CN106984061A - A kind of 1,5 pentanediamine continuous countercurrent extraction Processes and apparatus - Google Patents
A kind of 1,5 pentanediamine continuous countercurrent extraction Processes and apparatus Download PDFInfo
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- 238000000605 extraction Methods 0.000 title claims abstract description 91
- VHRGRCVQAFMJIZ-UHFFFAOYSA-N cadaverine Chemical compound NCCCCCN VHRGRCVQAFMJIZ-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 239000007788 liquid Substances 0.000 claims abstract description 68
- 238000006243 chemical reaction Methods 0.000 claims abstract description 51
- 230000002255 enzymatic effect Effects 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 27
- 230000003068 static effect Effects 0.000 claims abstract description 20
- 239000000523 sample Substances 0.000 claims abstract description 7
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 53
- 239000000284 extract Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000004891 communication Methods 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 8
- 238000012546 transfer Methods 0.000 claims description 8
- 230000008676 import Effects 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 7
- UHZZMRAGKVHANO-UHFFFAOYSA-M chlormequat chloride Chemical compound [Cl-].C[N+](C)(C)CCCl UHZZMRAGKVHANO-UHFFFAOYSA-M 0.000 claims description 5
- 230000005540 biological transmission Effects 0.000 claims description 4
- 239000011344 liquid material Substances 0.000 claims description 3
- 239000010865 sewage Substances 0.000 claims description 3
- 230000003416 augmentation Effects 0.000 claims description 2
- 239000012295 chemical reaction liquid Substances 0.000 claims description 2
- 238000006911 enzymatic reaction Methods 0.000 claims description 2
- 238000011144 upstream manufacturing Methods 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims 1
- 230000005494 condensation Effects 0.000 claims 1
- 239000012074 organic phase Substances 0.000 abstract 2
- 239000008346 aqueous phase Substances 0.000 abstract 1
- 238000012423 maintenance Methods 0.000 abstract 1
- 238000005191 phase separation Methods 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 10
- 239000000243 solution Substances 0.000 description 8
- 150000003839 salts Chemical class 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 235000011121 sodium hydroxide Nutrition 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000011953 bioanalysis Methods 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- KJOMYNHMBRNCNY-UHFFFAOYSA-N pentane-1,1-diamine Chemical compound CCCCC(N)N KJOMYNHMBRNCNY-UHFFFAOYSA-N 0.000 description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 3
- 229910001948 sodium oxide Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000855 fermentation Methods 0.000 description 2
- 230000004151 fermentation Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical class Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- BVHLGVCQOALMSV-JEDNCBNOSA-N L-lysine hydrochloride Chemical compound Cl.NCCCC[C@H](N)C(O)=O BVHLGVCQOALMSV-JEDNCBNOSA-N 0.000 description 1
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 description 1
- 239000004472 Lysine Substances 0.000 description 1
- 108010048581 Lysine decarboxylase Proteins 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 238000006114 decarboxylation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0446—Juxtaposition of mixers-settlers
- B01D11/0457—Juxtaposition of mixers-settlers comprising rotating mechanisms, e.g. mixers, mixing pumps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0446—Juxtaposition of mixers-settlers
- B01D11/0461—Juxtaposition of mixers-settlers mixing by counter-current streams provoked by centrifugal force
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0484—Controlling means
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D2011/002—Counter-current extraction
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses the continuous countercurrent extraction technique of a kind of 1,5 pentanediamine static mixers, liquid liquid cyclone separator, at the same there is provided it is a kind of be the special equipment realizing the technique.Special equipment includes pipeline, static mixer, liquid liquid cyclone separator, its designing points is to be fabricated to vertical tube heat exchanger form with static mixer, accelerate organic phase and aqueous phase separation built with liquid liquid cyclone separator in same tower body simultaneously, and each tower body is furnished with organic phase measuring pump and enzymatic conversion liquid measuring pump, temp probe is provided with provided with digital controlled valve, on tower body on pipeline, the probe, the signal output part of digital controlled valve are connected with computer control system.The technical process is simple, and easy to operate, extraction process is not disturbed by insoluble matter, and product extraction yield is high.Its device structure is simple, and cost is low, and is easy to maintenance.
Description
Technical field
The invention belongs to the abstraction technique field in biochemical industry separation, it is related to a kind of continuous extraction 1, the work of 5- pentanediamines
Skill and its special equipment.
Background technology
1,5- pentanediamines（Also referred to as cadaverine）It is the important source material of chemical industry, 1,5- pentanediamine is the important of synthesized polymer
Monomer, for example, being widely used in the synthesis of polyamide and polyurethane.
Bioanalysis synthesis 1,5- pentanediamines are a kind of environmental protection with potential competition power, the side of resources
Method.
Patent CN 205856354 is reported：As domestic and international 1,5- pentanediamines synthesize and developed further investigation, synthesis at present
1,5- pentanediamine is divided into two kinds of chemical synthesis and biological fermentation process, and chemical method has cyano reduction method, hydroxyl ammoniation process and bad ammonia
Acid and its salt cracking process, biological fermentation process be using containing lysine or its salt as the direct decarboxylation of substrate utilization lysine decarboxylase
Obtain.No matter 1, the 5- pentanediamines of which kind of technique synthesis will need purification process, at present, be purified for 1,5- pentanediamines
Processing report is relatively fewer, substantially can not find out in the aqueous solution from 1,5- pentanediamines, organic solution or its mixed liquor and separates
Purify 1,5- pentanediamine device systems.
Liquid-liquid extraction is a kind of important chemical separation technology, with separative efficiency is high, the applicable strong, energy consumption of material is low, can
To realize the advantage continuously mass produced, in the neck such as biological medicine, new material, new energy, environmental project, natural product extraction
Domain extensive use.Improved constantly with the requirement of product, increasingly sophisticated, the requirement to extraction process and equipment of separation of material
More and more higher.
Traditional liquid-liquid extractor can be divided into three major types because of the difference of specifically used purpose：Mixed settler extractor,
Tower or column extractor, centrifugal extractor.According to the difference of mode of operation, two classes can be divided into again：Contact is extracted step by step
Equipment and continuous differential contacts formula extraction equipment.
The present invention combines bioanalysis and prepares 1,5- pentanediamine particularity, adjusts enzymatic conversion liquid with sodium hydroxide before extraction
PH is 13 or so, and backflow can produce substantial amounts of carbon dioxide in 5 hours in a reservoir, while raw materials used is 1B hydrochloric acid
Salt, certainly will so cause to have when temperature is relatively low it is substantial amounts of salt out, salt crystal not only blocks pipeline, and influence extraction effect
Really.Simultaneously because because salinity is too high in extraction, can separate out 1,5- pentanediamines crystal, so as to influence product yield.
Although autoclave stirring extractor can strengthen mass transfer and heat transfer, it can only one-pot gap operating can not continuously grasp
Make, such utilization rate of equipment and installations is small, equipment investment is big, and floor space is big.In addition, although centrifugal extractor can be operated continuously,
Heat-transfer effect is poor, also influences effect of extracting.
Therefore, for the shortcoming of existing continous way extractor, design novel reactor is very necessary.
The content of the invention
The technical problem to be solved in the invention is, during bioanalysis prepares 1,5- pentanediamines, uses before extraction
The pH of sodium hydroxide regulation enzymatic conversion liquid is 13 or so, and mixed liquor flows back 5 hours in a reservoir can produce substantial amounts of carbon dioxide,
Simultaneously raw materials used is L lysine HCL, certainly will so cause to have when temperature is relatively low it is substantial amounts of salt out, salt crystal is not
But block pipeline, and influence effect of extracting.Simultaneously because because salinity is too high in extraction, can analyse 1,5- pentanediamines crystal
Go out, so as to influence product yield.
In order to solve the above problems, of the invention provides 1,5- of one kind pentanediamine continuous countercurrent extraction equipment and technique.
Specifically, the special extraction tower of 1,5- pentanediamine continuous flow upstreams is disclosed, the Automated condtrol complete set of equipments comprising extraction tower, with
And 1,5- pentanediamine continuous countercurrent extraction techniques.
The scheme provided by the present invention, 1,5- pentanediamine enzymatic conversion liquid is after separation of solid and liquid, in stainless steel reaction tank
It is 13 to adjust pH value with sodium hydrate aqueous solution, and being 80 DEG C in temperature reacts 5 hours, and pH value is constantly adjusted during the course of the reaction is
13, reaction terminates, and is cooled to 40 DEG C and is extracted, and it is 40 DEG C that solution temperature is remained during extraction, enzymatic conversion liquid and n-butanol
Volume ratio is 5:4, extraction yield can reach 97.5%.
Further, the solution of the present invention is：
A kind of continuous countercurrent extraction 1, the extraction tower of 5- pentanediamines, wherein, the extraction tower containing pre-mix zone, stiffened region, stable region, point
Four from area regions, including sewage draining exit（31）, extractant import（32）, enzymatic conversion liquid import（33）, steam condensate (SC) outlet and
Hot water inlet（34）, steam inlet and hot water outlet（36）, static mixer（35）, raffinate outlet（37）, liquid-liquid whirlwind point
From device import（38）, extract outlet（39）, non-condensable gas export（40）.
Extraction tower of the present invention, wherein, liquid-liquid cyclone separator（41）Provided with tangential flow guiding pipe（42）And rotating cone
Body.Mixed liquor is passing through tangential flow guiding pipe（42）During with rotating cone, the speed increase of two-phase laminated flow.
Extraction tower of the present invention, wherein, static mixer（43）In equipped with a positive and a negative spiral section.By quiet
State blender（43）When, mixed liquor is in a positive and a negative spiral state in static mixer.
Extraction tower of the present invention, wherein, static mixer pipe is heat exchanger form.Heat exchanger is described in this programme
Refer to, there is heat exchange layer, the heat exchanger of heat transfer can be carried out through heat transferring medium, be shell and tube heat exchange in a preferred scheme
Device.
A kind of continuous countercurrent extraction 1, the complete set of equipments of 5- pentanediamines, it is characterised in that the equipment is included, modular 1,
5- pentanediamine enzymatic conversions liquid material bucket（1）, pump（2）, Numerical control valve（3）, pressure gauge（4）, flowmeter（5）, extraction tower（7）, pump（8）、
Numerical control valve（9）, pressure gauge（10）, flowmeter（11）, extraction tower（16）, pump（17）, Numerical control valve（18）, pressure gauge（19）, flow
Meter（20）, extraction tower（29）；N-butanol charging basket（30）, pump（25）, Numerical control valve（26）, pressure gauge（28）, flowmeter（27）, pump
（21）, Numerical control valve（22）, pressure gauge（24）, flowmeter（23）, extraction tower（16）, pump（12）, Numerical control valve（13）, pressure gauge
（15）, flowmeter（14）, extraction tower（7）, connecting tube and Automated condtrol system；
Wherein, every extraction tower top is equipped with（6）Safety-valve；
In the present invention belonging to extraction tower, be at least containing pre-mix zone, stiffened region, stable region, four regions in Disengagement zone extraction tower.
Complete set of equipments of the present invention, wherein, the control device of the automation, including temp probe, the probe, number
Valve and control system are controlled, passes through on-line checking extraction tower（7）、（16）、（29）Strict control extraction feed temperature is in target temperature
Degree；Also include pump and be provided with flow sensor（5）、（11）、（14）、（20）、（23）、（27）；Pressure sensor（4）、（10）、
（15）、（19）、（24）、（28）And controller（3）、（9）、（13）、（18）、（22）、（26）, flow sensor and pressure sensor
The pressure imported and exported and data on flows in collection pump, and transmit to controller, provided with data reception module, processing mould in controller
Block and communication module, data reception module are transferred to processing module after receiving the data message of two sensor transmissions, again finally
Transmitted via communication module to service terminal；Service terminal receives the data message that controller is sent, and is shown in its display
Screen.
One kind 1,5- pentanediamine continuous countercurrent extraction techniques, 1,5- pentanediamine enzymatic conversion liquid and n-butanol are carried out continuous inverse
Stream extraction, wherein, the technique is in counter-current extraction tower（7）、（16）、（29）It is middle to carry out；Wherein, enzymatic conversion liquid and n-butanol enter extraction
Tower pre-mix zone is taken to be premixed, premixed liquid enters stable region through extraction tower augmentation of heat transfer, mass-transfer zone, is finally entered by stable region
Disengagement zone, and carry out liquid-liquid separation in Disengagement zone.
Technique of the present invention, wherein, enzyme reaction liquid pass sequentially through enzymatic conversion liquid tank (1), pump (2),（8）、
（25）, digital controlled valve（3）、（13）、（22）, flowmeter（5）、（11）、（20）, pressure gauge（4）、（10）、（19）Extract step by step.
Technique of the present invention, wherein, n-butanol passes sequentially through batch can（30）, pump（25）、（21）、（12）, Numerical control valve
Door（26）、（22）、（13）, flowmeter（27）、（23）、（14）, pressure gauge（28）、（24）、（15）It is stripped step by step.
Technique of the present invention, wherein, premixed liquid entered the static mixer cut into slices equipped with a positive and a negative spiral, its
In, static mixer pipe is heat exchanger form；And mixed liquor passes through tangential flow guiding pipe（42）Liquid-liquid point is carried out with rotating cone
From.
In a preferred scheme, operation temperature is 40 DEG C.The operation temperature refers in whole technique, is kept
Target temperature.
The beneficial effects of the present invention are
（1）Operation is simple and reliable for special equipment, and usability is strong, considerably reduces production cost, easily realizes industry amplification.
（2）All operations of the present invention have carried out integrated modular, by computer centralized Control, the steady quality of product,
Save human cost simultaneously.Pump is provided with flow sensor, pressure sensor and controller, and flow sensor and pressure are passed
The pressure imported and exported and data on flows in sensor collection pump, and transmit to controller, provided with data reception module, place in controller
Module and communication module are managed, data reception module is transferred to processing module after receiving the data message of two sensor transmissions, most
Transmitted again via communication module to service terminal afterwards；Service terminal receives the data message that controller is sent, and it is aobvious to be shown in it
Display screen.
（3）In a preferred approach, using 40 DEG C of continuous extractions, effectively prevent from having when temperature is relatively low it is substantial amounts of salt out, from
And influence effect of extracting.Meanwhile, also effectively prevent because salinity is too high, can separate out 1,5- pentanediamines crystal, so as to influence production
Product yield.
Brief description of the drawings
Fig. 1:The complete set of equipments of continuous countercurrent extraction 1,5- pentanediamines.
Wherein, (1) is enzymatic conversion liquid tank；（2）、（8）、（25）For enzymatic conversion liquid delivery pump；（3）、（13）、（22）For enzyme
Conversion fluid digital controlled valve；（5）、（11）、（20）For enzymatic conversion flow meters；（4）、（10）、（19）Convey and be pumped for enzymatic conversion liquid
Power table；（2）For extractant n-butanol batch can；（25）、（21）、（12）For n-butanol batch can delivery pump；（26）、（22）、（13）Extraction
Take agent n-butanol digital controlled valve；（27）、（23）、（14）N-butanol feed liquid flowmeter；（28）、（24）、（15）For n-butanol batch can
Delivery pump pressure gauge.
Fig. 2：The special extraction tower of 1,5- pentanediamine.
Wherein,（31）For sewage draining exit；（32）For extractant import；（33）For enzymatic conversion liquid import；（34）Condensed for steam
Water out and hot water inlet；（35）For static mixer；（36）For steam inlet and hot water outlet；（37）For raffinate outlet；
（38）For liquid-liquid cyclone inlet（39）Exported for extract；（40）For non-condensable gas export.
Fig. 3：1,5- pentanediamine extracts special equipment liquid-liquid rotary separator.
Wherein,（41）For liquid-liquid rotary separator staving；（42）For liquid guide flow pipe.
Fig. 4：Static mixer.
Wherein,（43）For static mixer pipe；（44）Cut into slices for static mixer a positive and a negative spiral.
Embodiment
Embodiment 1：This example demonstrates that extraction obtains the group of the complete set of equipments of 1,5- pentanediamines from enzymatic conversion liquid system
Into and annexation
The schematic diagram of the complete set of equipments is as shown in Figure 1.The specific equipment contains modular 1,5- pentanediamines enzymatic conversion liquid material
Bucket（1）, pump（2）, Numerical control valve（3）, pressure gauge（4）, flowmeter（5）, extraction tower（7）, pump（8）, Numerical control valve（9）, pressure gauge
（10）, flowmeter（11）, extraction tower（16）, pump（17）, Numerical control valve（18）, pressure gauge（19）, flowmeter（20）, extraction tower
（29）；N-butanol charging basket（30）, pump（25）, Numerical control valve（26）, pressure gauge（28）, flowmeter（27）, extraction tower（29）, pump
（21）, Numerical control valve（22）, pressure gauge（24）, flowmeter（23）, extraction tower（16）, pump（12）, Numerical control valve（13）, pressure gauge
（15）, flowmeter（14）, extraction tower（7）, connecting tube and Automated condtrol system.
Extraction tower includes liquid liquid separator（As shown in Figure 3）, liquid liquid separator sets liquid-liquid rotary separator staving
（41）；Liquid guide flow pipe（42）；Also include static mixer, including static mixer pipe in extraction tower（43）And static mixing
Device a positive and a negative spiral is cut into slices（44）.
Wherein, every extraction tower top is equipped with（6）Safety-valve, it is ensured that the normal operation of equipment.
The control device of automation, including temp probe, the probe, digital controlled valve and control system, pass through on-line checking
Extraction tower（As shown in Figure 2）（7）、（16）、（29）Strict control extraction feed temperature is in specified temp；Also it is provided with including pump
Flow sensor（5）、（11）、（14）、（20）、（23）、（27）；Pressure sensor（4）、（10）、（15）、（19）、（24）、（28）
And controller（3）、（9）、（13）、（18）、（22）、（26）, flow sensor and pressure sensor gather the pressure imported and exported in pump
Power and data on flows, and transmit to controller, data reception module, processing module and communication module, data are provided with controller
Receiving module receive two sensor transmissions data message after be transferred to processing module, finally again via communication module transmit to
Service terminal；Service terminal receives the data message that controller is sent, and is shown in its display screen.
Embodiment 2：This example demonstrates that extracting the technique of 1,5- pentanediamines from enzymatic conversion liquid system
Enzymatic conversion liquid is 13 in stainless steel reaction tank sodium hydrate aqueous solution regulation pH value, in temperature after separation of solid and liquid
Reacted 5 hours for 80 DEG C, constantly adjustment pH value is 13 during the course of the reaction, and reaction terminates, and is cooled to 40 DEG C and is extracted, extraction
It is 40 DEG C that solution temperature is remained when taking, and enzymatic conversion liquid and n-butanol volume ratio are 6：5, extraction yield is 97.5%.Such as table 1, say
Bright enzymatic conversion liquid and n-butanol volume ratio are 5：4 is appropriate, and the ratio between flow and liquid inventory of extractant n-butanol are 43：50.
Influence of the flow, volume ratio of the extractant of table 1 and solution to extraction yield
| Flow（l/min） | Extract pentanediamine content（g/l） | Raffinate pentanediamine content（g/l） | Extract raffinate volume ratio | Extraction yield |
| V extractions=V is molten=and 100 | 141.18 | 21.34 | 10:7 | 90.43% |
| V extractions=V is molten=and 200 | 166.34 | 69.73 | 7:10 | 62.64% |
| V extract=43 V it is molten=50 | 176 | 6.05 | 6:5 | 97.22% |
Embodiment 3：This example demonstrates that implementing the situation of present invention process in the equipment of embodiment 1
Take 500L1,5- pentanediamine enzymatic conversion liquid, the concentration of 1,5- pentanediamine is 141.18g/L, first in stainless steel reaction tank hydrogen
Aqueous solution of sodium oxide regulation pH value is 13, and being 80 DEG C in temperature reacts 5 hours, and constantly adjustment pH value is 13 during the course of the reaction,
Reaction terminates, and is cooled to 40 DEG C, then squeezes into charging basket（1）, and in charging basket（30）N-butanol is squeezed into, by enzymatic conversion liquid tank (1)
By pump (2),（8）、（25）, digital controlled valve（3）、（13）、（22）, flowmeter（5）、（11）、（20）, pressure gauge（4）、（10）、
（19）Extract step by step successively, extractant n-butanol batch can（30）Pass through pump（25）、（21）、（12）, digital controlled valve（26）、（22）、
（13）, flowmeter（27）、（23）、（14）, pressure gauge（28）、（24）、（15）It is stripped step by step successively.With 80 in extraction process
It is 40 DEG C that solution temperature is remained during DEG C hot water, and the ratio between flow of extractant n-butanol and liquid inventory are 43：50, enzymatic conversion
Liquid and n-butanol volume ratio are 5:4, it is 97.22% to finally obtain extraction yield.
Embodiment 4：This example demonstrates that implementing the situation of present invention process in the equipment of embodiment 1
Take 500L1,5- pentanediamine enzymatic conversion liquid, the concentration of 1,5- pentanediamine is 166.34g/L, first in stainless steel reaction tank hydrogen
Aqueous solution of sodium oxide regulation pH value is 13, and being 80 DEG C in temperature reacts 5 hours, and constantly adjustment pH value is 13 during the course of the reaction,
Reaction terminates, and is cooled to 40 DEG C, then squeezes into charging basket（1）, and in charging basket（30）N-butanol is squeezed into, by enzymatic conversion liquid tank (1)
By pump (2),（8）、（25）, digital controlled valve（3）、（13）、（22）, flowmeter（5）、（11）、（20）, pressure gauge（4）、（10）、
（19）Extract step by step successively, extractant n-butanol batch can（30）Pass through pump（25）、（21）、（12）, digital controlled valve（26）、（22）、
（13）, flowmeter（27）、（23）、（14）, pressure gauge（28）、（24）、（15）It is stripped step by step successively.With 80 in extraction process
It is 40 DEG C that solution temperature is remained during DEG C hot water, and the ratio between flow of extractant n-butanol and liquid inventory are 43：50, enzymatic conversion
Liquid and n-butanol volume ratio are 5：4, it is 97.60% to finally obtain extraction yield.
Embodiment 5：This example demonstrates that implementing the situation of present invention process in the equipment of embodiment 1
Take 500L1,5- pentanediamine enzymatic conversion liquid, the concentration of 1,5- pentanediamine is 176.12g/L, first in stainless steel reaction tank hydrogen
Aqueous solution of sodium oxide regulation pH value is 13, and being 80 DEG C in temperature reacts 5 hours, and constantly adjustment pH value is 13 during the course of the reaction,
Reaction terminates, and is cooled to 40 DEG C, then squeezes into charging basket（1）, and in charging basket（30）N-butanol is squeezed into, by enzymatic conversion liquid tank (1)
By pump (2),（8）、（25）, digital controlled valve（3）、（13）、（22）, flowmeter（5）、（11）、（20）, pressure gauge（4）、（10）、
（19）Extract step by step successively, extractant n-butanol batch can（30）Pass through pump（25）、（21）、（12）, digital controlled valve（26）、（22）、
（13）, flowmeter（27）、（23）、（14）, pressure gauge（28）、（24）、（15）It is stripped step by step successively.With 80 in extraction process
It is 40 DEG C that solution temperature is remained during DEG C hot water, and the ratio between flow of extractant n-butanol and liquid inventory are 43：50, enzymatic conversion
Liquid and n-butanol volume ratio are 5：4, it is 97.45% to finally obtain extraction yield.
Claims (10)
1. a kind of continuous countercurrent extraction 1, the extraction tower of 5- pentanediamines, it is characterised in that the extraction tower containing pre-mix zone, stiffened region,
Stable region, the region of Disengagement zone four, including sewage draining exit（31）, extractant import（32）, enzymatic conversion liquid import（33）, steam condensation
Water out and hot water inlet（34）, steam inlet and hot water outlet（36）, static mixer（35）, raffinate outlet（37）, liquid-
Liquid cyclone inlet（38）, extract outlet（39）, non-condensable gas export（40）.
2. extraction tower according to claim 1, it is characterised in that liquid-liquid cyclone separator（41）Provided with tangential flow guiding pipe
（42）And rotating cone.
3. extraction tower according to claim 1, it is characterised in that static mixer（43）In cut equipped with a positive and a negative spiral
Piece.
4. extraction tower according to claim 1, it is characterised in that static mixer pipe is heat exchanger form.
5. a kind of continuous countercurrent extraction 1, the complete set of equipments of 5- pentanediamines, it is characterised in that the equipment is included, modular 1,5-
Pentanediamine enzymatic conversion liquid material bucket（1）, pump（2）, Numerical control valve（3）, pressure gauge（4）, flowmeter（5）, extraction tower（7）, pump（8）, number
Control valve（9）, pressure gauge（10）, flowmeter（11）, extraction tower（16）, pump（17）, Numerical control valve（18）, pressure gauge（19）, flowmeter
（20）, extraction tower（29）；N-butanol charging basket（30）, pump（25）, Numerical control valve（26）, pressure gauge（28）, flowmeter（27）, pump
（21）, Numerical control valve（22）, pressure gauge（24）, flowmeter（23）, extraction tower（16）, pump（12）, Numerical control valve（13）, pressure gauge
（15）, flowmeter（14）, extraction tower（7）, connecting tube and Automated condtrol system；
Wherein, every extraction tower top is equipped with（6）Safety-valve.
6. complete set of equipments according to claim 5, it is characterised in that the control device of the automation, including temperature are visited
Head, the probe, digital controlled valve and control system pass through on-line checking extraction tower（7）、（16）、（29）Strict control extraction feed liquid
Temperature is in target temperature；Also include pump and be provided with flow sensor（5）、（11）、（14）、（20）、（23）、（27）；Pressure sensing
Device（4）、（10）、（15）、（19）、（24）、（28）And controller（3）、（9）、（13）、（18）、（22）、（26）, flow sensor
The pressure imported and exported and data on flows in pump are gathered with pressure sensor, and is transmitted to controller, are connect in controller provided with data
Module, processing module and communication module are received, data reception module is transferred to place after receiving the data message of two sensor transmissions
Module is managed, is finally transmitted again via communication module to service terminal；Service terminal receives the data message that controller is sent, and
It is shown in its display screen.
7. one kind 1,5- pentanediamine continuous countercurrent extraction techniques, continuous flow upstream is carried out by 1,5- pentanediamine enzymatic conversion liquid and n-butanol
Extraction, it is characterised in that：The technique is in counter-current extraction tower（7）、（16）、（29）It is middle to carry out, wherein, enzymatic conversion liquid and n-butanol enter
Enter extraction tower pre-mix zone to be premixed, premixed liquid enters stable region through extraction tower augmentation of heat transfer, mass-transfer zone, finally by stable region
Liquid-liquid separation is carried out into Disengagement zone, and in Disengagement zone.
8. technique according to claim 7, it is characterised in that enzyme reaction liquid passes sequentially through enzymatic conversion liquid tank (1), pump
(2)、（8）、（25）, digital controlled valve（3）、（13）、（22）, flowmeter（5）、（11）、（20）, pressure gauge（4）、（10）、（19）By
Level extraction.
9. technique according to claim 7, it is characterised in that n-butanol passes sequentially through batch can（30）, pump（25）、（21）、
（12）, digital controlled valve（26）、（22）、（13）, flowmeter（27）、（23）、（14）, pressure gauge（28）、（24）、（15）It is stripped step by step
Take.
10. technique according to claim 7, it is characterised in that premixed liquid entered equipped with the quiet of a positive and a negative spiral section
State blender；Wherein, static mixer control is made vertical tube heat exchanger form；And mixed liquor passes through tangential flow guiding pipe（42）And rotation
Turn cone and carry out liquid-liquid separation；
Wherein, operation temperature is 40 DEG C.
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