CN102009960A - Hydrogenation method for production of hydrogen peroxide by anthraquinone process - Google Patents
Hydrogenation method for production of hydrogen peroxide by anthraquinone process Download PDFInfo
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Abstract
The invention discloses a hydrogenation method for production of hydrogen peroxide by the anthraquinone process, belonging to the technical field of chemical industry reaction. The method provided by the invention comprises: dispersing the gaseous phase containing hydrogen into the working solution containing the anthraquinone derivatives to obtain the gas-liquid mixing fluid containing micron bubbles, so that the gas-liquid mixing fluid passes through the pipe reactor filled with the hydrogenation catalyst at the space velocity of 3 to 1000h<-1> to finish the hydrogenation process. In the method provided by the invention, the gas-liquid micro-dispersing process and the static bed catalytic hydrogenation process are directly integrated, so that the interphase mass transfer is strengthened, and the contacts between different reactants and between the reactant and the catalyst are more sufficient and more uniform, thereby enhancing the efficiency and the controllability of the hydrogenation process and improving the economical efficiency and the security of the production of the hydrogen peroxide.
Description
Technical field
The invention belongs to the chemical reaction technical field, be specifically related to a kind of method of hydrotreating of process for prepairng hydrogen peroxide by anthraquinone.
Background technology
Hydrogen peroxide is a kind of important industrial raw material; can be widely used in the industries such as chemosynthesis, environment protection, papermaking, weaving, national defense and military, electronics, medicine, food and agricultural, as oxygenant, SYNTHETIC OPTICAL WHITNER, sterilizing agent, polymerization initiator and linking agent, propelling agent etc.Anthraquinone is the main method of current industrial production hydrogen peroxide, and the hydrogen peroxide more than 98% is to adopt this method to produce in the world at present.The shortening process that contains the anthraquinone derivative working fluid is the important step in anthraquinone.This process all has great effect to the economy and the security of process for prepairng hydrogen peroxide by anthraquinone.
At present, industrial method of hydrotreating commonly used be activated alumina particle with supported palladium as catalyzer, working fluid and hydrogen fed simultaneously trickle-bed reactor, fluidized-bed reactor or the paste state bed reactor of loading catalyst realize.The problem that this method exists is that the contact efficiency of gas phase in the reactor, liquid phase and solid phase is low, and the shortening process efficiency is low, and material needs to stop the long period in equipment, causes equipment volume big, and selectivity is low.So, develop the hydrogenation novel method of efficient process for prepairng hydrogen peroxide by anthraquinone, have important economic technology and be worth.
Summary of the invention
The method of hydrotreating that the purpose of this invention is to provide a kind of process for prepairng hydrogen peroxide by anthraquinone, this method directly integrates diffusing technology of gas-liquid differential and fixed-bed catalytic hydrogenation process, strengthened interphase mass transfer and make between the differential responses thing, contacting more fully and evenly between reactant and catalyzer, the efficient and the controllability of hydrogenation process be can improve, the economy and the security of hydrogen peroxide manufacture improved.
A kind of method of hydrotreating of process for prepairng hydrogen peroxide by anthraquinone is characterized in that, carries out as follows:
(a) at first under 30～80 ℃ of temperature and 0～1MPa pressure (gauge pressure) with the gas phase dispersion of hydrogen in the working fluid that contains anthraquinone derivative, obtain containing the solution-air mixed stream of micro-bubble;
Secondly (b) under 30～80 ℃ of temperature and 0～1MPa pressure (gauge pressure), with the solution-air mixed stream with 3～1000h
-1Air speed flow through the tubular reactor of filling hydrogenation catalyst gained, hydrogenation reaction is carried out in reactor, obtains reacted solution-air mixed stream;
(c) at last reacted solution-air mixed stream is obtained liquid product hydrogenation working fluid through the solution-air separation.
The gas phase of hydrogen is the mixture of pure hydrogen or hydrogen and rare gas element in the described step (a), and rare gas element comprises nitrogen, helium, and the volume fraction of hydrogen in gas phase is 1%～100%.
Contain the anthraquinone derivatives working fluid in the described step (a), solute is an anthraquinone derivatives, mainly is 2-alkyl-anthraquinone and tetrahydrochysene 2-alkyl-anthraquinone, as 2-ethyl-anthraquinone, tetrahydrochysene 2-ethyl-anthraquinone.
Contain in the anthraquinone derivative working fluid in the described step (a), solvent is the mixture of anthraquinone solvent and hydrogen anthraquinone solvent, and the anthraquinone solvent is C
9～C
11High boiling point BTX aromatics or methylnaphthalene, hydrogen anthraquinone solvent is trioctyl phosphate or diisobutyl carbinol(DIBC).
Contain in the working fluid of anthraquinone derivative in the described step (a), the concentration of anthraquinone derivatives is 0.01mol/L～1mol/L.
Dispersion process comprises the dispersed with stirring process and is the dispersion process of dispersion medium with microporous membrane, micropore sieve plate, micron order passage in the described step (a).
The mean diameter of micro-bubble is 10～1000 microns in the described step (a).
Hydrogenation catalyst is nickel carried catalyst or palladium carried catalyst in the described step (b).
Beneficial effect of the present invention:
The present invention with the gas phase dispersion of hydrogen in containing the working fluid of anthraquinone derivative, the dispersion state of gas phase is the bubble of micron order size, compare with millimeter or centimetre-sized bubbles dispersion state in traditional gas-liquid mass transferring equipment, the mass transfer specific surface area can improve 100～1000 times, and gas phase and liquid phase have the more distribution of homogeneous respectively simultaneously; When the solution-air mixed stream with micron order bubble dispersion state contacted with hydrogenation catalyst, high specific surface area can provide big and contact area catalyzer, helps carrying out fast of shortening process; The distribution of gas phase and liquid phase homogeneous helps avoiding carrying out thereby help the controlled of shortening process because the local excessive hydrogenation that gas phase and liquid phase skewness one cause causes the appearance of the phenomenon of selectivity reduction.
Method provided by the present invention, in its hydrogenation process, gas-liquid-solid three-phase contact area is big, and the reaction times is short, can reduce equipment volume, and reduces the needed catalyst levels of unit volume hydrogenation products; Being evenly distributed of gas phase and liquid phase adjusted the reaction times according to dispersing mode and operational condition, and promptly the hydrogenation degree of may command anthraquinone and derivative thereof is avoided local hydrogenation, improves the selectivity of reaction process.
Embodiment
The invention will be further described below in conjunction with embodiment:
Embodiment 1:
At first, trimethylbenzene and trioctyl phosphate mixed preparing solution between inciting somebody to action, wherein, the trioctyl phosphate volume fraction is 25%, obtains solvent, with 2-ethyl-anthraquinone as solute and solvent, obtain solution obtains working fluid, and wherein 2-ethyl-anthraquinone concentration is 0.01mol/L.In temperature is 30 ℃, pressure is under the condition of 500kPa (gauge pressure), making total amount is that the mixed gas of the hydrogen of 0.01mol and nitrogen is that dispersion medium feeds in the working fluid of 40mL with the microporous membrane, is 10 microns solution-air mixed stream to bubble mean diameter, and wherein the volume fraction of hydrogen is 80%.Then, be 30 ℃ in temperature, pressure is under the condition of 500kPa (gauge pressure), makes the solution-air mixed stream with 400h
-1Air speed flow through palladium-α-Al
2O
3Fill the tubular reactor of gained, obtain reacted solution-air mixed stream.At last, in the solution-air neutral section, reacted solution-air mixed stream is separated, obtain liquid product hydrogenation working fluid.
The total concn of hydrogenation products can reach 0.005mol/L.
Embodiment 2:
At first, with hemimellitol and trioctyl phosphate mixed preparing solution, wherein, the trioctyl phosphate volume fraction is 30%, obtains solvent, with the tetrahydrochysene 2-ethyl-anthraquinone as solute and solvent, obtain solution obtains working fluid, and wherein tetrahydrochysene 2-ethyl-anthraquinone concentration is 0.1mol/L.In temperature is 40 ℃, pressure is under the condition of 500kPa (gauge pressure), making total amount is that the hydrogen of 0.02mol and the mixed gas of nitrogen are that dispersion medium feeds in the working fluid of 20mL with the microporous membrane, to bubble mean diameter is 100 microns solution-air mixed stream, and wherein the volume fraction of hydrogen is 75%.Then, be 40 ℃ in temperature, pressure is under the condition of 500kPa (gauge pressure), makes the solution-air mixed stream with 500h
-1Air speed flow through palladium-α-Al
2O
3Fill the tubular reactor of gained, obtain reacted solution-air mixed stream.At last, in the solution-air neutral section, reacted solution-air mixed stream is separated, obtain liquid product hydrogenation working fluid.
The total concn of hydrogenation products can reach 0.04mol/L.
Embodiment 3:
At first, will be to trimethylbenzene and diisobutyl carbinol(DIBC) mixed preparing solution, wherein, the diisobutyl carbinol(DIBC) volume fraction is 27%, obtains solvent, with 2-ethyl-anthraquinone and tetrahydrochysene 2-ethyl-anthraquinone as solute and solvent, obtain solution, obtain working fluid, wherein 2-ethyl-anthraquinone concentration is 0.2mol/L, and tetrahydrochysene 2-ethyl-anthraquinone concentration is 0.1mol/L.In temperature is 50 ℃, pressure is under the condition of 0 (gauge pressure), making total amount is that the mixed gas of the hydrogen of 0.05mol and nitrogen is that dispersion medium feeds in the working fluid of 100mL with the micropore sieve plate, is 200 microns solution-air mixed stream to bubble mean diameter, and wherein the volume fraction of hydrogen is 60%.Then, be 50 ℃ in temperature, pressure is under the condition of 0 (gauge pressure), makes the solution-air mixed stream with 700h
-1Air speed flow through palladium-α-Al
2O
3Fill the tubular reactor of gained, obtain reacted solution-air mixed stream.At last, in the solution-air neutral section, reacted solution-air mixed stream is separated, obtain liquid product hydrogenation working fluid.The total concn of hydrogenation products can reach 0.16mol/L.
Embodiment 4:
At first, with methylnaphthalene and diisobutyl carbinol(DIBC) mixed preparing solution, wherein, the diisobutyl carbinol(DIBC) volume fraction is 31%, obtains solvent, with 2-ethyl-anthraquinone as solute and solvent, obtain solution obtains working fluid, and wherein 2-ethyl-anthraquinone concentration is 0.3mol/L.In temperature is 40 ℃, pressure is under the condition of 600kPa (gauge pressure), making total amount is that the hydrogen of 0.05mol and the mixed gas of nitrogen are that dispersion medium feeds in the working fluid of 10mL with the micron order passage, to bubble mean diameter is 1000 microns solution-air mixed stream, and wherein the volume fraction of hydrogen is 10%.Then, be 40 ℃ in temperature, pressure is under the condition of 600kPa (gauge pressure), makes the solution-air mixed stream with 1000h
-1Air speed flow through palladium-α-Al
2O
3Fill the tubular reactor of gained, obtain reacted solution-air mixed stream.At last, in the solution-air neutral section, reacted solution-air mixed stream is separated, obtain liquid product hydrogenation working fluid.
The total concn of hydrogenation products can reach 0.12mol/L.
Embodiment 5:
At first, trimethylbenzene and diisobutyl carbinol(DIBC) mixed preparing solution between inciting somebody to action, wherein, the diisobutyl carbinol(DIBC) volume fraction is 29%, obtains solvent, with the tetrahydrochysene 2-ethyl-anthraquinone as solute and solvent, obtain solution obtains working fluid, and wherein tetrahydrochysene 2-ethyl-anthraquinone concentration is 0.4mol/L.In temperature is 80 ℃, pressure is under the condition of 1MPa (gauge pressure), making total amount is that the mixed gas of the hydrogen of 10mol and nitrogen is that dispersion medium feeds in the working fluid of 50mL with the microporous membrane, is 800 microns solution-air mixed stream to bubble mean diameter, and wherein the volume fraction of hydrogen is 1%.Then, be 80 ℃ in temperature, pressure is under the condition of 1MPa (gauge pressure), makes the solution-air mixed stream with 600h
-1Air speed flow through palladium-α-Al
2O
3Fill the tubular reactor of gained, obtain reacted solution-air mixed stream.At last, in the solution-air neutral section, reacted solution-air mixed stream is separated, obtain liquid product hydrogenation working fluid.
The total concn of hydrogenation products can reach 0.11mol/L.
Embodiment 6:
At first, with hemimellitol and diisobutyl carbinol(DIBC) mixed preparing solution, wherein, the diisobutyl carbinol(DIBC) volume fraction is 32%, obtains solvent, with 2-ethyl-anthraquinone and tetrahydrochysene 2-ethyl-anthraquinone as solute and solvent, obtain solution, obtain working fluid, wherein 2-ethyl-anthraquinone concentration is 0.1mol/L, and tetrahydrochysene 2-ethyl-anthraquinone concentration is 0.4mol/L.In temperature is 40 ℃, and pressure is under the condition of 300kPa (gauge pressure), make total amount be the hydrogen of 0.02mol by dispersed with stirring in the working fluid of 40mL, be 1000 microns solution-air mixed stream to bubble mean diameter.Then, be 40 ℃ in temperature, pressure is under the condition of 300kPa (gauge pressure), makes the solution-air mixed stream with 300h
-1Air speed flow through palladium-α-Al
2O
3Fill the tubular reactor of gained, obtain reacted solution-air mixed stream.At last, in the solution-air neutral section, reacted solution-air mixed stream is separated, obtain liquid product hydrogenation working fluid.
The total concn of hydrogenation products can reach 0.12mol/L.
Embodiment 7:
At first, will be to trimethylbenzene and diisobutyl carbinol(DIBC) mixed preparing solution, wherein, the diisobutyl carbinol(DIBC) volume fraction is 30%, obtains solvent, with 2-ethyl-anthraquinone and tetrahydrochysene 2-ethyl-anthraquinone as solute and solvent, obtain solution, obtain working fluid, wherein 2-ethyl-anthraquinone concentration is 0.5mol/L, and tetrahydrochysene 2-ethyl-anthraquinone concentration is 0.5mol/L.In temperature is 80 ℃, pressure is under the condition of 1MPa (gauge pressure), making total amount is that the mixed gas of the hydrogen of 0.07mol and helium is that dispersion medium feeds in the working fluid of 50mL with the microporous membrane, is 120 microns solution-air mixed stream to bubble mean diameter, and wherein the volume fraction of hydrogen is 75%.Then, be 80 ℃ in temperature, pressure is under the condition of 1MPa (gauge pressure), makes the solution-air mixed stream with 1000h
-1Air speed flow through palladium-α-Al
2O
3Fill the tubular reactor of gained, obtain reacted solution-air mixed stream.At last, in the solution-air neutral section, reacted solution-air mixed stream is separated, obtain liquid product hydrogenation working fluid.
The total concn of hydrogenation products can reach 0.6mol/L.
Embodiment 8:
At first, trimethylbenzene and trioctyl phosphate mixed preparing solution between inciting somebody to action, wherein, the trioctyl phosphate volume fraction is 22%, obtains solvent, with 2-ethyl-anthraquinone and tetrahydrochysene 2-ethyl-anthraquinone as solute and solvent, obtain solution, obtain working fluid, wherein 2-ethyl-anthraquinone concentration is 0.3mol/L, and tetrahydrochysene 2-ethyl-anthraquinone concentration is 0.3mol/L.In temperature is 50 ℃, pressure is under the condition of 200kPa (gauge pressure), making total amount is that the hydrogen of 0.3mol and the mixed gas of argon gas are that dispersion medium feeds in the working fluid of 200mL with the microporous membrane, to bubble mean diameter is 130 microns solution-air mixed stream, and wherein the volume fraction of hydrogen is 40%.Then, be 50 ℃ in temperature, pressure is under the condition of 200kPa (gauge pressure), makes the solution-air mixed stream with 3h
-1Air speed flow through the tubular reactor that nickel foam is filled gained, obtain reacted solution-air mixed stream.At last, in the solution-air neutral section, reacted solution-air mixed stream is separated, obtain liquid product hydrogenation working fluid.
The total concn of hydrogenation products can reach 0.1mol/L.
Although illustrated and described embodiments of the invention, for the ordinary skill in the art, be appreciated that without departing from the principles and spirit of the present invention and can carry out multiple variation, modification, replacement and modification to these embodiment, scope of the present invention is limited by claims and equivalent thereof.
Claims (8)
1. the method for hydrotreating of a process for prepairng hydrogen peroxide by anthraquinone is characterized in that, carries out as follows:
(a) at first under 30～80 ℃ of temperature and 0～1MPa pressure (gauge pressure), the gas phase dispersion of hydrogen in the working fluid that contains anthraquinone derivative, is obtained containing the solution-air mixed stream of micro-bubble;
Secondly (b) under 30～80 ℃ of temperature and 0～1MPa pressure (gauge pressure), with the solution-air mixed stream with 3～1000h
-1Air speed flow through the tubular reactor of filling hydrogenation catalyst gained, hydrogenation reaction is carried out in reactor, obtains reacted solution-air mixed stream;
(c) at last reacted solution-air mixed flow is obtained liquid product hydrogenation working fluid through the solution-air separation.
2. the method for hydrotreating of a kind of process for prepairng hydrogen peroxide by anthraquinone according to claim 1, it is characterized in that: the gas phase of hydrogen is the mixture of pure hydrogen or hydrogen and rare gas element described in the step (a), rare gas element comprises nitrogen, helium, and the volume fraction of hydrogen in gas phase is 1%～100%.
3. the method for hydrotreating of a kind of process for prepairng hydrogen peroxide by anthraquinone according to claim 1, it is characterized in that: the described anthraquinone derivatives working fluid that contains of step (a), solute is an anthraquinone derivatives, mainly be 2-alkyl-anthraquinone and tetrahydrochysene 2-alkyl-anthraquinone, as 2-ethyl-anthraquinone, tetrahydrochysene 2-ethyl-anthraquinone.
4. the method for hydrotreating of a kind of process for prepairng hydrogen peroxide by anthraquinone according to claim 1, it is characterized in that: contain in the anthraquinone derivative working fluid described in the step (a), solvent is the mixture of anthraquinone solvent and hydrogen anthraquinone solvent, and the anthraquinone solvent is C
9～C
11High boiling point BTX aromatics or methylnaphthalene, hydrogen anthraquinone solvent is trioctyl phosphate or diisobutyl carbinol(DIBC).
5. the method for hydrotreating of a kind of process for prepairng hydrogen peroxide by anthraquinone according to claim 1, it is characterized in that: contain in the anthraquinone derivative working fluid described in the step (a), the concentration of anthraquinone derivatives is 0.01mol/L～1mol/L.
6. the method for hydrotreating of a kind of process for prepairng hydrogen peroxide by anthraquinone according to claim 1 is characterized in that: the dispersion process described in the step (a) comprises the dispersed with stirring process and is the dispersion process of dispersion medium with microporous membrane, micropore sieve plate, micron order passage.
7. the method for hydrotreating of a kind of process for prepairng hydrogen peroxide by anthraquinone according to claim 1, it is characterized in that: the mean diameter of micro-bubble is 10～1000 microns described in the step (a).
8. the method for hydrotreating of a kind of process for prepairng hydrogen peroxide by anthraquinone according to claim 1, it is characterized in that: the hydrogenation catalyst described in the step (b) is nickel carried catalyst or palladium carried catalyst.
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