow into the next stage membrane bioreactor; Membrane bioreactors at different levels are after production concentration reaches the technological standards requirement, and product acrylamide, water, vinyl cyanide and by product vinylformic acid can see through membrane module enter the next stage membrane bioreactor, realizes separating with biological catalyst.
Described method, described multistage membrane bioreactor is in series by 3 to 10 membrane bioreactors.
Described method, after described biological catalyst cleaned, add-on accounted for the 5%-30% of the preceding reaction solution cumulative volume of reaction in the membrane bioreactor reactor.
Described method, described membrane bioreactor temperature controlling range at different levels are at 15-25 ℃.
Multistage membrane bioreactor continuous production acrylamide soln technology, according to producing (or market) design to acrylamide concentration needs and actual production technology, can realize that three grades, level Four, Pyatyi, six grades, seven grades, eight grades, nine grades, ten grades membrane bioreactors series connection serializations produce 8 kinds of technologies of acrylamide soln, form by 3,4,5,6,7,8,9,10 film bioreactor devices series connection respectively.
8 kinds of technologies of multistage membrane bioreactor continuous production acrylamide soln all can be produced 150-500g/L acrylamide concentration gradient solution.
Description of drawings
Fig. 1 is that the acrylamide soln technical process is produced in the serialization of Pyatyi membrane bioreactor among the embodiment 2, and 3,4 two-layer configurations omit, wherein AM: acrylamide, AN: vinyl cyanide with 1,2 two-stages.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
Select propionic acid rod bacillus or its mutagenic fungi cell that can produce Nitrile hydratase for use.
The preparation of zymogenic cells: carry out the cultivation of ferment-seeded earlier, the seed culture medium of 10-70% (volume ratio) of in triangular flask or seeding tank, packing into, the bacterial classification of 1-10% (volume ratio) is inserted in the sterilization back, under 20-40 ℃, in the rotary shaking table, 100-400rpm, shaking culture 30-120 hour.Perhaps use the seeding tank of 50L-2M3, the inclined-plane seed is inserted in real jar of sterilization back, air flux (air capacity that feeds in the unit volume fermented liquid unit time) is 1: 0.2-1: 1, V.V.M, stirring velocity is 10-400rpm, tank pressure remains on 0.03-0.06mPa, and temperature is 20-40 ℃, cultivates 30-200 hour.
Seed culture medium (weight ratio): 0.5-2% glucose, 0.2-1% yeast extract paste, 0.05-0.15%Nacl, 0.05-0.3%K
2HPO
4, 0.01-0.03%MgSO
4, urea 0.1-1%, PH7.0-7.5;
Then at 50L-20m
3Fermentor tank, its fermention medium Intake Quantity is 40%-70% (volume ratio), the seed liquor of 2-7% (volume ratio) is inserted in real jar of sterilization back, at air flow 1: 0.2-1: 1, V.V.M; Mixing speed: 50-400rpm; Tank pressure 0.03-0.06MP; Temperature: 20-40 ℃, fermented 30-200 hour;
Fermention medium (weight ratio): 1-2.5% glucose, 0.2-1% yeast extract paste, 0.1-2% urea, 0.03-0.1%K
2HPO
4, 0.03-0.1%KH
2PO
4, 0.03-0.1%MgSO
4, 2-20ppmCoCl
2(cobalt dichloride), monosodium glutamate 0.04-0.2%, PH6.5-7.5.
Embodiment 2
As shown in Figure 1, film bioreactor device: be coupled by reactor and membrane module, that Fig. 1 has also illustrated is multistage (among Fig. 1 be 5 grades, 3 to 10 grades all can), and the acrylamide soln technical process is produced in the membrane bioreactor serialization.
Present embodiment comprises the Pyatyi membrane bioreactor, is connected in series between at different levels.
(1) will cultivate qualified biological catalyst and squeeze into 1-10 ℃ of storage of biological catalyst storage tank, will in the 1 grade of membrane bioreactor reactor of 5%-30% adding by reaction solution cumulative volume before the reaction, open and stir through the biological catalyst that cleans.The hydration reaction controlled temperature begins current adding substrate vinyl cyanide and water in 1 grade of membrane bioreactor reactor at 15-25 ℃, and the two generates the product acrylamide through the katalysis of Nitrile hydratase.The every data target of reaction solution (acrylamide concentration, acrylonitrile concentration, acrylic acid concentration, specific conductivity, pH) in the online detection membrane bioreactor retort, the sampling of each hour at least of no on-line detecting system detects.Regulate the flow acceleration of vinyl cyanide and water according to reaction solution test sample data.
Acrylamide soln concentration reaches 150-230g/L in 1 grade of membrane bioreactor reactor liquid, (macromolecular particle material such as thalline can not see through through the lock out operation of 1 grade of membrane bioreactor membrane module system, acrylamide and water can see through), obtain the 150-230g/L acrylamide continuously and see through liquid and phegma (containing biological catalyst).Phegma returns in 1 grade of membrane bioreactor reactor through reflux pipeline, and the 150-230g/L acrylamide sees through liquid and enters in 2 grades of membrane bioreactor reactors.
(2) enter in 2 grades of membrane bioreactor reactors to certain liquid level when the 150-230g/L acrylamide soln, will be through the biological catalyst that cleans, in the 2 grades of membrane bioreactor reactors of 5%-30% adding by reaction solution cumulative volume before the reaction.Controlled temperature is at 15-25 ℃, and current adding substrate vinyl cyanide in 2 grades of membrane bioreactor reactors, vinyl cyanide and 1 grade of membrane bioreactor acrylamide see through water in the liquid to carry out hydration reaction and generate acrylamide.The every data target of reaction solution (acrylamide concentration, acrylonitrile concentration, acrylic acid concentration, specific conductivity, pH) in the online detection membrane bioreactor retort, the sampling of each hour at least of no on-line detecting system detects.Regulate the vinyl cyanide flow acceleration according to reaction solution test sample data.
When acrylamide soln concentration reaches 230-330g/L in 2 grades of membrane bioreactor reactors, carry out lock out operation, successively obtain the 230-330g/L acrylamide and see through liquid and phegma (containing biological catalyst) through the membrane module system.Phegma returns in 2 grades of membrane bioreactor reactors through reflux pipeline, and the 230-330g/L acrylamide sees through liquid and enters in 3 grades of membrane bioreactor reactors.
(3) enter in 3 grades of membrane bioreactor reactors to certain liquid level when the 230-330g/L acrylamide soln, will be through the biological catalyst that cleans, in the 3 grades of membrane bioreactor reactors of 5%-30% adding by reaction solution cumulative volume before the reaction.Controlled temperature is at 15-25 ℃, and current adding substrate vinyl cyanide in 3 grades of membrane bioreactor reactors, vinyl cyanide and 2 grades of membrane bioreactor acrylamides see through water in the liquid to carry out hydration reaction and generate acrylamide.The every data target of reaction solution (acrylamide concentration, acrylonitrile concentration, acrylic acid concentration, specific conductivity, pH) in the online detection membrane bioreactor retort, the sampling of each hour at least of no on-line detecting system detects.Regulate the vinyl cyanide flow acceleration according to reaction solution test sample data.
When acrylamide soln concentration reaches 330-420g/L in 3 grades of membrane bioreactor reactors, carry out lock out operation, successively obtain the 330-420g/L acrylamide and see through liquid and phegma (containing biological catalyst) through the membrane module system.Phegma returns in 3 grades of membrane bioreactor reactors through reflux pipeline, and the 330-420g/L acrylamide sees through liquid and enters in 4 grades of membrane bioreactor reactors.
(4) enter in 4 grades of membrane bioreactor reactors to certain liquid level when the 330-420g/L acrylamide soln, will be through the biological catalyst that cleans, in the 4 grades of membrane bioreactor reactors of 5%-30% adding by reaction solution cumulative volume before the reaction.15-25 ℃ of temperature control, current adding substrate vinyl cyanide in 4 grades of membrane bioreactor reactors, vinyl cyanide and 3 grades of membrane bioreactor acrylamides carry out hydration reaction through the water in the liquid and generate acrylamide.The every data target of reaction solution (acrylamide concentration, acrylonitrile concentration, acrylic acid concentration, specific conductivity, pH) in the online detection membrane bioreactor retort, the sampling of each hour at least of no on-line detecting system detects.Regulate the vinyl cyanide flow acceleration according to reaction solution test sample data.
When acrylamide soln concentration reaches 420-500g/L in 4 grades of membrane bioreactor reactors, carry out lock out operation, successively obtain the 420-500g/L acrylamide and see through liquid and phegma (containing biological catalyst) through the membrane module system.Phegma returns in 4 grades of membrane bioreactor reactors through reflux pipeline, and the 420-500g/L acrylamide sees through liquid and enters in 5 grades of membrane bioreactor reactors.
(5) enter in 5 grades of membrane bioreactor reactors to certain liquid level when the 420-500g/L acrylamide soln, will be through the biological catalyst that cleans, in the long-pending 5 grades of membrane bioreactor reactors of 5%-30% adding of total reaction liquid before the reaction.Temperature is controlled at 15-25 ℃, and the vinyl cyanide of reaction system remnants carries out hydration reaction.The every data target of reaction solution (acrylamide concentration, acrylonitrile concentration, acrylic acid concentration, specific conductivity, pH) in the online detection membrane bioreactor retort, the sampling of each hour at least of no on-line detecting system detects.
When acrylonitrile concentration is lower than 1g/L, carry out lock out operation, successively obtain acrylamide and see through liquid and phegma (containing biological catalyst) through the membrane module system.Phegma returns in 5 grades of membrane bioreactor reactors through reflux pipeline, and acrylamide sees through liquid and enters the acrylamide soln storage tank.
Should be understood that, for those of ordinary skills, can be improved according to the above description or conversion, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.
Claims (4)
1. the method that acrylamide soln is produced in multistage membrane bioreactor series connection serialization is characterized in that multistage membrane bioreactor connects by series system; Described film bioreactor device is formed by membrane module and reactor coupling; Described membrane module is one of hollow-fibre membrane, ceramic membrane, rolled film; Biological catalyst in the membrane bioreactors at different levels only circulates in membrane bioreactor at the corresponding levels, can not see through membrane module and flow into the next stage membrane bioreactor; Membrane bioreactors at different levels are after production concentration reaches the technological standards requirement, and product acrylamide, water, vinyl cyanide and by product vinylformic acid can see through membrane module enter the next stage membrane bioreactor, realizes separating with biological catalyst.
2. method according to claim 1 is characterized in that, described multistage membrane bioreactor is in series by 3 to 10 membrane bioreactors.
3. method according to claim 1 is characterized in that, after described biological catalyst cleaned, add-on accounted for the 5%-30% of the preceding reaction solution cumulative volume of reaction in membrane bioreactor reactors at different levels.
4. method according to claim 1 is characterized in that, described membrane bioreactor temperature controlling range at different levels are at 15-25 ℃.
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Cited By (6)
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| CN105247063A (en) * | 2012-12-10 | 2016-01-13 | 三菱丽阳株式会社 | Method for producing acrylamide |
| CN105420302A (en) * | 2015-12-15 | 2016-03-23 | 安徽巨成精细化工有限公司 | Method and device for continuously preparing acrylamide with microbiological method |
| CN107034124A (en) * | 2017-04-24 | 2017-08-11 | 如东南天农科化工有限公司 | A kind of system and its production method of acrylamide continuous production zymotic fluid |
| CN107779482A (en) * | 2017-12-05 | 2018-03-09 | 山东宝莫生物化工股份有限公司 | A kind of production technology of high concentration acrylamide |
| CN113999880A (en) * | 2021-11-10 | 2022-02-01 | 东营宝莫环境工程有限公司 | Efficient catalytic reaction production method for synthesizing acrylamide by changing mass transfer and heat transfer modes |
| CN114471172A (en) * | 2020-10-23 | 2022-05-13 | 中国石油化工股份有限公司 | Method for preparing high-quality acrylamide aqueous solution |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105247063A (en) * | 2012-12-10 | 2016-01-13 | 三菱丽阳株式会社 | Method for producing acrylamide |
| US10160982B2 (en) | 2012-12-10 | 2018-12-25 | Mitsubishi Chemical Corporation | Method for producing acrylamide |
| CN105247063B (en) * | 2012-12-10 | 2020-10-23 | 三菱化学株式会社 | Method for producing acrylamide |
| CN105420302A (en) * | 2015-12-15 | 2016-03-23 | 安徽巨成精细化工有限公司 | Method and device for continuously preparing acrylamide with microbiological method |
| CN105420302B (en) * | 2015-12-15 | 2019-04-16 | 安徽巨成精细化工有限公司 | A kind of serialization microbial method prepares the method and device of acrylamide |
| CN107034124A (en) * | 2017-04-24 | 2017-08-11 | 如东南天农科化工有限公司 | A kind of system and its production method of acrylamide continuous production zymotic fluid |
| CN107779482A (en) * | 2017-12-05 | 2018-03-09 | 山东宝莫生物化工股份有限公司 | A kind of production technology of high concentration acrylamide |
| CN114471172A (en) * | 2020-10-23 | 2022-05-13 | 中国石油化工股份有限公司 | Method for preparing high-quality acrylamide aqueous solution |
| CN113999880A (en) * | 2021-11-10 | 2022-02-01 | 东营宝莫环境工程有限公司 | Efficient catalytic reaction production method for synthesizing acrylamide by changing mass transfer and heat transfer modes |
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Application publication date: 20111221 |