CN1329112C - Microwave assisted non-aqueous phase enzyme catalytic reacting device - Google Patents
Microwave assisted non-aqueous phase enzyme catalytic reacting device Download PDFInfo
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- CN1329112C CN1329112C CNB2005100389665A CN200510038966A CN1329112C CN 1329112 C CN1329112 C CN 1329112C CN B2005100389665 A CNB2005100389665 A CN B2005100389665A CN 200510038966 A CN200510038966 A CN 200510038966A CN 1329112 C CN1329112 C CN 1329112C
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Abstract
The present invention relates to a nonaqueous-phase enzyme catalytic reactor with microwave assistance, which belongs to the technical field of chemical reaction. The present invention uses a magnetron of a household microwave oven sold in market as an adjustable microwave emission source and combines the characteristic of enzyme reaction to arrange an enzyme reaction container in a microwave shielding cavity, and then the enzyme reaction container is combined with an automatic feedback control system with microwave shielding and temperature sensing by magnetic agitation, and gas agitation or non-gas agitation, so that the present invention is a combined machine which combines a microwave radiation catalytic mode and a nonaqueous-phase enzyme catalytic mode to catalytic organic reaction. Nonaqueous-phase enzyme catalytic reaction is carried out in the device, which has the following characteristics: reaction is kept at the temperature in the range of (+/-)1 DEG C under the keep of the continuous radiation of whole-range constant microwave power; reaction materials can be rapidly and uniformly mixed; inline sampling can be carried out under uninterrupted microwave radiation so as to really reflect the characteristic of nonaqueous-phase enzyme catalytic reaction in a microwave field. The device has the advantages of simple operation process and stable running and provides large convenience for researching enzyme catalytic reaction in a microwave field.
Description
Technical field
A kind of microwave assisted non-aqueous phase enzyme catalytic reacting device the invention belongs to the chemical reaction equipment technical field.
Background technology
The auxiliary nonaqueous phase enzymic catalytic reaction of microwave is a kind of with microwave radiation and two kinds of means of nonaqueous phase enzymatic and be used for the emerging synthetic technology of catalyse organic reaction, and the fuel factor of microwave and non-thermal effect make this technology can reach the catalytic effect that single catalytic way institute can not reach.
Domestic existing microwave reaction device is not fit to the temperature control unit and the agitator of enzymatic reaction, their temperature control principle is by regulating microwave power or controlling reaction temperature with the batch microwave mode of heating, thereby can't be used for studying and making full use of the non-thermal effect of microwave, and can not effectively guarantee the mechanical stability of enzyme catalyst, the uniformly dispersed and reaction safety of reaction system, can not control temperature of reaction system quickly and accurately.Also existing abroad expensive microwave reaction devices come out, and the reaction unit seen in the research report of relevant microwave-assisted enzyme catalysis mostly very is fit to enzymatic reaction at present, such as aspect temperature control and the variation of temperature amplitude.One of significant difference of enzymatic reaction and conventional chemical reaction is the former mildness, promptly can and generally react at a lower temperature; Two of difference is the sensitiveness of enzymatic reaction to variations in temperature, and 5 ℃ reaction temperature difference generally can not have considerable influence to the conventional chemical reaction, but often very big to the influence of enzymatic reaction.But existing microwave reaction device can not satisfy the meticulous control requirement of enzymic catalytic reaction to temperature.
Summary of the invention
The purpose of this invention is to provide a kind of microwave assisted non-aqueous phase enzyme catalytic reacting device, be to overcome the shortcoming that above-mentioned commercially available microwave reaction device is not suitable for the nonaqueous phase enzymatic reaction; This Design of device scheme is kept continuous radiation and micro-wave screening TEMP automatic feedback control system by the constant microwave power of whole process, reaction is remained in the scope of design temperature ± 1 ℃ carry out, and can in time show reaction temperature; The alr mode that adopts can the realization response system be uniformly dispersed, and suffered microwave radiation is even; Use additional load to make the range of choice of reaction system inventory bigger, can satisfy the requirement of nonaqueous phase enzymic catalytic reaction.The present invention adopts the magnetron of commercially available household microwave oven as the adjustable type microwave rf generator, the characteristics of desmoenzyme reaction, the enzyme reaction container is placed in the micro-wave screening cavity, with magnetic agitation and with or stir without gas, with micro-wave screening TEMP automatic feedback control system combination, be a kind of composite set that microwave radiation and two kinds of means of nonaqueous phase enzymatic is applied to simultaneously catalyse organic reaction.
Technical scheme
Apparatus structure
The present invention as shown in drawings, by the micro-wave screening temperature sensor, probe tube, the glass reaction container of strap clamp cover, the micro-wave screening cavity, magnetic stirring apparatus, cooling medium, temperature feedback control unit, additional load etc. partly constitute.
The micro-wave screening cavity is the closed stainless steel cavity, installs magnetic stirring apparatus additional in its bottom, as long as put into the magnetic agitation rotor in reaction vessel, can control mixing speed like a cork like this.Magnetic agitation after the improvement is compared with mechanical agitation, more convenient operation, and rotating speed is more stable; And stir more fully, it is more even that reaction system is disperseed, and overcome the uneven shortcoming of the suffered microwave radiation of reaction system; The simultaneous adaptation enzymic catalytic reaction requires the relatively mild characteristics of alr mode.Reaction vessel is the glass jacket reaction vessel that can see through microwave, can lead to different cooling mediums in the chuck.At micro-wave screening cavity back or sidepiece have the turnover interface tube of the circular hole of two about 3.5cm of diameter as cooling medium.A circular hole is opened on micro-wave screening cavity top, faces the reaction vessel mouth, and the circular hole on this top is as the insertion mouth of micro-wave screening temperature sensor, online sample tap and gas introduction tube mouth.Sensor, probe tube and gas introduction tube all insert in the reaction vessel.All perforates of micro-wave screening cavity are all installed metal sleeve additional with shield microwaves, and microwave leakage meets national safety standard.Adopt thermocouple to have accurately, stablize, reliably reach advantages such as inexpensive as temperature transducer.Thermocouple itself and transmission line thereof are metal materials, can produce induced current under microwave field, because kelvin effect and eddy current effect, self temperature raises, and make the temperature indicating value produce very mistake or can't carry out stable temperature survey.For eliminating microwave interference, mainly on thermocouple probe, install the aluminium foil and the metallic shield cover net of the anti-microwave interference of energy additional, and proofread and correct with kerosene thermometer.The temperature feedback control unit shows the reaction system real time temperature, and is used for default reaction temperature, and the keying that the control cooling medium is carried also is equipped with additional load in the micro-wave screening cavity.
Operation principle
Add reactant in reaction vessel, connect cooling medium in catalyst enzyme and the stirrer, reaction vessel chuck, be placed on then on the magnetic stirring apparatus, opening is over against the circular hole on micro-wave screening cavity top.If need to add reactant in the course of reaction in addition, the circular hole that can pass through top easily adds.Be the protection magnetron, should place additional load simultaneously in the micro-wave screening cavity (generally is Al
3O
2, molecular sieve, water or polar organic solvent etc. can absorb the material of microwave energy in a large number), the not absorbent excess energy of absorption reaction thing.Utilize the temperature feedback control unit to preset reaction temperature, start agitating device simultaneously, transfer to suitable rotating speed, and carry cooling medium to realize automatic accurate temperature controlling.
Beneficial effect
Compare with existing microwave reaction device, the present invention has outstanding technical characterstic, as realize finely dispersed reaction system and suffered microwave radiation evenly, the range of choice of reaction system amount more greatly, in time shows and control temperature, maintenance continuous microwave radiation and online sampling.Concrete technique table is at first high to temperature control requirement according to enzymic catalytic reaction characteristics now, temperature automatic feedback system and jacketed reaction container have been designed, and temperature measuring equipment is installed additional gauze screen make it to be subjected to the microwave radiation less, be reflected in the more stable temperature range and carry out; Next increases magnetic stirring apparatus and gas stirring device, and reaction system is in the even microwave radiation; Add the range of choice that additional load guarantees reaction safety and increases the system inventory once more; By being set, shielded-plate tube realizes the online sampling to reacting under the microwave field at last.This reaction unit can be used for studying the speed of microwave radiation for the nonaqueous phase enzymic catalytic reaction, and the influence of selective effect and kinetics provides necessary basic means for accelerating the biological organic synthesis of microwave organic chemistry, particularly microwave.
Description of drawings
Fig. 1 microwave-assisted enzyme catalyst reaction device schematic diagram.1, micro-wave screening cavity, 2, magnetron, 3, reaction vessel, 4, chuck, 5, magnetic stirring apparatus, 6,7, micro-wave screening cooling medium inlet and outlet connectors, 8, micro-wave screening cavity top micro-wave screening interface, 9, micro-wave screening temperature sensor, 10, probe tube, 11, gas introduction tube, 12, temperature feedback control unit, 13, additional load.
The specific embodiment
Referring to apparatus structure and operation principle part and accompanying drawing.
Embodiment 1: microwave assisted non-aqueous phase enzyme catalytic reacting device
In micro-wave screening cavity 1, place magnetron 2 as the adjustable type microwave rf generator, be built-in with glass reaction container 3 at the micro-wave screening cavity, this reaction vessel has chuck 4, reaction vessel places on the magnetic stirring apparatus 5, magnetic stirring apparatus places the bottom of micro-wave screening cavity, at micro-wave screening cavity back or sidepiece have two circular holes 6,7 inlet and outlet connectors as cooling medium, be connected with in the reaction vessel chuck by the outer cooling medium that inserts of micro-wave screening cavity, have a circular hole on micro-wave screening cavity top, it is top micro-wave screening interface 8, face the reaction vessel mouth, in circular hole, be equipped with micro-wave screening temperature sensor 9, online probe tube 10, adorn or do not adorn gas introduction tube 11, all perforates on the micro-wave screening cavity are all installed metal sleeve additional with shield microwaves, microwave leakage meets national safety standard, adopt thermocouple as temperature sensor, on thermocouple probe, install the aluminium foil and the metallic shield cover net of the anti-microwave interference of energy additional, the micro-wave screening temperature sensor is connected with temperature feedback control unit 12 by lead, the temperature feedback control unit shows the reaction system real time temperature, and be used for default reaction temperature, the keying that the control cooling medium is carried also is equipped with additional load 13 in the micro-wave screening cavity.
With concrete examples of implementation application of the present invention is described below.
Embodiment 2: amyl octylate is synthesized in microwave-assisted enzyme catalysis
With the glass jacket reaction vessel that n-amyl alcohol and the 0.06g distilled water of 3.6g caprylic acid and 2.2g places the microwave reaction device, to open magnetic agitation reaction system is mixed, it is 200w that microwave power is set, setting reaction temperature is 50 ℃.Open the microwave reaction device, adding immobilized lipase LRI 200mg and timing began after the question response temperature rose to 50 ℃.At the initial velocity of the different phase of reacting from the sample tap sampling and measuring reaction of this device.The initial velocity of the auxiliary nonaqueous phase enzymic catalytic reaction of this microwave is 4.2mmol/ming; And under other reaction condition same cases, the initial velocity of reaction in the conventional heating mode only is 1.8mmol/ming.The microwave radiation has obviously improved the initial velocity of reaction.
Embodiment 3: butyl caprylate is synthesized in microwave-assisted enzyme catalysis
The tetrahydrofuran solvent of 1.44g caprylic acid, 0.74g n-butanol, 0.02g distilled water and 15mL is added in the glass jacket reaction vessel of microwave reaction device, opening magnetic agitation mixes reaction system, it is 400w that microwave power is set, and setting reaction temperature is 55 ℃.Open the microwave reaction device, adding immobilized lipase LRI 100mg and timing began after the question response temperature rose to 55 ℃.At the initial velocity of the different phase of reacting from the sample tap sampling and measuring reaction of this device.The initial velocity of the auxiliary nonaqueous phase enzymic catalytic reaction of this microwave is 0.76mmol/ming; And under other reaction condition same cases, the initial velocity of reaction in the conventional heating mode only is 0.25mmol/ming.The microwave radiation has obviously improved the initial velocity of reaction.
Two examples of above embodiment 2,3 show, use this microwave assisted non-aqueous phase enzyme catalytic reacting device, not only can improve initial velocity of reaction greatly, and this device operating process is simple, stable, for the enzymic catalytic reaction in the research microwave field provides a great convenience.
Claims (2)
1, a kind of microwave assisted non-aqueous phase enzyme catalytic reacting device, it is characterized in that in micro-wave screening cavity (1), placing magnetron (2) as the adjustable type microwave rf generator, be built-in with glass reaction container (3) at the micro-wave screening cavity, this reaction vessel has chuck (4), reaction vessel places on the magnetic stirring apparatus (5), magnetic stirring apparatus places the bottom of micro-wave screening cavity, at micro-wave screening cavity back or sidepiece have the inlet and outlet connectors (6 of two circular holes as cooling medium, 7), be connected with in the reaction vessel chuck by the outer cooling medium that inserts of micro-wave screening cavity, have a circular hole on micro-wave screening cavity top, be that top micro-wave screening interface (8) faces the reaction vessel mouth, in the micro-wave screening interface, be equipped with micro-wave screening temperature sensor (9), online probe tube (10), adorn or do not adorn gas introduction tube (11), all perforates on the micro-wave screening cavity are all installed metal sleeve additional with shield microwaves, microwave leakage meets national safety standard, adopt thermocouple as temperature sensor, on thermocouple probe, install the aluminium foil and the metallic shield cover net of the anti-microwave interference of energy additional, the micro-wave screening temperature sensor is connected with temperature feedback control unit (12) by lead, the temperature feedback control unit shows the reaction system real time temperature, and be used for default reaction temperature, the keying that the control cooling medium is carried also is equipped with additional load (13) in the micro-wave screening cavity.
2, microwave assisted non-aqueous phase enzyme catalytic reacting device according to claim 1 is characterized in that additional load is Al
3O
2, or molecular sieve or water or polar organic solvent.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100389665A CN1329112C (en) | 2005-04-18 | 2005-04-18 | Microwave assisted non-aqueous phase enzyme catalytic reacting device |
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| CNB2005100389665A CN1329112C (en) | 2005-04-18 | 2005-04-18 | Microwave assisted non-aqueous phase enzyme catalytic reacting device |
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| CN1329112C true CN1329112C (en) | 2007-08-01 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103028359A (en) * | 2012-12-26 | 2013-04-10 | 内蒙古科技大学 | Microwave high-temperature chemical reaction system |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102085464B (en) * | 2009-12-04 | 2013-02-13 | 中国石油天然气股份有限公司 | Automatic temperature control matching sampling stirring tank |
| CN102133516A (en) * | 2010-10-25 | 2011-07-27 | 湘潭大学 | Microwave catalytic reactor system |
| CN104275138A (en) * | 2013-07-01 | 2015-01-14 | 东莞市华青节能科技有限公司 | Microwave heating type glass reaction kettle |
| CN108295785A (en) * | 2018-04-10 | 2018-07-20 | 铜仁学院 | A kind of multiphase large capacity microwave reaction device |
| GB2577911B (en) * | 2018-10-10 | 2022-11-02 | Aeon Eng Ltd | Maser Environmental-Analysis System |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1555912A (en) * | 2004-01-06 | 2004-12-22 | 中国科学院广州能源研究所 | High pressure visible micro wave chemical reaction device |
| CN2792604Y (en) * | 2005-04-18 | 2006-07-05 | 江南大学 | Non-aqueous phase enzyme catalytic reactor with microwave assistant |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1555912A (en) * | 2004-01-06 | 2004-12-22 | 中国科学院广州能源研究所 | High pressure visible micro wave chemical reaction device |
| CN2792604Y (en) * | 2005-04-18 | 2006-07-05 | 江南大学 | Non-aqueous phase enzyme catalytic reactor with microwave assistant |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103028359A (en) * | 2012-12-26 | 2013-04-10 | 内蒙古科技大学 | Microwave high-temperature chemical reaction system |
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