CN105170049B - The method for preparing hydrogen peroxide using micro passage reaction - Google Patents
The method for preparing hydrogen peroxide using micro passage reaction Download PDFInfo
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- CN105170049B CN105170049B CN201510579131.4A CN201510579131A CN105170049B CN 105170049 B CN105170049 B CN 105170049B CN 201510579131 A CN201510579131 A CN 201510579131A CN 105170049 B CN105170049 B CN 105170049B
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Abstract
The invention discloses a kind of methods for preparing hydrogen peroxide using micro passage reaction, it passes through gas source first and each leads into unstripped gas hydrogen, oxygen in the feeding-passage, liquid phase carrier, hydrogen and oxygen are inputted into main channel, and mixing is spread rapidly by the facilitation of liquid phase carrier；Then the loading catalyst on chip unit, mixed hydrogen, oxygen advance along main channel to be mixed with catalyst, and is reacted at a certain temperature；Finally, after the reaction was completed, reaction product is taken out of by liquid phase carrier into collecting tank, gas phase is discharged after diluting in collecting tank or recycles into reaction system.It is dangerous high to solve the problems, such as that it is fired from the angle of essential safety, and improves reaction conversion ratio and selectivity by the design of micro-structure for realization of the direct synthesis from hydrogen and oxygen on microreactor in the present invention.
Description
Technical field
The present invention is to be related to the preparation technical field of hydrogen peroxide, and in particular to a kind of to be prepared using micro passage reaction
The method of hydrogen oxide.
Background technique
Hydrogen peroxide is a kind of common oxidants, since it does not generate the by-product of pollution environment, quilt during the reaction
A kind of clean chemical products of green are known as, the industries such as chemical industry, weaving, papermaking, food, medical treatment are had been widely used for.Mesh
The preceding industrial main stream approach of hydrogen peroxide is anthraquinone (production capacity, the production capacities of 98% or more the country of 95% or more foreign countries).
Its main flow are as follows: working solution is formed with the derivative of solvent appropriate dissolution anthraquinone first, uses hydrogen in the presence of a catalyst
It is hydrogen anthraquinone by anthraquinone reduction therein, the latter's autoxidation in the presence of oxygen or air at anthraquinone and generates hydrogen peroxide.
Aqueous hydrogen peroxide solution is separated to obtain with the hydrogen peroxide in water extraction solution, further refining and concentrating obtains the product of various concentration,
Extraction raffinate extracted returns to hydrogenation stage recycling after processing.Oxygen is not present in reaction process for anthraquinone technology maturation
It is relatively safer with the direct contact of hydrogen, however its process flow is more complicated, plant investment is big, big energy-consuming, used to have
Solvent system toxicity is big, and environmental pollution is serious.Since anthraquinone production technology is only in larger (40,000 tons of the annual output of production scale
More than) Shi Yingli, it needs to transport finished product to demand after centralized production, the safety wind of hydrogen peroxide during transportation
Danger and extra cost are also one of the defect of such production technology.
Hydrogen peroxide is produced by hydrogen and the direct chemical combination of oxygen, is a kind of ideal atom economy, environmentally protective production
Method.The method just receives the extensive concern of people after being proposed from 1914 by Henkel and Weber, however is limited to skill
Factor in terms of art, is not able to achieve industrialized production so far.Firstly, while hydrogen is oxidized to hydrogen peroxide, hydroxide
Symphysis Cheng Shui, hydrogen peroxide decompose and the side reactions such as hydrogen peroxide hydrogenation also can be with generation, and are favorable thermodynamics, instead
The selectivity answered is not high.Secondly as the explosion limit range of hydrogen is wide (4%-94% in oxygen, air in 4%-74%),
Technical process easily fires, and danger coefficient is big.Dupont company once attempted directly to synthesize peroxidating under 10% hydrogen atmosphere
Hydrogen, but because explosion accident takes place frequently, it has to close a set of pilot-plant.Such as peroxide is synthesized in the following concentration of hydrogen explosion lower limit
Change hydrogen, too low yield needs complicated separation and concentration step again, increases production cost, economically infeasible.
Microfluidic control technology refers in the low-dimensional channel design of micron or nanoscale, control volume be picoliters or nanoliter
Liquid flow and mass-and heat-transfer technology.The reaction scale of micro-fluid reactor is small, large specific surface area, and mass-and heat-transfer is fast
It is fast thoroughly accurately to control reaction process and condition, have application in chemical industry synthesis, field of biological detection, however about straight
It connects in terms of chemical combination method prepares hydrogen peroxide and but has not been reported.
Summary of the invention
The purpose of the present invention is to provide a kind of method for preparing hydrogen peroxide using micro passage reaction, hydrogen-oxygen is directly changed
It is dangerous high to solve the problems, such as that it is fired from the angle of essential safety, and passes through micro-structure for the legal realization on microreactor
Design improve reaction conversion ratio and selectivity.
Its technical solution includes:
A method of preparing hydrogen peroxide using micro passage reaction, the micro passage reaction include mixed zone,
Reaction zone and discharge zone, the mixed zone and reaction zone are realized on micro-channel chip, include several on the micro-channel chip
The microchannel of a array, the microchannel include the wing passage for gas feed and the main channel that passes through for liquid phase carrier,
The tail portion of the discharge zone is connected with collecting tank, the method successively the following steps are included:
A, unstripped gas hydrogen, oxygen are each led into the wing passage by gas source, is inputted in the main channel Xiang Suoshu
Liquid phase carrier, hydrogen and oxygen are mixed rapidly by diffusion；
B, the loading catalyst on the chip unit, mixed hydrogen, oxygen advance mixed with catalyst along main channel
It closes, and reacts at a certain temperature；
C, after the reaction was completed, reaction product is taken out of by liquid phase carrier into collecting tank, after gas phase dilutes in collecting tank
Discharge is recycled into reaction system.
As a preferred solution of the present invention, the first half for stating wing passage is bending section, and latter half is flat segments,
The bending section is for promoting unstripped gas to mix.
As another preferred embodiment of the invention, in step a, the gas source by unstripped gas pass sequentially through pressure reducing valve,
It is passed through in wing passage after gas flowmeter.
Preferably, in step b, catalyst is by cladding process or completion method load on micro-channel chip.
Preferably, in step b, the residence time of unstripped gas is controlled by the way that quencher is added into 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 to support in Al2O3、TiO2、ZrO2Or Pd, Au, Pt on absorbent charcoal carrier or
The noble metal of Ag or its alloy.
Advantageous effects brought by the present invention:
The present invention provides a kind of safety, green, easily synthesis hydrogen peroxide new method.Compared with prior art,
The present invention prepares hydrogen peroxide using micro passage reaction, since micro passage reaction size is small, large specific surface area, and reaction life
At free radical with tube wall it is continuous collision in be quenched, flame is difficult to propagate, though hydrogen-oxygen mixing after an explosion occurred, by
Inventory is few in being related to, the little energy for release of exploding, and damages caused by ambient enviroment and personnel also smaller, can greatly drop
The risk of low oxyhydroxide process.Therefore, the concentration of hydrogen and oxygen is no longer by explosion pole when reacting in micro passage reaction
The limitation of limit, directly enhances reaction speed, in turn avoids to improve density of hydrogen using condition of high voltage, is a kind of essence
The new technology of safe.Further, since microreactor unit is light and small portable, yield is flexibly adjustable, can be mounted directly reactor
To at demand, the risk of high-strength hydrogen peroxide during transportation is eliminated.
Realization of the 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 reaction conversion ratio and selectivity are improved by the design of micro-structure.
Detailed description of the invention
The present invention will be further described with reference to the accompanying drawing:
Fig. 1 is apparatus structure schematic diagram used by preparation method of the present invention；
Fig. 2 is to contact to form bubble schematic diagram with liquid phase carrier after gas phase premix on chip unit；
Fig. 3 be on chip unit gas phase contacted with liquid phase carrier to form bubble after the schematic diagram that mixes；
Fig. 4 is the structural schematic diagram of the main pipeline with surface micro-structure；
Fig. 5 is the part connection relationship 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, receipts
Collect tank, 6, quencher, 7, reaction zone in microchannel.
Specific embodiment
It is of the invention excellent in order to make the invention discloses a kind of method for preparing hydrogen peroxide using micro passage reaction
Point, technical solution are clearer, clear, elaborate combined with specific embodiments below to the present invention.
As shown in Figure 1, the preparation of hydrogen peroxide of the present invention is reacted in micro passage reaction 1, the knot of micro passage reaction
Structure is substantially similar with the prior art, is formed by stacking by several groups of chip units, has several logical on every group of chip unit
Road passes through in channel for unstripped gas and liquid phase carrier, is loaded with catalyst, hydrogen-oxygen in microchannel reaction zone 7 on chip unit
Direct combination reaction occurs herein.
There are hydrogen container 2, oxygen container 3 and collecting tank 5, hydrogen container, oxygen container difference with what micro passage reaction was used cooperatively
It is connected to the feeding-passage of micro passage reaction, pressure reducing valve and gas flowmeter is provided on the pipeline of connection, for monitoring
The flow of unstripped gas, collecting tank 5 are used to empty or be recycled to reaction system for the gas dilution in reaction product and utilize, this hair
Bright selection inert gas dilution.
The selection and loading method of catalyst: the direct chemical combination of hydrogen-oxygen generally uses Pd, Au, Pt or Ag catalyst, common to urge
Agent carrier is Al2O3、TiO2、ZrO2Or active carbon, the loading method that can be used are generally but are not limited to coating and fill out
Fill method；Coating applies in general to the microchannel of smaller internal diameter, by catalyst (and carrier) introduction passage in the form of suspension
It is interior, the catalyst coat of cladding channel inner surface is formed through processes such as drying and dehydratings；Completion method applies in general to larger interior diameter
Microchannel, be it is a kind of catalyst (and carrier) is supported on packaged type filler surface (such as bead), after by this filler
Fill the practice of full microchannel.
Chip unit: it is that hydrogen is mixed with the uniform of oxygen that chip, which needs the function of realizing, under carrier phase induced effect
Or pressure pushes the lower catalyst layer passed through in microchannel reaction zone 7, product finally flows out chip.When use liquid-carrier facies tract
When dynamic gas bubbles movement, hydrogen is contacted after being pre-mixed uniformly with oxygen with liquid, can also be same in certain channel node
When contact to form bubble with liquid.When being pushed directly on using pressure, hydrogen is directly contacted with catalyst with after oxygen mix.
Unstripped gas mixing:, should be in gas since the mixed proportion of hydrogen 2a and oxygen 3a directly affects the composition of product
Mixture is mixed uniformly before contacting with catalyst, and two kinds of gases can contact preceding premix with liquid phase carrier 4, such as Fig. 2 institute
Show, can also be in contact after forming bubble and mix with liquid-carrier simultaneously, as shown in Figure 3.The micro-structure that can use pipeline promotees
Air inlet body is flowed to reinforce mixed effect, and part bending section as shown in Figure 2,3, compared with flat segments, mixed effect is more preferable.
By the design and addition of micro-structure in main pipeline, the function such as mass transfer enhancement, accurate control residence time can be passed through
Energy.By designing rough surface or column structure in microchannel reaction zone 7, as shown in figure 4, increasing the catalyst that can be coated
Layer specific surface area, further increases reaction efficiency.By introducing quencher 6 and diluent in the fixed position of pipeline and accurately controlling
Flow velocity can accurately control the residence time and reaction time of material.
During flowing through catalyst, hydrogen-oxygen material reaction may not exclusively, and in the lower situation of conversion ratio, having must
Unreacted material is recycled, be recycled.Since the product of this reaction is liquid, easily divided with unreacted material
From, collection/separation list and collecting tank 5 are set after chip, carries out gas-liquid separation using gravity, isolated gaseous product through plus
Chip is reentered after pressure and participates in new round reaction, as shown in Figure 5.
The present invention provides a kind of device that hydrogen peroxide is prepared using hydrogen and the direct chemical combination of oxygen, which optionally goes back
Micro-mixer, reducer union, product collector unit etc. before reactor can be added.
Embodiment 1:
Gas source is hydrogen and oxygen gas cylinder in laboratory test, and gas is decompressed to 2MPa through pressure reducing valve, passes through quality
It is respectively 5sccm, 5sccm (or other ratios) that flowmeter, which controls flow, is entered by after reducer union by Teflon hose
Chip reaction member.Liquid-carrier is mutually the phosphoric acid of sodium bromide, sulfuric acid mixture liquid, sucks in 100mL syringe in advance, passes through note
It penetrates pump and is forced into chip reaction member, flow velocity 0.01mL/min.Gas phase and liquid phase are mixed near Reactor inlet,
Water is continuous phase, and bubble is dispersed phase, is reacted commonly through the channel for having supported catalyst.Reaction product enters collector
Two separation are carried out, system is discharged after dilution or reenters reaction system and is recycled for gas phase.
The direct chemical combination of hydrogen-oxygen prepares the catalyst of hydrogen peroxide based on Pd and Au at present, and catalyst carrier is mainly
Al2O3、TiO2、ZrO2Or active carbon, the research of the second metal active constituent of doping also have been obtained for centainly being in progress.It will catalysis
Agent supports there are mainly two types of the methods in reaction channel: cladding process and completion method.The former principle is by catalyst and carrier
For the suspension or colloidal sol (such as PMI method) of (Pd/C of such as 5%wt) at a slow speed by reaction channel, catalyst and carrier pass through physics
Effect is adsorbed on tube wall, through solvent seasoning (passing through gas flow purging or natural drying) after a period of time, forms cladding inner tube
One layer of catalyst layer of wall.The principle of the latter is that catalyst and carrier are coated on the outer of certain medium (such as bead) first
Side forms the three-dimensional filling space of catalyst then by this media filler in reaction channel.
Enter chip after pressure and flow are adjusted by the gas of electrolytic preparation or cylinder storage, under surface tension effects
Bubble is formed, advances along channel and is contacted with catalyst.Two kinds of gases can premix before entering chip, can on chip with liquid
Before being in contact premix as shown in Fig. 2, can also channel a certain position simultaneously be in contact to form bubble such as Fig. 3 with liquid-carrier
Shown, the relative concentration of two kinds of gas is determined by the relative velocity of the two, such as: when using Fig. 3 structure, such as hydrogen and oxygen stream
Amount is 5sccm, then is 1:1 in the ratio between the two molar concentration of reaction zone.
In flat tube, mixing of the gas in bubble relies primarily on diffusion and bubble and contacts initiation with tube wall
Bubble internal convection, when by pipeline from it is straight become bending when, the convection current direction of gas in bubble will be changed, promote gas mixed
It closes.Such as: crooked pipeline structure is added in flat tube section, main line width is 100 μm, and bending section width is constant, each bending
Angle is 90 °.Other numerical value can also be used in bending angle and width, as shown in Figure 2,3.
When one timing of flow velocity of liquid-carrier phase, the flow distance by controlling liquid can accurately control the stop of material
Time.As shown in figure 4, when pipeline diameter is 50 μm, bubble flows through distance with liquid when control flow rate of liquid is 0.01mL/min
Free radical quencher or diluent gas are introduced when 10mm in bubble, can control the reaction time is 118ms.
Although flame is not easy to propagate since wall effect causes free radical to be easy to be quenched in micro passage reaction, this
Requirement is proposed to channel size, when reactor size is more than certain threshold value, fires and still is possible to occur.Meanwhile for film
For reactor, although its isolating problem for thoroughly solving hydrogen and oxygen, reaction is only in the micropore for having supported catalyst
Occur on film, reaction efficiency is not high.If the two combined, membrane reactor is designed and sized to microreactor size, " film is logical
Oxygen stream is passed through inside road ", outside is passed through hydrogen stream, and reaction outside wall is still by general microreactor processing method, so that it may
The safety and efficiency of reaction are further increased with both comprehensive advantage.
It should be noted that those skilled in the art can also make such or such appearance under the introduction of this specification
Easy variation pattern, such as equivalent way or obvious mode of texturing, should all be within protection scope of the present invention.
Claims (2)
1. a kind of method for preparing hydrogen peroxide using micro passage reaction, it is characterised in that: the micro passage reaction packet
Mixed zone, reaction zone and discharge zone are included, the mixed zone and reaction zone are realized on micro-channel chip, on the micro-channel chip
Microchannel including several arrays, the microchannel include passing through for the wing passage of gas feed and for liquid phase carrier
The first half of main channel, the wing passage is bending section, and latter half is flat segments, and the bending section is for promoting unstripped gas
Mixing, the tail portion of the discharge zone is connected with collecting tank, gas feed and liquid phase carrier and is mixed in mixed zone, then passed through
Catalyst layer in reaction zone is reacted, and reaction product is flowed out through discharge zone, the method successively the following steps are included:
A, unstripped gas hydrogen, oxygen are each led into the wing passage by gas source, liquid phase is inputted in the main channel Xiang Suoshu
Carrier, hydrogen and oxygen are mixed rapidly by diffusion；
B, the loading catalyst on the micro-channel chip, mixed hydrogen, oxygen advance along main channel to be mixed with catalyst,
And it reacts at a certain temperature；
C, after the reaction was completed, reaction product is taken out of by liquid phase carrier into collecting tank, and gas phase is discharged after diluting in collecting tank
Or it is recycled into reaction system；
In step a, liquid phase carrier is water or acid solution；
In step b, catalyst is by cladding process or completion method load on micro-channel chip；By the way that quenching is added into main channel
Agent controls residence time of unstripped gas；Catalyst is to support in Al2O3、TiO2、ZrO2Or Pd, Au, Pt on absorbent charcoal carrier
Or the noble metal or its alloy of Ag.
2. the method according to claim 1 for preparing hydrogen peroxide using micro passage reaction, it is characterised in that: step a
In, the gas source is passed through in wing passage after unstripped gas is passed sequentially through pressure reducing valve, gas flowmeter.
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| 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 |
| US20210155476A1 (en) * | 2018-04-17 | 2021-05-27 | Electriq-Global Energy Solutions Ltd. | Batch systems and methods for hydrogen gas extraction from a liquid hydrogen carrier |
| CN108704589A (en) * | 2018-05-23 | 2018-10-26 | 西南民族大学 | Prepare the micro passage reaction of 2 cyano pyrazine |
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| 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 |
| CN109589890B (en) * | 2019-01-11 | 2021-02-26 | 北京机械设备研究所 | Hydrogen peroxide synthesis device and method |
| CN112499597A (en) * | 2019-09-14 | 2021-03-16 | 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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| AR057787A1 (en) * | 2005-08-31 | 2007-12-19 | Fmc Corp | PRODUCTION BY SELF-OXIDATION OF HYDROGEN PEROXIDE THROUGH HYDROGENATION IN A MICRORREACTOR |
| CN103539770B (en) * | 2013-10-08 | 2016-06-08 | 常州大学 | A kind of continuous reaction process method and microchannel reaction equipment preparing 6-caprolactone |
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| CN102186577A (en) * | 2008-10-15 | 2011-09-14 | 独立行政法人产业技术综合研究所 | Fixed bed mixed gas/liquid phase reactor and mixed gas/liquid phase reaction process using the same |
| CN102784542A (en) * | 2011-05-17 | 2012-11-21 | 中国科学院大连化学物理研究所 | Multi-channel micro reactor system for enhancing CO2 absorption, and method thereof |
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