CN104418308B - A kind of hydrogenation process of hydrogen dioxide solution production by anthraquinone process - Google Patents
A kind of hydrogenation process of hydrogen dioxide solution production by anthraquinone process Download PDFInfo
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- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/01—Hydrogen peroxide
- C01B15/022—Preparation from organic compounds
- C01B15/023—Preparation from organic compounds by the alkyl-anthraquinone process
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Abstract
The invention discloses the hydrogenation process of a kind of hydrogen dioxide solution production by anthraquinone process, including following content: the working solution of hydrogen dioxide solution production by anthraquinone process hydrogenation process and hydrogen-containing gas, along reactor, the share split of Flow of Goods and Materials direction introduces reactor, hydrogenation reaction is carried out at beds, per share working solution one hydrogen-containing gas corresponding, wherein hydrogen-containing gas is divided into 2 ~ 10 strands, and the number of share of stock of working solution is less than hydrogen-containing gas number of share of stock, and along Flow of Goods and Materials direction, most end stock material is hydrogen-containing gas。Present invention process can be prevented effectively from over-hydrogenation, improves hydrogen effect and extend catalyst service life。
Description
Technical field
The present invention relates to a kind of Hydrogen Peroxide Production technique, particularly to the hydrogenation process of a kind of hydrogen dioxide solution production by anthraquinone process。
Background technology
The industrialized production of current hydrogen peroxide mainly adopts anthraquinone, hydrogen dioxide solution production by anthraquinone process technique is usually with 2-ethyl-anthraquinone (EAQ) for working material, it is made into working solution for solvent with heavy aromatics (Ar) and trioctyl phosphate (TOP), through operations such as over hydrogenation, oxidation, extraction and working solution post processings, obtain hydrogen peroxide product。Wherein hydrogenation process refers to that the EAQ in working solution is under the existence of palladium catalyst, generates 2-ethyl hydrogen anthraquinone (HEAQ) with hydrogen generation hydrogenation reaction。
The uneven meeting of hydriding process makes anthraquinone generation excessive hydrogenation, produce degradation product, gathering of degradation product can make the viscosity of working solution, density and surface tension change, thus affecting the stable operation of follow-up extraction process, product quality, catalyst service life and device, anthraquinone consumption can be increased simultaneously, add production cost。In order to reduce excessive hydrogenation, the hydrogenation degree allowed in general anthraquinone hydrogenation process will lower than 50%, and domestic palladium catalyst to control below 40%, thus have impact on the production capacity of device。
Therefore the side reaction in the hydrogenation process of hydrogen dioxide solution production by anthraquinone process controls just to seem more important, it is ideally to improve hydrogenation degree, improve device capbility, anthraquinone will not be made again to occur because of excessive hydrogenation to degrade largely, keep good working solution level and catalyst service life。At present in the prior art mainly by controlling reaction condition, such as reaction temperature, reaction pressure and hydrogen flowing quantity, and the liquid distribution trough that serviceability is good, however the excessive hydrogenation phenomenon in Hydrogen Peroxide Production is controlled effectively not yet。
CN101229915A proposes the process of a kind of process for prepairng hydrogen peroxide by anthraquinone, the method is to pass into equipped with in the fixed bed reactors of palladium catalyst by working solution and hydrogen, working solution is continuous phase, utilize gas distributor that hydrogen is dispersed into minute bubbles and be distributed in working solution, to reach to control side reaction, minimizing over-hydrogenation phenomenon, improve the purpose that hydrogen is imitated。But being as the carrying out of reaction and the diffusion motion of gas, air pocket can be grown up gradually and be become continuous phase, also without fundamentally solving local excessive hydrogenation phenomenon。
Summary of the invention
For the deficiency of currently available technology, the present invention provides a kind of can be prevented effectively from over-hydrogenation, improve hydrogen effect, extend the hydrogenation process of the hydrogen dioxide solution production by anthraquinone process in catalyst service life。
The hydrogenation process of hydrogen dioxide solution production by anthraquinone process of the present invention, including following content: the working solution of hydrogen dioxide solution production by anthraquinone process hydrogenation process and hydrogen-containing gas, along reactor, the share split of Flow of Goods and Materials direction introduces reactor, hydrogenation reaction is carried out at beds, per share working solution one hydrogen-containing gas corresponding, wherein hydrogen-containing gas is divided into 2 ~ 10 strands, and the number of share of stock of working solution, less than hydrogen-containing gas number of share of stock, is hydrogen-containing gas along Flow of Goods and Materials direction most end stock material。
In present invention process, hydrogen-containing gas is the one in the mixture of pure hydrogen, hydrogen and nitrogen or the mixture of hydrogen and noble gas, and hydrogen volume fraction in the gas phase is 10% ~ 100%。
In present invention process, the volume flow (Nm of per share hydrogen-containing gas and total hydrogen-containing gas3/ h) than be 1:2～1:10。
In present invention process, the volume flow (Nm of per share working solution and total working liquid3/ h) than be 1:1～1:9。
In present invention process, the volume flow (Nm of per share working solution and per share hydrogen-containing gas3/ h) than be 1:1.5 ~ 1:15。
In present invention process, the quantity of catalyst reactor bed is 2 ~ 10, and is not less than the number of share of stock of hydrogen-containing gas。
In present invention process, the flow direction of material is along reactor from top to bottom or from bottom to top。
In present invention process, reaction mass is 1～3.5 minute in the time of staying of each beds。
In present invention process, the reaction temperature of hydrogenation process is 40～60 DEG C, and reaction pressure is 0.2～0.3MPa。
In present invention process, beds adopts the noble metal catalyst being active component with palladium or platinum。
In present invention process, it is preferable that working solution is divided into two strands, respectively working solution I and II, hydrogen-containing gas is divided into three strands, respectively hydrogen-containing gas I, II and III, and beds is 3, and wherein hydrogenation process is divided into following two situation:
(1) beds respectively the entering from the top of reactor of beds I, II and III, working solution I and hydrogen-containing gas I from top to bottom, carries out hydrogenation reaction at catalytic bed I, and reacted material enters the second beds；Working solution II and hydrogen-containing gas II, from entering reactor between beds I and beds II, carries out hydrogenation reaction with the reacted mixing of materials of catalyst layer I at beds II, and reacted material enters beds III；Hydrogen-containing gas III, from entering reactor between beds II and beds III, carries out hydrogenation reaction with the reacted mixing of materials of beds II at catalyst layer III, and final hydrogenated products flows out from reactor, enters subsequent processing；
(2) beds respectively the entering from the bottom of reactor of beds I, II and III, working solution I and hydrogen-containing gas I from the bottom to top, carries out hydrogenation reaction at catalytic bed I, and reacted material enters the second beds；Working solution II and hydrogen-containing gas II, from entering reactor between beds I and beds II, carries out hydrogenation reaction with the reacted mixing of materials of catalyst layer I at beds II, and reacted material enters beds III；Hydrogen-containing gas III, from entering reactor between beds II and beds III, carries out hydrogenation reaction with the reacted mixing of materials of beds II at catalyst layer III, and final hydrogenated products flows out from reactor head, enters subsequent processing。
Wherein, the volume flow (Nm of working solution I and hydrogen-containing gas I3/ h) than be 1:1.6～1:2.5；Volume flow (the Nm of working solution II and hydrogen-containing gas II3/ h) than be 1:3.5～1:10；Volume flow (the Nm of hydrogen-containing gas III and total hydrogen-containing gas3/ h) than be 1:2～1:5。
In present invention process, hydrogen-containing gas share split enters reactor, originally the hydrogenation process that a step completes is divided into a few step carry out, hydrogenation reaction is made to be initially located in the state of the few gas of a kind of many liquid, avoid anthraquinone excessive hydrogenation when the activity entering reactor is the highest in working solution, degrade, carrying out along with reaction, continue hydrogen make-up and fresh working solution, enable the anthraquinone in working solution that abundant hydrogenation to occur, reaction is finally introducing one hydrogen, ensure working solution hydrogenation completely, improve production efficiency, and excessive hydrogenation will not be there is, improve the selectivity of hydrogenation reaction, effectively suppress the generation of side reaction, improve the quality level of working solution, reduce expensive anthraquinone consumption, reduce production cost, be conducive to follow-up oxidation and extraction process。
Accompanying drawing explanation
Fig. 1 is the process flow diagram (working solution is two strands, and hydrogen-containing gas is three strands, by reactor head charging) of the present invention。
Fig. 2 is the process flow diagram (working solution is two strands, and hydrogen-containing gas is three strands, by reactor bottom charging) of the present invention。
Wherein, 1 is fixed bed hydrogenation reactor, and 2 is working solution I and hydrogen-containing gas I, and 3 is working solution II and hydrogen-containing gas II, and 4 is hydrogen-containing gas III, and 5 is hydride。
Detailed description of the invention
Illustrate with embodiment, this technological invention scheme to be described in detail below in conjunction with accompanying drawing, but be not so limited the present invention。
Present invention process is realized by such mode: working solution I and hydrogen-containing gas I2 enters from top or the bottom of fixed bed hydrogenation reactor 1, carries out hydrogenation reaction at catalytic bed I, and reacted material enters the second beds；Working solution II and hydrogen-containing gas II3, from entering reactor between beds I and beds II, carries out hydrogenation reaction with the reacted mixing of materials of catalyst layer I at beds II, and reacted material enters beds III；Hydrogen-containing gas III, from entering reactor between beds II and beds III, carries out hydrogenation reaction with the reacted mixing of materials of beds II at catalyst layer III, and hydride 5 flows out from reactor bottom or top, enters subsequent processing。
The embodiment of the present invention adopts anthraquinone to form working solution as working material, heavy aromatics and trioctyl phosphate as solvent, adopts Pd/Al2O3As anthraquinone hydrogenation catalyst, the character of catalyst is as follows: Ф 3～4mm's is spherical, and bulk density is 0.58 ± 0.02g/ml；Anti-crushing power >=40N/cm；Palladium content is 0.3 ± 0.02wt%；Activity kg (H2O2100%)/kg catalyst sky: >=3.3。In working solution, anthraquinone content is 72g/L, and tetrahydro-anthraquinone content is 41g/L。
Embodiment 1
Load three sections of catalyst in hydrogenation reactor, by upper under be followed successively by beds I, II and III, hydrogen is divided into hydrogen I, II and III three stock not to introduce reactor, and hydrogenation temperature is 42 DEG C, and hydrogenation pressure is 0.23Mpa。First all working solutions and hydrogen I autoreactor tops flow into reactor, there is the volume flow (Nm of hydrogenation reaction, hydrogen I and total hydrogen in beds I3/ h) than be 1:3.78, the material time of staying in beds I is 3.05 minutes；Volume flow (the Nm of hydrogen II and total hydrogen3/ h) than be 1:1.97, material residence time of material in beds II is 1.64 minutes；Hydrogen III and the volume ratio of total hydrogen that beds III introduces are 1:4.96, and the residence time of material in beds III is 1.5 minutes。Hydrogen anthraquinone and tetrahydrochysene hydrogen anthraquinone content respectively 28.8g/L and 16.3g/L after the processing of the method, hydrogen effect reaches 6.12g/L, and the consumption of anthraquinone is 0.38kg/T27.5%H2O2。
Embodiment 2
Three sections of catalyst are loaded in hydrogenation reactor, by upper under be followed successively by beds I, II and III, working solution is divided into working solution I and II two strands, hydrogen are divided into hydrogen I, II and III three strands to introduce reactor, hydrogenation temperature is 45 DEG C, hydrogenation pressure is 0.25Mpa。Working solution I and hydrogen I autoreactor top also flow into reactor, in beds I, hydrogenation reaction occur。Volume flow (the m of working solution I and total working liquid3/ h) than the volume flow (m for 1:1.24, hydrogen I Yu total hydrogen3/ h) than be 1:2.8, the residence time of material in beds I is 2.25 minutes；Volume flow (the m of working solution II and total working liquid3/ h) than being 1:5.21, the volume flow (m of hydrogen and total hydrogen in beds II3/ h) than be 1:2.69, the residence time of material in beds II is 1.85 minutes；Volume flow (the m of hydrogen III and total hydrogen3/ h) than be 1:3.70, the residence time of material of beds III is 1.5 minutes。Hydrogen anthraquinone tetrahydrochysene hydrogen anthraquinone content respectively 30.24g/L and 17.22g/L after the processing of the method, hydrogen effect reaches 6.44g/L, and the consumption of anthraquinone is 0.38kg/T27.5%H2O2。
Embodiment 3
Four sections of catalyst are loaded in hydrogenation reactor, by upper under be followed successively by beds I, II, III and IV, working solution is divided into working solution I, II and III three strands, hydrogen are divided into hydrogen I, II, III and IV four strands to introduce reactor, and hydrogenation temperature is 43 DEG C, and hydrogenation pressure is 0.2Mpa。Working solution I and hydrogen I autoreaction top also flow into reactor, in beds I, hydrogenation reaction occur。Volume flow (the m of working solution I and total working liquid3/ h) than the volume flow (Nm for 1:1.84, hydrogen I Yu total hydrogen3/ h) than be 1:4.66, the residence time of material in beds I is 1.94 minutes；Volume flow (the m of working solution II and total working liquid3/ h) than the volume flow (Nm for 1:4.38, hydrogen II Yu total hydrogen3/ h) than be 1:5.7, the residence time of material in the second bed is 1.7 minutes；Volume flow (the m of working solution III and total working liquid3/ h) than the volume flow (Nm for 1:4.38, hydrogen III Yu total hydrogen3/ h) than be 1:5.7, the residence time of material in beds III is 1.57 minutes；Volume flow (the Nm of hydrogen IV and total hydrogen3/ h) than be 1:4.09；Residence time of material in beds IV is 1.5 minutes。
After the processing of the method hydrogen anthraquinone, tetrahydrochysene hydrogen anthraquinone content respectively 33.7g/L and 15.9g/L, hydrogen effect reach 6.82g/L, the consumption of anthraquinone is 0.36kg/T27.5%H2O2。
Comparative example 1
Three sections of catalyst are loaded in hydrogenation reactor, hydrogenation temperature is 48 DEG C, and hydrogenation pressure is 0.25Mpa, and whole working solutions and hydrogen autoreactor top also flow into reactor, sequentially passing through first, second, and third bed generation hydrogenation reaction, residence time of material is 5.6 minutes。After the processing of the method, hydrogen anthraquinone and tetrahydrochysene hydrogen anthraquinone content respectively 26.7g/L and 15g/L, hydrogen effect is 5.66g/L, and the consumption of anthraquinone is 0.47kg/T27.5%H2O2。
Claims (15)
1. the hydrogenation process of a hydrogen dioxide solution production by anthraquinone process, it is characterized in that including following content: the working solution of hydrogen dioxide solution production by anthraquinone process hydrogenation process and hydrogen-containing gas, along reactor, the share split of Flow of Goods and Materials direction introduces reactor, hydrogenation reaction is carried out at beds, per share working solution one hydrogen-containing gas corresponding, wherein hydrogen-containing gas is divided into 2 ~ 10 strands, and the number of share of stock of working solution is less than hydrogen-containing gas number of share of stock, and along Flow of Goods and Materials direction, most end stock material is hydrogen-containing gas。
2. technique according to claim 1, it is characterised in that: hydrogen-containing gas is the one in the mixture of pure hydrogen, hydrogen and nitrogen or the mixture of hydrogen and noble gas, and hydrogen volume fraction in the gas phase is 10% ~ 100%。
3. technique according to claim 1, it is characterised in that: the volume flow ratio of per share hydrogen-containing gas and total hydrogen-containing gas is 1:2～1:10, and wherein volume flow unit is Nm3/h。
4. technique according to claim 1, it is characterised in that: the volume flow ratio of per share working solution and total working liquid is 1:1～1:9, and wherein volume flow unit is m3/h。
5. technique according to claim 1, it is characterised in that: the volume flow ratio of per share working solution and corresponding per share hydrogen-containing gas is 1:1.5 ~ 1:15, and wherein volume flow unit is Nm3/h。
6. technique according to claim 1, it is characterised in that: the quantity of catalyst reactor bed is 2 ~ 10, and no less than the number of share of stock of hydrogen-containing gas。
7. technique according to claim 1, it is characterised in that: the flow direction of material is along reactor from top to bottom or from bottom to top。
8. the technique according to claim 1 or 6, it is characterised in that: reaction mass is 1～3.5 minute in the time of staying of each beds。
9. technique according to claim 1, it is characterised in that: the reaction temperature of hydrogenation process is 40～60 DEG C, and reaction pressure is 0.2～0.3MPa。
10. technique according to claim 1, it is characterised in that: beds adopts the noble metal catalyst being active component with palladium or platinum。
11. technique according to claim 1, it is characterised in that: working solution is divided into two strands, respectively working solution I and II, hydrogen-containing gas is divided into three strands, respectively hydrogen-containing gas I, II and III, beds is 3, from top to bottom respectively beds I, II and III；Wherein hydrogenation process is as follows: working solution I and hydrogen-containing gas I enters from the top of reactor, carries out hydrogenation reaction at catalytic bed I, and reacted material enters the second beds；Working solution II and hydrogen-containing gas II, from entering reactor between beds I and beds II, carries out hydrogenation reaction with the reacted mixing of materials of catalyst layer I at beds II, and reacted material enters beds III；Hydrogen-containing gas III, from entering reactor between beds II and beds III, carries out hydrogenation reaction with the reacted mixing of materials of beds II at catalyst layer III, and final hydrogenated products flows out from reactor bottom, enters subsequent processing。
12. technique according to claim 1, it is characterised in that: working solution is divided into two strands, respectively working solution I and II, hydrogen-containing gas is divided into three strands, respectively hydrogen-containing gas I, II and III, beds is 3, from the bottom to top respectively beds I, II and III；Wherein hydrogenation process is as follows: working solution I and hydrogen-containing gas I enters from the bottom of reactor, carries out hydrogenation reaction at catalytic bed I, and reacted material enters the second beds；Working solution II and hydrogen-containing gas II, from entering reactor between beds I and beds II, carries out hydrogenation reaction with the reacted mixing of materials of catalyst layer I at beds II, and reacted material enters beds III；Hydrogen-containing gas III, from entering reactor between beds II and beds III, carries out hydrogenation reaction with the reacted mixing of materials of beds II at catalyst layer III, and final hydrogenated products flows out from reactor head, enters subsequent processing。
13. the technique according to claim 11 or 12, it is characterised in that: the volume flow ratio of working solution I and hydrogen-containing gas I is 1:1.6～1:2.5。
14. the technique according to claim 11 or 12, it is characterised in that: the volume flow ratio of working solution II and hydrogen-containing gas II is 1:3.5～1:10, and wherein volume flow unit is Nm3/h。
15. the technique according to claim 11 or 12, it is characterised in that: the volume flow ratio of hydrogen-containing gas III and total hydrogen-containing gas is 1:2～1:5, and wherein volume flow unit is Nm3/h。
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| CN106542502B (en) * | 2015-09-17 | 2018-07-31 | 中国石油化工股份有限公司 | Cycle working fluid regeneration method and a kind of method producing hydrogen peroxide in a kind of process for prepairng hydrogen peroxide by anthraquinone technique |
| CN106892408B (en) * | 2015-12-18 | 2019-03-19 | 中国石油化工股份有限公司 | A kind of method for oxidation of hydrogen peroxide production process |
| CN109911860B (en) * | 2019-04-26 | 2021-05-25 | 北京凯迪森科技有限公司 | Method for producing hydrogen peroxide hydrogenation fixed bed layer gas-liquid distribution by using intensified anthraquinone method |
| CN115247077B (en) * | 2021-04-26 | 2023-11-03 | 中国石油化工股份有限公司 | Gasoline hydrodesulfurization method |
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