CN105170049A - Method of preparing hydrogen peroxide by utilizing microchannel reactor - Google Patents
Method of preparing hydrogen peroxide by utilizing microchannel reactor Download PDFInfo
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- CN105170049A CN105170049A CN201510579131.4A CN201510579131A CN105170049A CN 105170049 A CN105170049 A CN 105170049A CN 201510579131 A CN201510579131 A CN 201510579131A CN 105170049 A CN105170049 A CN 105170049A
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- hydrogen peroxide
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Abstract
The invention discloses a method of preparing hydrogen peroxide by utilizing a microchannel reactor. The method comprises the steps of firstly introducing the feed gases, namely hydrogen and oxygen, into a feeding channel respectively through a gas source, and feeding a liquid-phase carrier into a main channel, and enabling the hydrogen and the oxygen to rapidly disperse and mix through the promoting effect of the liquid-phase carrier; secondly loading a catalyst onto a chip unit so as to let the mixed hydrogen and oxygen moving forward along the main channel to mix with the catalyst and react under a certain temperature; finally,,bringing out reaction products by the liquid-phase carrier to enter a collection tank after the reaction is finished, and discharging a gas phase diluted in the collection tank or enabling the gas phase to enter a reaction system for recycling. According to the method disclosed by the invention, hydrogen and oxygen direct chemical combination is realized on a microreactor, so that the problem of high explosive danger of the combination is solved from the view of intrinsic safety, and the reaction conversion rate and selectivity are improved through the design of a microstructure.
Description
Technical field
The present invention relates to the preparing technical field of hydrogen peroxide, is specifically related to a kind of method utilizing micro passage reaction to prepare hydrogen peroxide.
Background technology
Hydrogen peroxide is a kind of common oxidants, due to the accessory substance that it does not produce contaminated environment in course of reaction, is acknowledged as the chemical products that a kind of green is clean, has been widely used in the industries such as chemical industry, weaving, papermaking, food, medical treatment.The industrial main stream approach of current hydrogen peroxide is anthraquinone (production capacity of external more than 95%, the production capacity of domestic more than 98%).Its main flow is: first form working solution with the derivative of suitable dissolution with solvents anthraquinone, is hydrogen anthraquinone in the presence of a catalyst with hydrogen by anthraquinone reduction wherein, and the latter's autoxidation under the existence of oxygen or air becomes anthraquinone and generates hydrogen peroxide.With the hydrogen peroxide in water extraction solution through being separated to obtain aqueous hydrogen peroxide solution, the further product of refining concentrated various concentration, the remaining liquid after extraction is got back to hydrogenation stage after treatment and is recycled., there is not oxygen and contact with the direct of hydrogen in anthraquinone technology maturation, safer in course of reaction, but its technological process more complicated, plant investment is large, big energy-consuming, and the organic solvent system toxicity used is large, and environmental pollution is serious.Because anthraquinone production technology is only got a profit when production scale comparatively large (producing more than 40,000 tons), need, after centralized production, finished product is transported to demand place, the security risk of hydrogen peroxide in transportation and extra cost are also one of defects of this type of production technology.
Producing hydrogen peroxide by hydrogen and the direct chemical combination of oxygen, is the production method of a kind of desirable atom economy, environmental protection.The method just receives the extensive concern of people after being proposed by Henkel and Weber from 1914, but is limited to the factor of technical elements, fails so far to realize suitability for industrialized production.First, while hydrogen is oxidized to hydrogen peroxide, oxyhydroxide generates the side reaction such as water, peroxide decomposition and hydrogen peroxide hydrogenation also with occurring, and can be favorable thermodynamics, reaction selective not high.Secondly, due to the explosion limit wide ranges (in oxygen 4%-94%, 4%-74% in air) of hydrogen, technical process easily fires, and danger coefficient is large.Dupont company once attempted producing hydrogen peroxide by direct synthesis under 10% hydrogen atmosphere, but took place frequently because of explosion accident, had to close a set of pilot-plant.As at the following concentration synthesize hydrogen peroxide of hydrogen explosion lower limit, too low productive rate needs again complicated isolation and identification step, increases production cost, infeasible economically.
Microfluidic control technology refers in the low-dimensional channel design of micron or nanoscale, and controlling volume is that Pi Shenghuo receives the liquid risen and carries out flowing and the technology of mass-and heat-transfer.The reaction yardstick of micro-fluid reactor is little, and specific area is large, and mass-and heat-transfer is thorough rapidly, can accurately control course of reaction and condition, in chemical industry synthesis, the existing application of field of biological detection, but prepares in hydrogen peroxide about the direct synthesis and but has no report.
Summary of the invention
The object of the present invention is to provide a kind of method utilizing micro passage reaction to prepare hydrogen peroxide, the realization of direct synthesis from hydrogen and oxygen on microreactor, solve it from the angle of essential safety and fire dangerous high problem, and improve reaction conversion ratio and selective by the design of micro-structural.
Its technical solution comprises:
A kind of method utilizing micro passage reaction to prepare hydrogen peroxide, described micro passage reaction comprises mixed zone, reaction zone and discharge zone, described mixed zone and reaction zone realize on micro-channel chip, described micro-channel chip comprises the microchannel of several arrays, described microchannel comprises for the wing passage of gas feed and the main channel passed through for liquid phase carrier, the afterbody of described discharge zone is connected with collecting tank, and described method comprises the following steps successively:
A, pass in described wing passage by gas source respectively by unstripped gas hydrogen, oxygen, in described main channel, input liquid phase carrier, hydrogen and oxygen are mixed rapidly by diffusion;
B, on described chip unit loading catalyst, mixed hydrogen, oxygen advance and catalyst mix along main channel, and react at a certain temperature;
C, reacted after, product is taken out of by liquid phase carrier and is entered in collecting tank, and gas phase is discharged after diluting in collecting tank or entered reaction system and recycles.
As a preferred version of the present invention, the first half stating wing passage is bending section, and latter half is flat segments, and described bending section is for promoting that unstripped gas mixes.
As another preferred version of the present invention, in step a, described gas source by unstripped gas successively by passing in wing passage after pressure-reducing valve, gas flowmeter.
Preferably, in step b, catalyst is carried on micro-channel chip by cladding process or completion method.
Preferably, in step b, by adding the time of staying that quencher controls unstripped gas in main channel.
Preferably, in step a, liquid phase carrier is water, acid solution or the acid solution containing halogen family ion.
Preferably, in step b, catalyst is for supporting in Al
2o
3, TiO
2, ZrO
2or the noble metal of Pd, Au, Pt or Ag on absorbent charcoal carrier or its alloy.
The Advantageous Effects that the present invention brings:
The invention provides a kind of new method that is safe, green, synthesize hydrogen peroxide easily.Compared with prior art, the present invention utilizes micro passage reaction to prepare hydrogen peroxide, because micro passage reaction size is little, specific area is large, the free radical that reaction generates with the continuous collision of tube wall in by quencher, flame is difficult to propagate, even if after hydrogen-oxygen mixing, an explosion occurred, few owing to relating to inventory, the little energy of blast release, the damage caused surrounding environment and personnel is also less, greatly can reduce the risk of oxyhydroxide process.Therefore, when reacting in micro passage reaction, the concentration of hydrogen and oxygen is no longer by the restriction of explosion limit, and directly enhancing reaction speed, turn avoid and adopt condition of high voltage to improve density of hydrogen, is a kind of new technology of Essential Safety.In addition, due to the light little portable of microreactor unit, output is adjustable flexibly, reactor directly can be installed to demand place, eliminates the risk of high-strength hydrogen peroxide in transportation.
The realization of direct synthesis from hydrogen and oxygen on microreactor in the present invention, solves it from the angle of essential safety and fires dangerous high problem, and improves reaction conversion ratio and selective by the design of micro-structural.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention will be further described:
The apparatus structure schematic diagram that Fig. 1 adopts for preparation method of the present invention;
Fig. 2 chip unit contacts with liquid phase carrier after gas phase premix form bubble schematic diagram;
Fig. 3 be on chip unit gas phase contact with liquid phase carrier form bubble after the schematic diagram that mixes;
Fig. 4 is the structural representation of the main pipeline with surface micro-structure;
Fig. 5 is the part annexation schematic diagram of collecting tank and micro passage reaction;
In figure, 1, micro passage reaction, 2, hydrogen container, 2a, hydrogen, 3, oxygen container, 3a, oxygen, 4, liquid phase carrier, 5, collecting tank, 6, quencher, 7, reaction zone in microchannel.
Detailed description of the invention
The invention discloses a kind of method utilizing micro passage reaction to prepare hydrogen peroxide, in order to make advantage of the present invention, technical scheme clearly, clearly, below in conjunction with specific embodiment, the present invention being elaborated.
As shown in Figure 1, being prepared in micro passage reaction 1 of hydrogen peroxide of the present invention is reacted, the structure of micro passage reaction and prior art are substantially similar, it is formed by stacking by a few core assembly blade unit, every core assembly blade unit there are several passages, pass through for unstripped gas and liquid phase carrier in passage, chip unit is loaded with catalyst in microchannel reaction zone 7, and the direct combination reaction of hydrogen-oxygen occurs at this.
With micro passage reaction with the use of have hydrogen container 2, oxygen container 3 and collecting tank 5, hydrogen container, oxygen container are communicated with the feeding-passage of micro passage reaction respectively, the pipeline be communicated with is provided with pressure-reducing valve and gas flowmeter, for monitoring the flow of unstripped gas, collecting tank 5 for by emptying for the gas dilution in product or be recycled to reaction system utilize, the present invention selects inert gas dilution.
The selection of catalyst and load mode: the direct chemical combination of hydrogen-oxygen generally adopts Pd, Au, Pt or Ag catalyst, common catalytic agent carrier is Al
2o
3, TiO
2, ZrO
2or active carbon, the loading method that can adopt is generally but is not limited to coating and completion method; Coating is generally applicable to the microchannel of less internal diameter, and by catalyst (and carrier) with in the form introduction passage of suspension, the processes such as drying dehydration form the catalyst coat of coated channel inner surface; Completion method is generally applicable to the microchannel compared with large diameter, is a kind of catalyst (and carrier) to be supported on packaged type filler surface (as bead), after this filler filled the practice of full microchannel.
Chip unit: the function that chip needs realize is the Homogeneous phase mixing of hydrogen and oxygen, by the catalyst layer in microchannel reaction zone 7 under carrier phase induced effect or under pressure promotion, product finally flows out chip.When use liquid-carrier facies tract move gas bubbles move time, hydrogen and oxygen can be pre-mixed evenly and liquid comes into contact, also certain passage node while, can form bubble with liquid comes into contact.When using pressure directly to promote, direct and catalyst exposure after hydrogen and oxygen mix.
Unstripped gas mixes: the mixed proportion due to hydrogen 2a and oxygen 3a directly affects the composition of product, should be mixed with before catalyst exposure at admixture of gas, two kinds of gases can contact front premix with liquid phase carrier 4, as shown in Figure 2, also can contact with liquid-carrier after forming bubble simultaneously and mix, as shown in Figure 3.The micro-structural of pipeline can be utilized to promote, and gas flowing is to strengthen mixed effect, and bend portions section as shown in Figure 2,3, compared with flat segments, mixed effect is better.
By design and the interpolation of micro-structural in main pipeline, mass transfer enhancement can be passed through, accurately control the functions such as the time of staying.By designing rough surface or column structure in microchannel reaction zone 7, as shown in Figure 4, increase the catalyst layer specific area that can apply, improve reaction efficiency further.By introducing quencher 6 and diluent also accurate coutroi velocity in pipeline fixed position, the time of staying and the reaction time of material accurately can be controlled.
In the process flowing through catalyst, hydrogen-oxygen material reaction not exclusively, when conversion ratio is lower, may be necessary to reclaim unreacted material, recycles.Product due to this reaction is liquid, easily be separated with unreacted material, after chip, establish collection/separation list and collecting tank 5, utilize gravity to carry out gas-liquid separation, be separated the gaseous product obtained after pressurization, reenter the reaction of a chip participation new round, as shown in Figure 5.
The invention provides a kind of device utilizing hydrogen and the direct chemical combination of oxygen to prepare hydrogen peroxide, this device optionally also can add micro-mixer, reducer union, product-collecting unit etc. before reactor.
Embodiment 1:
In the test of laboratory, gas source is hydrogen and oxygen gas cylinder, gas is decompressed to 2MPa through pressure-reducing valve, control flow by mass flowmenter and be respectively 5sccm, 5sccm (or other ratio), enter chip reaction member by after reducer union by Teflon flexible pipe.Liquid-carrier is phosphoric acid, the sulfuric acid mixture liquid of sodium bromide mutually, sucks in 100mL syringe in advance, and promote to enter chip reaction member by syringe pump, flow velocity is 0.01mL/min.Gas phase mixes near Reactor inlet with liquid phase, and water is continuous phase, and bubble is decentralized photo, and the passage jointly by supporting catalyst reacts.Product enters collector and carries out two separation, and gas phase is discharged system after dilution or reentered reaction system and recycles.
The direct chemical combination of current hydrogen-oxygen prepares the catalyst of hydrogen peroxide based on Pd and Au, and catalyst carrier is mainly Al
2o
3, TiO
2, ZrO
2or active carbon, the research of second metal active constituent that adulterates also has obtained certain progress.Catalyst loading is mainly contained two kinds to the method in reaction channel: cladding process and completion method.The former principle is that the suspension of catalyst and carrier (Pd/C as 5%wt) or colloidal sol (as PMI method) are passed through reaction channel at a slow speed, catalyst and carrier are adsorbed on tube wall by physical action, through solvent seasoning (by gas flow purging or natural drying) after a while, form one deck catalyst layer of coated inner tubal wall.The principle of the latter is the outside first catalyst and carrier being coated on certain medium (as bead etc.), then by this Filled Dielectrics in reaction channel, form the three-dimensional packing space of catalyst.
After pressure and Flow-rate adjustment, enter chip by the gas of electrolytic preparation or cylinder storage, under surface tension effects, form bubble, advance and catalyst exposure along passage.Two kinds of gas can before entering chip premix, before can contacting with liquid phase on chip, premix as shown in Figure 2, also can contact with liquid-carrier in a certain position of passage simultaneously form bubble as shown in Figure 3, the relative concentration of two kinds of gases is determined by the relative velocity of the two, as: when using Fig. 3 structure, as hydrogen and oxygen flow are 5sccm, be then 1:1 at the ratio of the two molar concentration of reaction zone.
In flat tube, the mixing of gas in bubble mainly relies on diffusion and bubble to contact the bubble internal convection caused with tube wall, when by pipeline from straight become bending time, by change gas in bubble to flow path direction, promote gas and vapor permeation.As: add crooked pipeline structure in flat tube section, main line width is 100 μm, and bending section width is constant, and each angle of bend is 90 °.Angle of bend and width also can adopt other numerical value, as shown in Figure 2,3.
When flow velocity one timing of liquid-carrier phase, the time of staying of material accurately can be controlled by the flow distance controlling liquid.As shown in Figure 4, when control flow rate of liquid is 0.01mL/min, when pipeline diameter is 50 μm, introduce free radical quencher or diluent gas when bubble flows through distance 10mm with liquid in bubble, can control the reaction time is 118ms.
Although because wall effect causes the easy cancellation of free radical in micro passage reaction, flame is not easily propagated, and this proposes requirement to channel size, when reactor size exceedes certain threshold value, fire and still likely occur.Meanwhile, for membrane reactor, although it thoroughly solves the isolating problem of hydrogen and oxygen, reaction only occurs on the microporous barrier supporting catalyst, and reaction efficiency is not high.If the two is combined, membrane reactor is designed and sized to microreactor size, oxygen stream is passed in " membrane channels " inside, outside passes into hydrogen stream, reaction outside wall still by general microreactor processing method, just can comprehensively the two advantage and improve security and the efficiency of reaction further.
It should be noted that, under the instruction of this description, those skilled in the art can also make such or such easy variation pattern, such as equivalent way, or obvious mode of texturing, all should within protection scope of the present invention.
Claims (7)
1. the method utilizing micro passage reaction to prepare hydrogen peroxide, it is characterized in that: described micro passage reaction comprises mixed zone, reaction zone and discharge zone, described mixed zone and reaction zone realize on micro-channel chip, described micro-channel chip comprises the microchannel of several arrays, described microchannel comprises for the wing passage of gas feed and the main channel passed through for liquid phase carrier, the afterbody of described discharge zone is connected with collecting tank, and described method comprises the following steps successively:
A, pass in described wing passage by gas source respectively by unstripped gas hydrogen, oxygen, in described main channel, input liquid phase carrier, hydrogen and oxygen are mixed rapidly by diffusion;
B, on described chip unit loading catalyst, mixed hydrogen, oxygen advance and catalyst mix along main channel, and react at a certain temperature;
C, reacted after, product is taken out of by liquid phase carrier and is entered in collecting tank, and gas phase is discharged after diluting in collecting tank or entered reaction system and recycles.
2. the method utilizing micro passage reaction to prepare hydrogen peroxide according to claim 1, is characterized in that: the first half of described wing passage is bending section, and latter half is flat segments, and described bending section is for promoting that unstripped gas mixes.
3. the method utilizing micro passage reaction to prepare hydrogen peroxide according to claim 1, is characterized in that: in step a, described gas source by unstripped gas successively by passing in wing passage after pressure-reducing valve, gas flowmeter.
4. the method utilizing micro passage reaction to prepare hydrogen peroxide according to claim 1, it is characterized in that: in step b, catalyst is carried on micro-channel chip by cladding process or completion method.
5. the method utilizing micro passage reaction to prepare hydrogen peroxide according to claim 1, is characterized in that: in step b, by adding the time of staying that quencher controls unstripped gas in main channel.
6. the method utilizing micro passage reaction to prepare hydrogen peroxide according to claim 1, is characterized in that: in step a, and liquid phase carrier is water, acid solution or the acid solution containing halogen family ion.
7. the method utilizing micro passage reaction to prepare hydrogen peroxide according to claim 1, it is characterized in that: in step b, catalyst is for supporting in Al
2o
3, TiO
2, ZrO
2or the noble metal of Pd, Au, Pt or Ag on absorbent charcoal carrier or its alloy.
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Cited By (10)
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| CN107216296A (en) * | 2016-03-22 | 2017-09-29 | 中国石油化工股份有限公司 | The method that expoxy propane is prepared in micro passage reaction |
| CN108704589A (en) * | 2018-05-23 | 2018-10-26 | 西南民族大学 | Prepare the micro passage reaction of 2 cyano pyrazine |
| CN108786677A (en) * | 2018-05-31 | 2018-11-13 | 浙江大学 | A kind of microreactor of Click labelled synthesis PET developers and its preparation and reaction method |
| CN108815866A (en) * | 2018-05-31 | 2018-11-16 | 浙江大学 | One kind being used for drying18The glass-micropipe of F ion reagent and its preparation, drying means |
| CN108976271A (en) * | 2018-06-27 | 2018-12-11 | 浙江大学 | A kind of synthesis18The method of F-FLT |
| CN109134381A (en) * | 2018-06-27 | 2019-01-04 | 浙江大学 | A kind of micro-fluidic synthesis18The method of F-FMISO |
| CN109387544A (en) * | 2018-09-03 | 2019-02-26 | 中国辐射防护研究院 | High activity liquid waste basin hydrogen gas mixture explosion source item evaluation method |
| CN109589890A (en) * | 2019-01-11 | 2019-04-09 | 北京机械设备研究所 | A kind of hydrogen peroxide synthesizer and method |
| WO2021047057A1 (en) * | 2019-09-14 | 2021-03-18 | 南京延长反应技术研究院有限公司 | System and process for preparing hydrogen peroxide based on isopropanol method |
| CN112996591A (en) * | 2018-04-17 | 2021-06-18 | 以列特环球能源解决方案有限公司 | Hydrogen reactor with catalyst in flow conduit |
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| CN107216296A (en) * | 2016-03-22 | 2017-09-29 | 中国石油化工股份有限公司 | The method that expoxy propane is prepared in micro passage reaction |
| CN107216296B (en) * | 2016-03-22 | 2020-07-17 | 中国石油化工股份有限公司 | Method for preparing propylene oxide in microchannel reactor |
| CN112996591B (en) * | 2018-04-17 | 2023-08-29 | 以列特环球能源解决方案有限公司 | Hydrogen reactor with catalyst in flow conduit |
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| CN108704589A (en) * | 2018-05-23 | 2018-10-26 | 西南民族大学 | Prepare the micro passage reaction of 2 cyano pyrazine |
| CN108786677B (en) * | 2018-05-31 | 2019-11-05 | 浙江大学 | A kind of microreactor of Click labelled synthesis PET imaging agent and its preparation and reaction method |
| CN108786677A (en) * | 2018-05-31 | 2018-11-13 | 浙江大学 | A kind of microreactor of Click labelled synthesis PET developers and its preparation and reaction method |
| CN108815866A (en) * | 2018-05-31 | 2018-11-16 | 浙江大学 | One kind being used for drying18The glass-micropipe of F ion reagent and its preparation, drying means |
| CN108815866B (en) * | 2018-05-31 | 2019-11-05 | 浙江大学 | One kind being used for drying18The glass-micropipe of F ion reagent and its preparation, drying means |
| CN108976271A (en) * | 2018-06-27 | 2018-12-11 | 浙江大学 | A kind of synthesis18The method of F-FLT |
| CN109134381B (en) * | 2018-06-27 | 2020-06-30 | 浙江大学 | Microfluidic synthesis18Method of F-FMISO |
| CN109134381A (en) * | 2018-06-27 | 2019-01-04 | 浙江大学 | A kind of micro-fluidic synthesis18The method of F-FMISO |
| CN109387544B (en) * | 2018-09-03 | 2021-01-15 | 中国辐射防护研究院 | Method for estimating explosion source item of hydrogen mixed gas in high-level radioactive waste liquid storage tank |
| CN109387544A (en) * | 2018-09-03 | 2019-02-26 | 中国辐射防护研究院 | High activity liquid waste basin hydrogen gas mixture explosion source item evaluation method |
| CN109589890A (en) * | 2019-01-11 | 2019-04-09 | 北京机械设备研究所 | A kind of hydrogen peroxide synthesizer and method |
| WO2021047057A1 (en) * | 2019-09-14 | 2021-03-18 | 南京延长反应技术研究院有限公司 | System and process for preparing hydrogen peroxide based on isopropanol method |
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