CN101524631B - Electrothermal microreactor preparation system - Google Patents
Electrothermal microreactor preparation system Download PDFInfo
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- CN101524631B CN101524631B CN2009100293622A CN200910029362A CN101524631B CN 101524631 B CN101524631 B CN 101524631B CN 2009100293622 A CN2009100293622 A CN 2009100293622A CN 200910029362 A CN200910029362 A CN 200910029362A CN 101524631 B CN101524631 B CN 101524631B
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Abstract
The invention relates to an electrothermal microreactor preparation system which is characterized by comprising a peristaltic pump, a micro-mixer, an intelligent PID temperature controller, a micro fluid reactor and an electric heater, wherein the input end of the peristaltic pump is connected with different reaction material containers through two or more than two connecting pipes; the output end of the peristaltic pump is connected with the input end of the micro-mixer through a connecting pipe; the output end of the micro-mixer is connected with the input end of the micro fluid reactor through a connecting pipe; the micro fluid reactor (8) is connected with a product collecting device and mounted on the electric heater; and the electric heater is electrically connected with the intelligent PID temperature controller; and a liquid supply channel in the micro fluid reactor is provided with a micro temperature sensor. The invention can be used as a tool for the production and researchof continuous quantum points. In the production and research of continuous quantum points, the invention heats evenly, can work in the environment with high temperature, has environmental friendly working conditions, is stable and safe, and has low cost.
Description
Technical field
The present invention relates to a kind of little Chemical Process Equipment, especially a kind of with low cost, control is simple and precision is higher, working environment close friend's the doctorization preparation of product system based on microreactor, specifically a kind of electrothermal microreactor preparation system that can be used for quantum dot experiment and preparation.
Background technology
As everyone knows, the reinforcement passage of technical process is divided into two branches at present, and one is the large of equipment, the application of HTHP and critical condition; Another one is exactly the microminiaturization development of equipment.The former fund input is big, and actual production capacity data and small lot test data have bigger discrepancy, and microminiaturization has small investment, the advantage of stable reaction, especially the conversion ratio that reacts under minute yardstick, selectivity obviously improve, heat transfer coefficient and mass-transfer performance are strengthened greatly, and therefore little chemical industry equipment and process are acknowledged as one of important directions of current Chemical Engineering subject development.
The microchannel size of microreactor inner fluid, is compared with traditional consersion unit to the submillimeter magnitude in sub-micron, and its advantage is the reinforcement of quality and heat transfer process and the improvement of fluid-flow mode.In microreactor, thermograde is along with the very fast increase that reduces of linear content, and the remarkable increase of driving force of heat transfer has enlarged the thermal diffusion flux of unit volume or unit are; In addition, by reducing fluid thickness, the corresponding area-volume ratio that increased.Therefore by controlling reaction time and reaction temperature accurately, control the process of reaction, improve conversion of raw material, and because reducing of reaction volume can reduce the harm that dangerous generation is produced to greatest extent.
Aspect the microreactor heat exchange mode, early stage over-borrowing helps modes such as oil bath, water-bath, baking oven or ice chest.This mode influences the integrated and accuracy control over temperature of microreactor and system element, and is unfavorable for on-line monitoring.Therefore integrated heat exchange unit and raw material mixes and reacts the development trend that becomes microreactor.
When oil bath was heated, oil bath can be considered a stable temperature field on the whole, but the flowability of fluid in heating process, had caused the difference of temperature between regional area, and instrument shows non-true test temperature; And the oil bath equipment volume is bigger, heavy, is subjected to condition restriction such as place; Add deep fat and be heated and cause air pollution easily in the process, bring harmful effect to be subjected to surrounding environment; And adding the influence of deep fat boiling point, the reaction system maximum heating temperature is restricted, and more because conduction oil is volatile under the condition of high temperature, for the long-time reaction that needs heating, also so has also limited the prolongation of heat time heating time.Chinese invention patent (application number 200610088398.4) discloses a kind of composite heat transfer micro reactor, can realize the control of many humidity provinces; Chinese invention patent (application number 200710048166.0) discloses a kind of combined type heat exchange filling type micro-reactor, Chinese invention patent (application number 200610085433.7) discloses a kind of micro passage reaction that utilizes and has prepared method of bio-diesel oil, Chinese invention patent (application number 200710134498.0) discloses method and a kind of method of utilizing micro passage reaction to prepare nano zeolite of Chinese invention patent (application number 200710021824.7) that a kind of micro passage reaction prepares fatty acid ester, more than Fan Ying heat provides, and all is to obtain by the oil bath heating.By relatively can finding, inhomogeneous and equipment volume is huge with the heating of finish application bath heating ubiquity is unfavorable for shortcomings such as integrated.
Summary of the invention
The objective of the invention is to adopt oil bath to heat that the inhomogeneous and equipment volume of existing heating is huge to be unfavorable for integrated shortcoming at existing microreactor, it is lower to design a kind of cost, working environment is good, the electrothermal microreactor preparation system that operating condition is controlled easily and is beneficial to processing.
Technical scheme of the present invention is:
A kind of electrothermal microreactor preparation system, it is characterized in that it comprises peristaltic pump 3, micro-mixer is 4, intelligent PID temperature controller 5, micro-fluid reactor 8 and electric heater 9, the input of described peristaltic pump 3 is continuous with different reaction raw materials containers 1 by two or more tube connectors, the output of peristaltic pump 3 links to each other by the input of tube connector with micro-mixer 4, the output of micro-mixer 4 links to each other by the input of tube connector with micro-fluid reactor 8, micro-fluid reactor 8 is connected with product gathering-device 6, micro-fluid reactor 8 is installed on the electric heater 9, electric heater 9 is electrically connected with intelligent PID temperature controller 5, on the feed flow runner in micro-fluid reactor 8 micro temperature sensor 10 is installed.
Described electric heater 9 is made up of base plate 93, thermal insulation layer 94, thermoelectric resistance layer 95, insulating barrier 96, heating plate 97 successively, they connect into an integral body by securing member 98, uniform winding has resistance wire 92 on thermoelectric resistance layer 95, a plurality of temperature sensors 7 are installed on heating plate 97, and the output of temperature sensor 7 links to each other with the corresponding input of intelligent PID temperature controller 5.
Described temperature sensor 7 is inlaid in the described heating plate 97.
The temperature-sensitive head of described micro temperature sensor 10 is arranged in the feed flow runner of micro-fluid reactor 8.
Described micro-fluid reactor 8 is the stainless steel microreactor, and the hydraulic radius of the feed flow runner that it is inner is a passage 0.05-0.07 millimeter.
Beneficial effect of the present invention:
1, the present invention adopts electrical heating to avoid the inhomogeneities of oil bath heating-up temperature field, can realize the constant unification of temperature at whole plate face, simultaneously by adopting the intelligent PID temperature controller can realize the intelligent thermostatic control of whole temperature and can regulate automatically, control is convenient, is that advanced temperature control technique is used in the novelty in microreactor field;
2, the present invention has avoided oil bath firing equipment volume heaviness, is subjected to the shortcoming of place restriction, can finish the heating of temperature in a less space, realizes succinct light effect;
3, the present invention has avoided the oil bath heating time to add deep fat being heated and causing the air-polluting influence easily, the working environment close friend in the process;
4, the present invention has avoided adding the influence that deep fat is subjected to the boiling point restriction, can require to change heating power according to reaction system and improve heating-up temperature and prolong heat time heating time;
5, the present invention can adopt conventional material and manufacturing process to be realized, so cost is lower.
Description of drawings
Fig. 1 is the schematic diagram of preparation structure of the present invention.
Fig. 2 is the structural representation of electric heater of the present invention.
Fig. 3 is the layout drawing of thermoelectric heated filament of the present invention.
Fig. 4 is the arrangement schematic diagram of the temperature detecting resistance on the electric boiling plate of the present invention.
Fig. 5 is the installation site schematic diagram of micro temperature sensor of the present invention in the feed flow runner.
2 is the second reaction raw materials container among the figure, and 91 is micro thermocouple.
The specific embodiment
The present invention is further illustrated below in conjunction with drawings and Examples.
As shown in Figure 1.
A kind of electrothermal microreactor preparation system, it comprises peristaltic pump 3, micro-mixer is 4, intelligent PID temperature controller 5, micro-fluid reactor 8 and electric heater 9 etc., their annexation as shown in Figure 1, the input of described peristaltic pump 3 is continuous with different reaction raw materials containers 1 (liquid material for reaction or synthetic usefulness is housed respectively in two or more material containers 1) by two or more tube connectors, the output of peristaltic pump 3 links to each other by the input of tube connector with micro-mixer 4, the output of micro-mixer 4 links to each other by the input of tube connector with micro-fluid reactor 8, micro-fluid reactor 8 is connected with product gathering-device 6, micro-fluid reactor 8 can adopt the stainless steel microreactor (can adopt the disclosed microreactor of existing Chinese patent, the stainless steel microreactor that also can adopt the applicant to apply for is on the same day realized), the hydraulic radius of the feed flow runner that it is inner is a passage 0.05-0.07 millimeter.Micro-fluid reactor 8 is installed on the electric heater 9, electric heater 9 is electrically connected with intelligent PID temperature controller 5, on the feed flow runner in micro-fluid reactor 8 micro temperature sensor 10 is installed, the temperature-sensitive head of micro temperature sensor 10 is arranged in the feed flow runner of micro-fluid reactor 8.
During concrete enforcement, the structure of electric heater 9 as shown in Figure 2, it is made up of base plate 93, thermal insulation layer 94, thermoelectric resistance layer 95, insulating barrier 96, heating plate 97 successively, they connect into an integral body by securing member 98, uniform winding has resistance wire 92 (as shown in Figure 3) on thermoelectric resistance layer 95, on heating plate 97, be embedded with a plurality of temperature sensors 7 be installed, its arrangement as shown in Figure 4, the corresponding input of the output of temperature sensor 7 and intelligent PID temperature controller 5 links to each other.
Details are as follows:
Electric heater is divided into 5 layers: base plate 93, thermal insulation layer 94, thermoelectric resistance layer 95, insulating barrier 96, heating plate 97 and securing member 98.Uniform winding resistance wire 92 on thermoelectric resistance layer, through software temperature field numerical simulation analysis, this method for arranging helps the even distribution in temperature field.For requiring temperature for the reaction below 350 ℃, require resistance can meet the demands at 100 Ω.Arrange temperature sensor 7 in different azimuth on the heating plate 97, because it is blocked up that the thickness of heating plate is difficult for, and is unfavorable for transmitting rapidly heat, therefore common sensor can't be used, adopting diameter herein is miniature armoured thermocouple-K type of 1mm, has satisfied the requirement for heating plate thickness.This thermocouple can be measured the temperature about 800 ℃, has good linear relationship for the temperature survey below 350 ℃.As shown in Figure 2.
The material that electric heater adopted: base plate 93 is firm heat proof material stainless steel, thermal insulation layer 94 adopts hear resistance, and asbestos, thermoelectric resistance layer 95 adopt fe-cr-ni alloy Cr20Ni80 preferably, insulating barrier 96 adopts mica sheet (heat conduction and insulation), heating plate 97 adopts heat transfer property aluminium sheet preferably, reduce PID adjusting time heat time heating time, 98 of securing members adopt general carbon steel material, and the stretch-proof performance is good.
Intelligent PID temperature controller 5 has a plurality of demonstration epi-positions, and one of them can be used for controlling temperature, and all the other then by connecting the temperature sensor of different parts, show real time temperature.As connecting temperature sensor 7 and the built-in micro temperature sensor 10 of pipeline on the heating plate 97.
For the mensuration of temperature in the pipeline, adopt the mode that built-in temperature sensor is installed to carry out under normal conditions, but because conveyance conduit too tiny (2mm), general temperature sensor can't play effect.Measure if collect again, bigger heat loss is then arranged, and therefore situation that can not the actual response temperature adopts special miniature armoured thermocouple 101, be built in the stainless steel pipes 102 (being the feed flow microchannel), can finish monitoring out temperature.Snap joint is installed at two of taking over to be satisfied and being connected and sealing of other pipelines.
The hydraulic radius of the feature channel size of micro-fluid reactor is about 0.06mm, and passage length is about 565mm.
Below be to utilize preparation system of the present invention to carry out two reference cases of quantum dot experiment, to those skilled in the art, can carry out equivalent transformation with reference to content of the present invention and reference case fully.
Reference example 1.
Cadmium presoma preparation: get 0.6ml oleic acid (0A, 90%) and 3.4ml octadecylene (ODE, 90%), dissolving 25.68mg cadmium oxide powder (Cd0,99.9%) is heated to 200 ℃ (helping abundant dissolving) on the magnetic force heating stirrer, obtain yellow transparent solution, and be cooled to about 40 ℃.The preparation of selenium presoma: get positive tri octyl phosphine (TOP, 90%) 1.8ml and 2.2mlODE, dissolving selenium powder (Se, 99.5%) 78.96mg is heated to 100 ℃ on the magnetic force heating stirrer, obtain colourless transparent solution, and be cooled to about 40 ℃.It is 260 ℃ that reaction temperature is set, and when reaction time was 30s, 45s, 60,120s, the gained lateral size of dots was 4.2nm, 4.3nm, 4.4nm, 4.6nm.Color adds gradually with the prolongation of reaction time and is deep to bronzing as a result, shows under different reaction time conditions, obtains the different CdSe quantum dot of particle diameter
Reference example 2.
Cadmium presoma preparation: get 0.6ml oleic acid (0A, 90%) and 3.4ml octadecylene (ODE, 90%), dissolving 25.68mg cadmium oxide powder (CdO, 99.9%) is heated to 200 ℃ (helping abundant dissolving) on the magnetic force heating stirrer, obtain yellow transparent solution, and be cooled to about 40 ℃.The preparation of selenium presoma: get positive tri octyl phosphine (TOP, 90%) 1.8ml and 2.2mlODE, dissolving selenium powder (Se, 99.5%) 78.96mg is heated to 100 ℃ on the magnetic force heating stirrer, obtain colourless transparent solution, and be cooled to about 40 ℃.It is 300 ℃ that reaction temperature is set, and when reaction time was 30s, 45s, 120s, the gained lateral size of dots was 4.2nm, 4.2nm, 4.6nm.The result is similar to reference example 1, and color adds gradually with the prolongation of reaction time and is deep to bronzing, shows under different reaction time conditions, obtains the different CdSe quantum dot of particle diameter.
The part that the present invention does not relate to prior art that maybe can adopt all same as the prior art is realized.
Claims (4)
1. electrothermal microreactor preparation system, it is characterized in that it comprises peristaltic pump (3), micro-mixer (4), intelligent PID temperature controller (5), micro-fluid reactor (8) and electric heater (9), the input of described peristaltic pump (3) is continuous with different reaction raw materials containers (1) by two or more tube connectors, the output of peristaltic pump (3) links to each other by the input of tube connector with micro-mixer (4), the output of micro-mixer (4) links to each other by the input of tube connector with micro-fluid reactor (8), micro-fluid reactor (8) is connected with product gathering-device (6), micro-fluid reactor (8) is installed on the electric heater (9), electric heater (9) is electrically connected with intelligent PID temperature controller (5), and micro temperature sensor (10) is installed on the feed flow runner in micro-fluid reactor (8); Described electric heater (9) is made up of base plate (93), thermal insulation layer (94), thermoelectric resistance layer (95), insulating barrier (96), heating plate (97) successively, they connect into an integral body by securing member (98), go up uniform winding in thermoelectric resistance layer (95) resistance wire (92) is arranged, a plurality of temperature sensors (7) are installed on heating plate (97), and the output of temperature sensor (7) links to each other with the corresponding input of intelligent PID temperature controller (5).
2. electrothermal microreactor preparation system according to claim 1 is characterized in that described temperature sensor (7) is inlaid in the described heating plate (97).
3. electrothermal microreactor preparation system according to claim 1 is characterized in that the temperature-sensitive head of described micro temperature sensor (10) is arranged in the feed flow runner of micro-fluid reactor (8).
4. electrothermal microreactor preparation system according to claim 1 is characterized in that described micro-fluid reactor (8) is the stainless steel microreactor, the hydraulic radius 0.05-0.07 millimeter of the feed flow runner that it is inner.
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| CN2009100293622A CN101524631B (en) | 2009-04-10 | 2009-04-10 | Electrothermal microreactor preparation system |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| GB2494623B (en) | 2011-09-02 | 2013-09-25 | Tristel Plc | Pump apparatus |
| WO2015005407A1 (en) | 2013-07-09 | 2015-01-15 | 三菱化学株式会社 | Zeolite production method |
| CN103551096B (en) * | 2013-10-25 | 2015-05-27 | 南京工业大学 | Carbon fiber microchip reactor |
| CN103949198B (en) * | 2014-04-16 | 2016-02-03 | 中国地质大学（武汉） | Integrated form crystal gel medium progressive forming device |
| CN105749833B (en) * | 2016-05-18 | 2018-06-29 | 杭州沈氏节能科技股份有限公司 | A kind of reactor with channel design |
| CN109634321B (en) * | 2018-12-31 | 2021-02-05 | 西安优耐特容器制造有限公司 | Accurate temperature control system and method suitable for micro-reaction experiment |
| CN113617309B (en) * | 2021-08-06 | 2022-09-23 | 温州大学新材料与产业技术研究院 | Intelligent temperature control microfluid reaction device and method for controllably synthesizing composite material |
| CN113976056B (en) * | 2021-11-04 | 2022-09-06 | 南京星宁环保科技有限公司 | Integrated device of continuous flow method and application thereof |
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