CN1279020C - Method of removing thallus and macromolecular protein from acrylamide produced via biological process - Google Patents
Method of removing thallus and macromolecular protein from acrylamide produced via biological process Download PDFInfo
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- CN1279020C CN1279020C CN 03129828 CN03129828A CN1279020C CN 1279020 C CN1279020 C CN 1279020C CN 03129828 CN03129828 CN 03129828 CN 03129828 A CN03129828 A CN 03129828A CN 1279020 C CN1279020 C CN 1279020C
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- China
- Prior art keywords
- acrylamide
- membrane module
- membrane
- thalline
- macro
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 27
- 102000004169 proteins and genes Human genes 0.000 title claims abstract description 25
- 108090000623 proteins and genes Proteins 0.000 title claims abstract description 25
- 230000031018 biological processes and functions Effects 0.000 title claims abstract description 14
- 239000012528 membrane Substances 0.000 claims abstract description 89
- 239000007788 liquid Substances 0.000 claims abstract description 27
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 238000004140 cleaning Methods 0.000 claims abstract description 12
- 230000002457 bidirectional effect Effects 0.000 claims abstract description 7
- FRXSZNDVFUDTIR-UHFFFAOYSA-N 6-methoxy-1,2,3,4-tetrahydroquinoline Chemical compound N1CCCC2=CC(OC)=CC=C21 FRXSZNDVFUDTIR-UHFFFAOYSA-N 0.000 claims description 29
- 239000000835 fiber Substances 0.000 claims description 19
- 239000012510 hollow fiber Substances 0.000 claims description 18
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 18
- 238000004519 manufacturing process Methods 0.000 claims description 17
- 230000000694 effects Effects 0.000 claims description 10
- -1 polyethylene Polymers 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 238000000108 ultra-filtration Methods 0.000 claims description 7
- 230000036571 hydration Effects 0.000 claims description 6
- 238000006703 hydration reaction Methods 0.000 claims description 6
- 238000001471 micro-filtration Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000011001 backwashing Methods 0.000 claims description 5
- 239000004698 Polyethylene Substances 0.000 claims description 4
- 239000004743 Polypropylene Substances 0.000 claims description 4
- 229920006393 polyether sulfone Polymers 0.000 claims description 4
- 229920000573 polyethylene Polymers 0.000 claims description 4
- 229920001155 polypropylene Polymers 0.000 claims description 4
- 239000004695 Polyether sulfone Substances 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229920002492 poly(sulfone) Polymers 0.000 claims description 3
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 3
- AVSXGQJYEFAQNK-UHFFFAOYSA-N prop-2-enamide;hydrate Chemical compound O.NC(=O)C=C AVSXGQJYEFAQNK-UHFFFAOYSA-N 0.000 abstract 3
- 241001052560 Thallis Species 0.000 abstract 2
- 238000010992 reflux Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 11
- 239000000047 product Substances 0.000 description 9
- 238000000926 separation method Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 5
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 4
- 238000005374 membrane filtration Methods 0.000 description 3
- 238000000386 microscopy Methods 0.000 description 3
- 230000000712 assembly Effects 0.000 description 2
- 238000000429 assembly Methods 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The present invention provides a method for removing thalli and molecular protein from acrylamide product prepared by a biological process, which comprises: acrylamide hydrate liquid is supplied to a membrane module for filtration, and the products, such as the thalli, the protein, etc., in the product are removed. The operating state adopts a filtration technique of bidirectional flow, and comprises a forward operating state and a reverse operating state; in the forward operating state, the acrylamide hydrate liquid is led into a fibrous membrane module from the lower port of the membrane module for filtration under the function of a circulation pump, the concentrated solution which is filtered is discharged from the upper port of the membrane module into a circulation tank, and the acrylamide solution is discharged from an upper-side mouth; the membrane module works in the opposite direction after a certain time: the acrylamide hydrate liquid is led into the membrane module from the upper port for filtration under the function of the circulation pump, the concentrated solution is discharged from the lower port into a circulation reflux loop, and the acrylamide solution is discharged from the upper-side mouth; the alternation of the forward and the reverse can make the separating work and the cleaning work of a membrane simultaneous and efficient.
Description
Technical field
The present invention relates to a kind of in biological process production acrylamide, remove the thalline in the product and the method for macro-molecular protein, be specifically related to produce in the acrylamide with hollow-fibre membrane and remove thalline and the isolation technique of macro-molecular protein and the separating device that is adopted in the product at biological process.
Background technology
Biological process is produced the production technique that acrylamide is a kind of directed conversion, by product is few.Concrete production process is that stream adds quantitative acrylonitrile in the free thalline aqueous solution of 0.3%～2.0% (weight), the concentration of product acrylamide is generally between 25～50% (weight), except that containing acrylamide, also contain thalline, macro-molecular protein and a spot of other by product of thalline, fragmentation in the product.
In order to obtain the higher acrylamide of purity, just need go out thalline and protein separation.Original separation method is with whizzer thalline and macro-molecular protein to be separated, or filters with rolled film after the whizzer separation again.
And there is following shortcoming in the isolating method of whizzer:
Yield is low, generally about 85%; Inferior separating effect still contains a small amount of thalline and amounts of protein in the acrylamide soln after often separating; Production cycle is long, and energy consumption is big, and efficient is low, and this has increased very big burden for follow-up purification.
If use rolled film again after adopting whizzer to separate, the production cycle extends greatly, and production efficiency reduces greatly, and overlapping investment.
Summary of the invention
The present invention adopts Hollow Fiber Ultrafiltration or microfiltration membrane device, thalline in the separation of acrylamide aqua liquid and macro-molecular protein, and purpose is for the purity that improves acrylamide soln, increase yield and enhances productivity.
In order to realize the foregoing invention purpose, the invention provides a kind of biological process of removing and produce the thalline in the acrylamide product and the method for macro-molecular protein, it is characterized in that: the acrylamide aqua liquid is fed in the membrane module filters, remove thalline in the product, protein etc., the treatment process of its membrane module comprises working order and to the cleaning state of membrane module.
In addition, above-mentioned working order adopts the bidirectional flow filtration process, comprises forward working order and reverse operation state;
When the forward working order, the acrylamide aqua liquid is under the effect of recycle pump, enter the fiber film component from the lower port of membrane module and to filter, concentrated solution after the filtration is discharged to the pump around circuit pipeline from the upper port of membrane module, enter circulation tank again and circulate, acrylamide soln is discharged by the upside mouth;
Behind the work certain hour, make membrane module carry out opposite direction work, its working order is: the acrylamide aqua liquid enters membrane module from the upper port of membrane module and filters under the effect of recycle pump, concentrated solution is drained into the pump around circuit loop from lower port, and acrylamide soln is discharged by the upside mouth;
Forward, oppositely alternation can be carried out membrane sepn and cleaning efficiently simultaneously.
After work for some time, equipressure is carried out in the cleaning elder generation backwash of membrane module again clean;
Backwash process is: under the effect of backwashing pump, backwash liquor enters membrane module, and film is carried out backwash, and water enters the inboard of tunica fibrosa under pressure from the outside of membrane module hollow-fibre membrane, makes the whole refunds of thalline in hydration tank;
Isobaric cleaning process is: with the port closing of acrylamide soln, tunica fibrosa medial and lateral pressure is consistent.
In addition, the material of above-mentioned hollow fiber film assembly is materials such as polysulfones, polyethersulfone, polyacrylonitrile, polyvinylidene difluoride (PVDF), polyethylene or polypropylene one or both or two or more mixtures wherein.
The material of above-mentioned hollow fiber film assembly is a polyvinylidene difluoride (PVDF).
Hollow-fibre membrane is hollow fiber microfiltration membrane or hollow fiber ultrafiltration membrane.
Hollow-fibre membrane can be an individual layer, also can be composite hollow fiber membrane.
By employing Hollow Fiber Ultrafiltration provided by the invention or microfiltration membrane device, the thalline in the separation of acrylamide aqua liquid and the method for macro-molecular protein, compare with other separation method of the prior art, directly adopt the tubular fibre membrane filter appts to filter the acrylamide aqua liquid, particularly adopt bidirectional flow technology, improve filtration velocity greatly, shortened the production cycle, reduce cost, and reached desired high purity.Resultant acrylamide soln (seeing through liquid), microscopy does not have thalline, and protein content is less than 10ppm, and yield is more than 99%, and production efficiency improves greatly.
Description of drawings
Fig. 1 is a hollow membrane component system synoptic diagram used in the present invention
Embodiment
Below, the present invention is described in detail by drawings and Examples.Embodiment just further specifies of the present invention, and it does not limit protection scope of the present invention.
As shown in Figure 1, shown hollow membrane component system used in the present invention.
The thalline in the above-mentioned use hollow membrane assembly removal production acrylamide product and the system component of macro-molecular protein comprise: parts such as circulation tank 1, recycle pump 14, working line 21, membrane module 2, pump around circuit pipeline 24, back wash tank 12, backwashing pump 15, backwash pipeline.Wherein, working line 21 pipes are connected between circulation tank 1 and the membrane module 2, and working line is provided with parts such as recycle pump 14, valve.Working line 21 was divided into two branch roads before pipe connects membrane module 2: forward working line 23 and reverse operation pipeline 22.Wherein the relative membrane module of the fluid in the forward working line 23 goes out on advancing for 2 times, goes out under the relative membrane module of the fluid in the reverse operation pipeline 22 2 is enterprising.Forward working line 23 pipes are connected on the lower port 7 of membrane module 2, are used under the forward working order, the acrylamide aqua liquid are fed in the membrane module 2 switching of valve 4 control forward working lines; Reverse operation pipeline 22 pipes are connected on the upper port 6 of membrane module 2, are used under the reverse operation state, the acrylamide aqua liquid are fed in the membrane module 2 switching of valve 5 control reverse operation pipelines.The upper port 6 of membrane module 2 also is connected with an end of forward work escape route 26, the other end of forward work escape route 26 is connected on the pump around circuit pipeline 24, be used for the concentrated solution under the forward working order is discharged into the pump around circuit pipeline discharging of valve 10 control concentrated solutions.The lower port 7 of reverse operation escape route 27 junctional membrane assemblies 2, its other end is connected on the pump around circuit pipeline 24, is used for the concentrated solution under the reverse operation state is discharged into the pump around circuit pipeline discharging of valve 11 control concentrated solutions.Clarifying acrylamide soln is discharged by discharge pipe 25 from the upside mouth of membrane module 2.
In addition, carry out work better in order to make membrane separation assemblies, the present invention has also met the backwash system to the membrane module pipe.Back wash tank 12 is connected to the downside mouth 8 of membrane module by the backwash pipeline, and the backwash pipeline is provided with parts such as backwashing pump 15, valve.
Method with thalline in the hollow membrane assembly removal production acrylamide product and macro-molecular protein comprises that working order and film clean state.Wherein, the working process of membrane module is as described below:
In adopting the bidirectional flow filtration process, working order comprises forward working order and reverse operation state.When the forward working order, the acrylamide aqua liquid is under the effect of recycle pump 14, arrive the lower port 7 of membrane module 2 by feed liquor valve 4 along working line 21, forward working line 23, the acrylamide aqua liquid filters in fiber film component 2, concentrated solution after the filtration is discharged to pump around circuit pipeline 24 from the upper port 6 of membrane module along pipeline 26, enter circulation tank 1 again and circulate, clarifying acrylamide soln is discharged to escape route 25 by upside mouth 9.Behind the work certain hour, when the working efficiency of membrane module and acrylamide soln flux decrease, make membrane module carry out opposite direction work.The reverse operation state is: the acrylamide aqua liquid enters into the upper port 6 of membrane module 2 by reverse feed liquor valve 5 along working line 21, reverse operation pipeline 22, entering membrane module filters, concentrated solution is drained into the pump around circuit loop from lower port 7, and clarifying acrylamide soln (seeing through liquid) is discharged by upside mouth 9.Forward, oppositely alternation can be carried out membrane sepn and cleaning efficiently simultaneously.
After work for some time, under the effect of backwashing pump 15, backwash liquor enters membrane module 2 by backwash pipeline 28 from back wash tank 12, film is carried out backwash, water under pressure, enter the inboard of tunica fibrosa from the outside of membrane module hollow-fibre membrane, make the whole refunds of thalline in circulation tank (hydration tank just) 1.This backwash process is cleaned separately the membrane module system after filtering end.After the backwash, membrane module is carried out equipressure clean.The isobaric cleaning is in normal operation, and the outlet 9 of acrylamide soln is closed, and tunica fibrosa medial and lateral pressure is consistent.
Wherein, the material of above-mentioned hollow fiber film assembly can be polysulfones, polyethersulfone, polyacrylonitrile, polyvinylidene difluoride (PVDF), polyethylene or polypropylene etc., also can be two or more the mixture in them.Wherein, the performance of polyvinylidene difluoride (PVDF) hollow-fibre membrane is best, and the material of preferred hollow fiber film assembly is a polyvinylidene difluoride (PVDF).
Employed hollow-fibre membrane can be common hollow-fibre membrane, hollow fiber microfiltration membrane or hollow fiber ultrafiltration membrane etc.Hollow-fibre membrane can be an individual layer, also can be composite hollow fiber membrane.
Following mask body illustrates employing effect of the present invention in the mode of embodiment.
Acrylamide aqua liquid 6.2m
3, acrylamide concentration is 26.8% (weight), uses 160m
3The polyvinylidene fluoride (PVDF) ultrafiltration membrane filtration unit filter, adopt the bidirectional flow filtration process, microscopy does not have thalline in the acrylamide soln, protein content is 4ppm, filtration time is 68 minutes, the filtered liquid volume is 5.8m
3, remain unfiltered concentrated solution, by backwash system refunds in hydration tank, but reaction repeated is used 3～6 times.
Embodiment 2:
Acrylamide aqua liquid 4.5m
3, acrylamide concentration is 27.6 (weight), uses 160m
3Polysulphones hyperfiltration membrane or poly (ether-sulfone) ultrafiltration membrane filtration unit filter, adopt the bidirectional flow filtration process, microscopy does not have thalline in the acrylamide soln, protein content is 6ppm, filtration time is 48 minutes, the filtered liquid volume is 4.1m
3, remain unfiltered concentrated solution, by backwash system refunds in hydration tank, but reaction repeated is used 3～6 times.
Embodiment 3:
Continuous processing is produced acrylamide, retort volume 30m
3Cell concentration is 5.0 (weight) in the reaction solution, Continuous Flow adds acrylonitrile and pure water, and with tubular fibre polyvinylidene difluoride (PVDF), polyethylene or polypropylene microfiltration membrane, constantly the acrylamide soln of reacted not mycetome and macro-molecular protein is separated, simultaneously, the volume that makes acrylonitrile that stream adds and pure water equates with the volume of the acrylamide soln that hollow fiber filter device leaches, and makes the constant volume in the hydration tank (being circulation tank).The flow of filtrate is 5.0m
3/ h, successive reaction stopped stream and adds acrylonitrile and pure water after 72 hours, and the feed liquid in the retort is filtered with the tubular fibre membrane filter appts, in tubular fibre membrane filtration system feed liquid very little, not enough circulation time, the feed liquid in this moment jar is less than 1m
3, shut down, separate remaining feed liquid with additive method.
Claims (7)
1, a kind of biological process of removing is produced the thalline in the acrylamide product and the method for macro-molecular protein, it is characterized in that:
The acrylamide aqua liquid is fed in the membrane module filters, remove thalline, protein in the product, the treatment process of its membrane module comprises working order and to the cleaning state of membrane module.
2, the thalline in the removal biological process production acrylamide product according to claim 1 and the method for macro-molecular protein is characterized in that:
Working order adopts the bidirectional flow filtration process, comprises forward working order and reverse operation state;
When the forward working order, the acrylamide aqua liquid is under the effect of recycle pump, enter the fiber film component from the lower port of membrane module and to filter, concentrated solution after the filtration is discharged to the pump around circuit pipeline from the upper port of membrane module, enter circulation tank again and circulate, acrylamide soln is discharged by the upside mouth;
Behind the work certain hour, make membrane module carry out opposite direction work, its working order is: the acrylamide aqua liquid enters membrane module from the upper port of membrane module and filters under the effect of recycle pump, concentrated solution is drained into the pump around circuit loop from lower port, and acrylamide soln is discharged by the upside mouth;
Forward, oppositely alternation can be carried out membrane sepn and cleaning efficiently simultaneously.
3, the thalline that produces in the removal biological process production acrylamide according to claim 1 and the method for macro-molecular protein is characterized in that:
The cleaning state adopts the equipressure cleaning is carried out in the backwash of membrane module elder generation again;
Backwash process is: under the effect of backwashing pump, backwash liquor enters membrane module, and film is carried out backwash, and water enters the inboard of tunica fibrosa under pressure from the outside of membrane module hollow-fibre membrane, makes the whole refunds of thalline in hydration tank;
Isobaric cleaning process is: with the port closing of acrylamide soln, tunica fibrosa medial and lateral pressure is consistent.
4, the thalline in the removal biological process production acrylamide product according to claim 3 and the method for macro-molecular protein is characterized in that:
The material of above-mentioned hollow fiber film assembly is polysulfones, polyethersulfone, polyacrylonitrile, polyvinylidene difluoride (PVDF), polyethylene or polypropylene one or both or a two or more mixture wherein.
5, the thalline in the removal biological process production acrylamide product according to claim 4 and the method for macro-molecular protein is characterized in that:
The material of above-mentioned hollow fiber film assembly is a polyvinylidene difluoride (PVDF).
6, the thalline in the removal biological process production acrylamide product according to claim 3 and the method for macro-molecular protein is characterized in that:
Hollow-fibre membrane is hollow fiber microfiltration membrane or hollow fiber ultrafiltration membrane.
7, the thalline in the removal biological process production acrylamide product according to claim 3 and the method for macro-molecular protein is characterized in that:
Hollow-fibre membrane can be an individual layer, also can be composite hollow fiber membrane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03129828 CN1279020C (en) | 2003-05-20 | 2003-05-20 | Method of removing thallus and macromolecular protein from acrylamide produced via biological process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03129828 CN1279020C (en) | 2003-05-20 | 2003-05-20 | Method of removing thallus and macromolecular protein from acrylamide produced via biological process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1548417A CN1548417A (en) | 2004-11-24 |
| CN1279020C true CN1279020C (en) | 2006-10-11 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03129828 Expired - Lifetime CN1279020C (en) | 2003-05-20 | 2003-05-20 | Method of removing thallus and macromolecular protein from acrylamide produced via biological process |
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| Country | Link |
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| CN (1) | CN1279020C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103977710B (en) * | 2014-03-20 | 2016-09-28 | 河海大学 | A kind of inner pressed membranous system chemical cleaning method |
| CN105671097A (en) * | 2016-04-01 | 2016-06-15 | 如东南天农科化工有限公司 | Preparation technology of acrylamide aqueous solution with high purity and ultralow protein content |
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2003
- 2003-05-20 CN CN 03129828 patent/CN1279020C/en not_active Expired - Lifetime
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| Publication number | Publication date |
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| CN1548417A (en) | 2004-11-24 |
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Address after: 300457 No. eleventh, 60 Avenue, Tianjin economic and Technological Development Zone, Tianjin Patentee after: Tianjin Motimo Membrane Technology Co.,Ltd. Address before: 300457 No. 11, 60 Avenue, Tianjin economic and Technological Development Zone Patentee before: Tianjin Motimo Membrane Technology Co.,Ltd. |
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