CN104418308A - Hydrogenation technology for producing hydrogen peroxide by anthraquinone process - Google Patents
Hydrogenation technology for producing hydrogen peroxide by anthraquinone process Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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 a hydrogenation technology for producing hydrogen peroxide by an anthraquinone process, which comprises the following steps: operating fluid and hydrogen-containing gas in the hydrogenation technology for producing hydrogen peroxide by the anthraquinone process are introduced in a reactor along flowing direction of materials in the reactor, a hydrogenation reaction is carried out on a bed layer of a catalyst, each strand of operating fluid corresponds a strand of hydrogen-containing gas, wherein hydrogen-containing gas is divided into 2-10 strands, the strand number of operating fluid is less than that of the hydrogen-containing gas, The last strand of the material long the flowing direction of the material is the hydrogen-containing gas. The technology can effectively avoid the excessive hydrogenation, increase hydrogen effect and prolong the usage life of the catalyst.
Description
Technical field
The present invention relates to a kind of Hydrogen Peroxide Production technique, particularly a kind of hydrogenation process of hydrogen dioxide solution production by anthraquinone process.
Background technology
The suitability for industrialized production of current hydrogen peroxide mainly adopts anthraquinone, hydrogen dioxide solution production by anthraquinone process technique is generally for working material with 2-ethyl-anthraquinone (EAQ), with heavy aromatics (Ar) and trioctyl phosphate (TOP) for solvent is made into working fluid, through operations such as over hydrogenation, oxidation, extraction and working fluid aftertreatments, obtain hydrogen peroxide product.Wherein hydrogenation process refers to that the EAQ in working fluid 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 fluid, density and surface tension change, thus affect the steady running of follow-up extraction process, quality product, catalyzer work-ing 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 will control below 40%, so just have impact on the production capacity of device.
Side reaction in the hydrogenation process of therefore hydrogen dioxide solution production by anthraquinone process controls just to seem more important, ideally to improve hydrogenation degree, improve device capbility, anthraquinone can not be made again to occur because of excessive hydrogenation to degrade largely, keep good working solution level and catalyzer work-ing life.At present in the prior art mainly by controlling reaction conditions, as temperature of reaction, reaction pressure and hydrogen flowing quantity, and the liquid distributor that use properties is good, the excessive hydrogenation phenomenon however in Hydrogen Peroxide Production is controlled effectively not yet.
CN101229915A proposes a kind of processing method of process for prepairng hydrogen peroxide by anthraquinone, the method working fluid and hydrogen is passed into be equipped with in the fixed-bed reactor of palladium catalyst, working fluid is external phase, utilizing gas distributor hydrogen to be dispersed into small bubbles is distributed in working fluid, to reach the object controlling side reaction, reduce over-hydrogenation phenomenon, improve hydrogen effect.But along with the carrying out of reaction and the diffusion motion of gas, air pocket can be grown up gradually and become external phase, fundamentally do not solve local excessive hydrogenation phenomenon equally.
Summary of the invention
For the deficiency of currently available technology, the invention provides a kind of hydrogenation process effectively can avoided over-hydrogenation, improve hydrogen effect, the hydrogen dioxide solution production by anthraquinone process in extending catalyst work-ing life.
The hydrogenation process of hydrogen dioxide solution production by anthraquinone process of the present invention, comprise following content: the working fluid of hydrogen dioxide solution production by anthraquinone process hydrogenation process and hydrogen-containing gas, reactor is introduced along Flow of Goods and Materials direction share split in reactor, hydrogenation reaction is carried out at beds, per share working fluid one hydrogen-containing gas corresponding, wherein hydrogen-containing gas is divided into 2 ~ 10 strands, and the number of share of stock of working fluid is 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 rare gas element, and hydrogen volume fraction is in the gas phase 10% ~ 100%.
In present invention process, the volumetric flow rate (Nm of per share hydrogen-containing gas and total hydrogen-containing gas
3/ h) than being 1:2 ~ 1:10.
In present invention process, the volumetric flow rate (Nm of per share working fluid and total working liquid
3/ h) than being 1:1 ~ 1:9.
In present invention process, the volumetric flow rate (Nm of per share working fluid and per share hydrogen-containing gas
3/ h) than being 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 residence time of each beds.
In present invention process, the temperature of reaction of hydrogenation process is 40 ~ 60 DEG C, and reaction pressure is 0.2 ~ 0.3MPa.
In present invention process, the noble metal catalyst that to adopt with palladium or platinum in beds be active ingredient.
In present invention process, preferred working fluid is divided into two strands, is respectively working fluid I and II, and hydrogen-containing gas is divided into three strands, is respectively hydrogen-containing gas I, II and III, and beds is 3, and wherein hydrogenation process is divided into following two kinds of situations:
(1) beds is respectively beds I, II and III from top to bottom, and working fluid 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 fluid II and hydrogen-containing gas II enters reactor between beds I and beds II, and carry out hydrogenation reaction with the reacted mixing of materials of catalyst layer I at beds II, reacted material enters beds III; Hydrogen-containing gas III enters reactor between beds II and beds III, and carry out hydrogenation reaction with the reacted mixing of materials of beds II at catalyst layer III, final hydrogenated products flows out from reactor, enters subsequent processing;
(2) beds is respectively beds I, II and III from the bottom to top, and working fluid 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 fluid II and hydrogen-containing gas II enters reactor between beds I and beds II, and carry out hydrogenation reaction with the reacted mixing of materials of catalyst layer I at beds II, reacted material enters beds III; Hydrogen-containing gas III enters reactor between beds II and beds III, and carry out hydrogenation reaction with the reacted mixing of materials of beds II at catalyst layer III, final hydrogenated products flows out from reactor head, enters subsequent processing.
Wherein, the volumetric flow rate (Nm of working fluid I and hydrogen-containing gas I
3/ h) than being 1:1.6 ~ 1:2.5; Volumetric flow rate (the Nm of working fluid II and hydrogen-containing gas II
3/ h) than being 1:3.5 ~ 1:10; Volumetric flow rate (the Nm of hydrogen-containing gas III and total hydrogen-containing gas
3/ h) than being 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 a kind of state of many liquid weak breath, avoid anthraquinone excessive hydrogenation when the activity entering reactor is the highest in working fluid, degrade, along with the carrying out of reaction, continue hydrogen make-up and fresh working fluid, enable the anthraquinone in working fluid that abundant hydrogenation occur, reaction is last introduces one hydrogen, ensure that working fluid hydrogenation is complete, enhance productivity, and can not excessive hydrogenation be there is, improve the selectivity of hydrogenation reaction, effectively to suppress the generation of side reaction, improve the quality level of working fluid, reduce expensive anthraquinone consumption, reduce production cost, be conducive to follow-up oxidation and extraction process.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention (working fluid is two strands, and hydrogen-containing gas is three strands, by reactor head charging).
Fig. 2 is process flow diagram of the present invention (working fluid is two strands, and hydrogen-containing gas is three strands, by reactor bottom charging).
Wherein, 1 is fixed bed hydrogenation reactor, and 2 is working fluid I and hydrogen-containing gas I, and 3 is working fluid II and hydrogen-containing gas II, and 4 is hydrogen-containing gas III, and 5 is hydride.
Embodiment
Illustrate below in conjunction with accompanying drawing and with embodiment, this technological invention scheme to be described in detail, but therefore do not limit the present invention.
Present invention process is realized by such mode: working fluid I and hydrogen-containing gas I 2 enters from the top of fixed bed hydrogenation reactor 1 or bottom, and carry out hydrogenation reaction at catalytic bed I, reacted material enters the second beds; Working fluid II and hydrogen-containing gas II 3 enters reactor between beds I and beds II, and carry out hydrogenation reaction with the reacted mixing of materials of catalyst layer I at beds II, reacted material enters beds III; Hydrogen-containing gas III enters 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 as working material, and heavy aromatics and trioctyl phosphate, as solvent composition working fluid, adopt Pd/Al
2o
3as anthraquinone hydrogenation catalyst, the character of catalyzer 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%; Active kg (H
2o
2100%)/kg catalyst sky:>=3.3.In working fluid, anthraquinone content is 72g/L, and tetrahydro-anthraquinone content is 41g/L.
Embodiment 1
Load three sections of catalyzer in hydrogenation reactor, by upper under be followed successively by beds I, II and III, hydrogen be divided into hydrogen I, II and III tri-stock do not introduce reactor, hydrogenation temperature is 42 DEG C, and hydrogenation pressure is 0.23Mpa.First all working fluid and hydrogen I autoreactor tops flow to into reactor, there is hydrogenation reaction in beds I, the volumetric flow rate (Nm of hydrogen I and total hydrogen
3/ h) than being 1:3.78, the residence time of material in beds I is 3.05 minutes; Volumetric flow rate (the Nm of hydrogen II and total hydrogen
3/ h) than being 1:1.97, the residence time of material of material in beds II is 1.64 minutes; The volume ratio of the hydrogen III that beds III introduces and total hydrogen is 1:4.96, and the residence time of material in beds III is 1.5 minutes.After this method process, hydrogen anthraquinone and tetrahydrochysene hydrogen anthraquinone content are respectively 28.8g/L and 16.3g/L, and hydrogen effect reaches 6.12g/L, and the consumption of anthraquinone is 0.38 kg/T27.5% H
2o
2.
Embodiment 2
Three sections of catalyzer are loaded in hydrogenation reactor, by upper under be followed successively by beds I, II and III, working fluid is divided into working fluid I and II two strands, hydrogen be divided into hydrogen I, II and III tri-strands introduce reactor, hydrogenation temperature is 45 DEG C, hydrogenation pressure is 0.25Mpa.Working fluid I and hydrogen I autoreactor top also flow to into reactor, in beds I, hydrogenation reaction occur.Volumetric flow rate (the m of working fluid I and total working liquid
3/ h) than being 1:1.24, the volumetric flow rate (m of hydrogen I and total hydrogen
3/ h) than being 1:2.8, the residence time of material in beds I is 2.25 minutes; Volumetric flow rate (the m of working fluid II and total working liquid
3/ h) than being 1:5.21, the volumetric flow rate (m of hydrogen and total hydrogen in beds II
3/ h) than being 1:2.69, the residence time of material in beds II is 1.85 minutes; Volumetric flow rate (the m of hydrogen III and total hydrogen
3/ h) than being 1.5 minutes for the residence time of material of 1:3.70, beds III.After this method process, hydrogen anthraquinone tetrahydrochysene hydrogen anthraquinone content is respectively 30.24g/L and 17.22g/L, and hydrogen effect reaches 6.44g/L, and the consumption of anthraquinone is 0.38 kg/T27.5% H
2o
2.
Embodiment 3
Four sections of catalyzer are loaded in hydrogenation reactor, by upper under be followed successively by beds I, II, III and IV, working fluid is divided into working fluid I, II and III tri-strands, hydrogen be divided into hydrogen I, II, III and IV tetra-strands introduce reactor, hydrogenation temperature is 43 DEG C, and hydrogenation pressure is 0.2Mpa.Working fluid I and hydrogen I autoreaction top also flow to into reactor, in beds I, hydrogenation reaction occur.Volumetric flow rate (the m of working fluid I and total working liquid
3/ h) than being 1:1.84, the volumetric flow rate (Nm of hydrogen I and total hydrogen
3/ h) than being 1:4.66, the residence time of material in beds I is 1.94 minutes; Volumetric flow rate (the m of working fluid II and total working liquid
3/ h) than being 1:4.38, the volumetric flow rate (Nm of hydrogen II and total hydrogen
3/ h) than being 1:5.7, the residence time of material in the second bed is 1.7 minutes; Volumetric flow rate (the m of working fluid III and total working liquid
3/ h) than being 1:4.38, the volumetric flow rate (Nm of hydrogen III and total hydrogen
3/ h) than being 1:5.7, the residence time of material in beds III is 1.57 minutes; Volumetric flow rate (the Nm of hydrogen IV and total hydrogen
3/ h) than being 1:4.09; Residence time of material in beds IV is 1.5 minutes.
After this method process, hydrogen anthraquinone, tetrahydrochysene hydrogen anthraquinone content are respectively 33.7g/L and 15.9g/L, and hydrogen effect reaches 6.82g/L, and the consumption of anthraquinone is 0.36 kg/T27.5% H
2o
2.
Comparative example 1
Three sections of catalyzer are loaded in hydrogenation reactor, hydrogenation temperature is 48 DEG C, and hydrogenation pressure is 0.25Mpa, and whole working fluid and hydrogen autoreactor top also flow to into reactor, successively through first, second, and third bed generation hydrogenation reaction, residence time of material is 5.6 minutes.After this method process, hydrogen anthraquinone and tetrahydrochysene hydrogen anthraquinone content are respectively 26.7g/L and 15g/L, and hydrogen effect is 5.66g/L, and the consumption of anthraquinone is 0.47kg/T27.5% H
2o
2.
Claims (15)
1. the hydrogenation process of a hydrogen dioxide solution production by anthraquinone process, it is characterized in that comprising following content: the working fluid of hydrogen dioxide solution production by anthraquinone process hydrogenation process and hydrogen-containing gas, reactor is introduced along Flow of Goods and Materials direction share split in reactor, hydrogenation reaction is carried out at beds, per share working fluid one hydrogen-containing gas corresponding, wherein hydrogen-containing gas is divided into 2 ~ 10 strands, and the number of share of stock of working fluid is less than hydrogen-containing gas number of share of stock, is hydrogen-containing gas along most end stock material on Flow of Goods and Materials direction.
2. technique according to claim 1, is characterized in that: hydrogen-containing gas is the one in the mixture of pure hydrogen, hydrogen and nitrogen or the mixture of hydrogen and rare gas element, and hydrogen volume fraction is in the gas phase 10% ~ 100%.
3. technique according to claim 1, is characterized in that: the volumetric flow rate (Nm of per share hydrogen-containing gas and total hydrogen-containing gas
3/ h) than being 1:2 ~ 1:10.
4. technique according to claim 1, is characterized in that: the volumetric flow rate (m of per share working fluid and total working liquid
3/ h) than being 1:1 ~ 1:9.
5. technique according to claim 1, is characterized in that: the volumetric flow rate (Nm of per share working fluid and corresponding per share hydrogen-containing gas
3/ h) than being 1:1.5 ~ 1:15.
6. technique according to claim 1, is characterized in that: the quantity of catalyst reactor bed is 2 ~ 10, and is no less than the number of share of stock of hydrogen-containing gas.
7. technique according to claim 1, is characterized in that: the flow direction of material is for along reactor from top to bottom or from bottom to top.
8. the technique according to claim 1 or 6, is characterized in that: reaction mass is 1 ~ 3.5 minute in the residence time of each beds.
9. technique according to claim 1, is characterized in that: the temperature of reaction of hydrogenation process is 40 ~ 60 DEG C, and reaction pressure is 0.2 ~ 0.3MPa.
10. technique according to claim 1, is characterized in that: the noble metal catalyst that to adopt with palladium or platinum in beds be active ingredient.
11. techniques according to claim 1, is characterized in that: working fluid is divided into two strands, are respectively working fluid I and II, hydrogen-containing gas is divided into three strands, be respectively hydrogen-containing gas I, II and III, beds is 3, is respectively beds I, II and III from top to bottom; Wherein hydrogenation process is as follows: working fluid 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 fluid II and hydrogen-containing gas II enters reactor between beds I and beds II, and carry out hydrogenation reaction with the reacted mixing of materials of catalyst layer I at beds II, reacted material enters beds III; Hydrogen-containing gas III enters reactor between beds II and beds III, and carry out hydrogenation reaction with the reacted mixing of materials of beds II at catalyst layer III, final hydrogenated products flows out from reactor bottom, enters subsequent processing.
12. techniques according to claim 1, is characterized in that: working fluid is divided into two strands, are respectively working fluid I and II, hydrogen-containing gas is divided into three strands, be respectively hydrogen-containing gas I, II and III, beds is 3, is respectively beds I, II and III from the bottom to top; Wherein hydrogenation process is as follows: working fluid 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 fluid II and hydrogen-containing gas II enters reactor between beds I and beds II, and carry out hydrogenation reaction with the reacted mixing of materials of catalyst layer I at beds II, reacted material enters beds III; Hydrogen-containing gas III enters reactor between beds II and beds III, and carry out hydrogenation reaction with the reacted mixing of materials of beds II at catalyst layer III, final hydrogenated products flows out from reactor head, enters subsequent processing.
13. techniques according to claim 11 or 12, is characterized in that: the volumetric flow rate (Nm of working fluid I and hydrogen-containing gas I
3/ h) than being 1:1.6 ~ 1:2.5.
14. techniques according to claim 11 or 12, is characterized in that: the volumetric flow rate (Nm of working fluid II and hydrogen-containing gas II
3/ h) than being 1:3.5 ~ 1:10.
15. techniques according to claim 11 or 12, is characterized in that: the volumetric flow rate (Nm of hydrogen-containing gas III and total hydrogen-containing gas
3/ h) than being 1:2 ~ 1:5.
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Cited By (4)
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| CN106542502A (en) * | 2015-09-17 | 2017-03-29 | 中国石油化工股份有限公司 | Cycle working fluid renovation process and a kind of method for producing hydrogen peroxide in a kind of process for prepairng hydrogen peroxide by anthraquinone technique |
| CN106892408A (en) * | 2015-12-18 | 2017-06-27 | 中国石油化工股份有限公司 | A kind of method for oxidation of hydrogen peroxide production process |
| CN109911860A (en) * | 2019-04-26 | 2019-06-21 | 北京凯迪森科技有限公司 | A method of strengthening hydrogen dioxide solution production by anthraquinone process and hydrogen fixed bed gas-liquid is added to be distributed |
| CN115247077A (en) * | 2021-04-26 | 2022-10-28 | 中国石油化工股份有限公司 | Gasoline hydrodesulfurization method |
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