CN115745770A - Method and system for recovering anthraquinone from inactivated alumina - Google Patents
Method and system for recovering anthraquinone from inactivated alumina Download PDFInfo
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- CN115745770A CN115745770A CN202211587076.XA CN202211587076A CN115745770A CN 115745770 A CN115745770 A CN 115745770A CN 202211587076 A CN202211587076 A CN 202211587076A CN 115745770 A CN115745770 A CN 115745770A
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- alumina
- soaking
- solution
- anthraquinone
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 150000004056 anthraquinones Chemical class 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 21
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 title abstract description 24
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000002791 soaking Methods 0.000 claims abstract description 26
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims abstract description 16
- 238000004821 distillation Methods 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 16
- SJEBAWHUJDUKQK-UHFFFAOYSA-N 2-ethylanthraquinone Chemical compound C1=CC=C2C(=O)C3=CC(CC)=CC=C3C(=O)C2=C1 SJEBAWHUJDUKQK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000011084 recovery Methods 0.000 claims abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012046 mixed solvent Substances 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 16
- 238000007670 refining Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 4
- 239000002351 wastewater Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000010865 sewage Substances 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- 238000010411 cooking Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000005453 pelletization Methods 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- 238000010025 steaming Methods 0.000 claims description 2
- 230000001502 supplementing effect Effects 0.000 claims description 2
- 239000002699 waste material Substances 0.000 abstract description 10
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 13
- 239000012224 working solution Substances 0.000 description 6
- YEVQZPWSVWZAOB-UHFFFAOYSA-N 2-(bromomethyl)-1-iodo-4-(trifluoromethyl)benzene Chemical compound FC(F)(F)C1=CC=C(I)C(CBr)=C1 YEVQZPWSVWZAOB-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 238000006277 sulfonation reaction Methods 0.000 description 1
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention belongs to the technical field of organic raw material recovery, and particularly relates to a method and a system for recovering anthraquinone from deactivated alumina in hydrogen peroxide production. The method is realized by the following steps: weighing the inactivated alumina, and crushing; adding the crushed alumina into a mixed solvent consisting of heavy aromatic hydrocarbon and toluene, and heating and soaking; after soaking, the solution is pressed out by nitrogen, then the solution is distilled, and distillate after distillation is refined to obtain the 2-ethyl anthraquinone. The inactivated alumina is soaked by the specific solvent, so that the recovery rate of anthraquinone is high; the system provided by the invention can effectively recover anthraquinone adsorbed in waste alumina, reduce production consumption and save cost.
Description
Technical Field
The invention belongs to the technical field of organic raw material recovery, and particularly relates to a method and a system for recovering anthraquinone from deactivated alumina in hydrogen peroxide production.
Background
The method is characterized in that 2-ethyl anthraquinone is used as a carrier, heavy aromatic hydrocarbon and trioctyl phosphate are used as mixed solvents to prepare working solution with a certain solvent ratio, and the working solution is subjected to catalytic hydrogenation, air oxidation, sieve plate extraction and purification, working solution post-treatment and other processes in a closed circulating system to produce hydrogen peroxide. The post-treatment unit comprises a clay bed, and the filled active alumina further reduces the alkalinity of the working solution and plays a role in regenerating anthraquinone degradation products.
The active alumina is white spherical particles, the interior of the active alumina has a porous structure, the inactivated alumina can adsorb a certain amount of working solution components (anthraquinone, aromatic hydrocarbon and trioctyl phosphate) and other impurities, and the active alumina cannot be used repeatedly. Therefore, the research on how to recover the anthraquinone in the waste alumina has important significance on effectively reducing consumption and saving production cost.
Disclosure of Invention
The invention aims to provide a method for recovering anthraquinone from deactivated alumina, which can effectively recover anthraquinone adsorbed in waste alumina, reduce production consumption and save cost.
The invention also provides a system for recovering anthraquinone from the deactivated alumina based on the method.
The technical scheme adopted by the invention for realizing the purpose is as follows:
the invention provides a method for recovering anthraquinone from deactivated alumina, which comprises the following steps:
(1) Weighing the inactivated alumina, and crushing;
(2) Adding the crushed alumina into a mixed solvent consisting of heavy aromatic hydrocarbon and toluene, and heating and soaking;
(3) After soaking, the solution is pressed out by nitrogen, then the solution is distilled, and distillate after distillation is refined to obtain the 2-ethyl anthraquinone.
Further, in the step (2), the feed-liquid ratio of the alumina to the mixed solution is 1-2mL; the soaking temperature is 40 ℃, and the soaking time is 24 hours.
Further, the mixed solvent is composed of heavy aromatic hydrocarbon and toluene according to a volume ratio of 1.
Further, the soaking time is 20-24h.
The invention also provides a system for recovering anthraquinone from deactivated alumina based on the method, which comprises the following steps:
(1) Sending the inactivated alumina into a washing tank, and supplementing a mixed solvent in a solvent storage tank into the washing tank for soaking;
(2) After soaking for a certain time, transferring the solution into a distillation still through a filter, steaming the treated inactivated alumina with steam, cooling the solution by a cooler, then feeding the cooled solution into an oil-water separator, separating the solution, feeding the separated solution into a wastewater tank, and then treating sewage;
(3) Controlling the temperature of the distillation kettle, and returning the evaporated solvent to the solvent recovery tank through a first-stage condenser and a second-stage condenser for recycling;
(4) Refining distillate discharged from the bottom of the distillation kettle, controlling the pressure and the temperature, transferring the product to a product kettle, cooling and slicing by a slicer to obtain a finished product of the 2-ethyl anthraquinone.
Further, in the step (1), in the soaking treatment process, standing or circulating auxiliary treatment is carried out through a circulating pump.
Further, in the step (2), the cooking time is 10-12h.
Further, in the step (3), the temperature of the distillation kettle is controlled to be 130-160 ℃.
Further, in the step (4), the refining process comprises: and (3) conveying the distillate to a rectifying kettle, transferring the product to a product kettle under the action of a vacuum system by controlling the pressure and the temperature, and cooling and slicing the product by a grain cutting system to obtain a finished product of the 2-ethylanthraquinone.
Further, under the action of a vacuum system, the pressure is controlled to be minus 0.1 to minus 0.13MPa, and the temperature is 200 ℃.
The heavy aromatic hydrocarbon used in the invention is mixed aromatic hydrocarbon mainly containing carbon nonaromatic hydrocarbon, is one of solvents of working solution used for preparing hydrogen peroxide, is colorless or yellowish transparent liquid, and has a boiling range as follows: 150-180 ℃ (150 ℃ front cut is less than or equal to 5%) (normal pressure), aromatic hydrocarbon content: not less than 98 percent (measured by a sulfonation method) and purchased from Jiangsu Zhengdan chemical industry Co.
The invention provides a device for recovering anthraquinone from deactivated alumina, which relates to the extraction of crude anthraquinone and the refining of anthraquinone, and mainly comprises the following steps: and (3) putting the waste alumina spheres into a newly-built washing tank, completely soaking the waste alumina spheres by using a solvent, dissolving for a certain time, then pressing the solution into a distillation kettle by using nitrogen, transferring the evaporated substances into a refining kettle, and obtaining anthraquinone solids through a product kettle and a granulating system.
The invention has the beneficial effects that:
(1) The inactivated alumina is soaked by the specific solvent, so that the recovery rate of anthraquinone is high;
(2) The system provided by the invention can effectively recover anthraquinone adsorbed in waste alumina, reduce production consumption and save cost.
Drawings
FIG. 1 is a diagram of an apparatus for recovering anthraquinones from deactivated alumina; wherein, 1, a washing tank; 2. a distillation kettle; 3. a first-stage condenser; 4. a secondary condenser; 5. a recovery liquid tank; 6. a solvent storage tank; 7. a circulation pump; 8. a filter; 9. an oil-water separator; 10. a wastewater tank; 11. a cooler; 12. a vacuum system.
FIG. 2 is a view of a refining system after recovery of anthraquinones; wherein, 13, a refining kettle; 14. a product kettle; 15. a pelletizing system; 16. a vacuum system.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The invention provides a method for recovering anthraquinone from deactivated alumina, which comprises the steps of loading waste alumina balls into a newly-built washing tank, completely soaking the waste alumina balls by using a solvent, and starting auxiliary facilities for treatment.
The invention provides a device for recovering anthraquinone from deactivated alumina, which comprises the following steps:
(1) Conveying the waste alumina into a washing tank 1 by using a belt conveyor, adding a corresponding appropriate amount of solvent into the washing tank 1, and starting a circulating pump 7 for circulation or standing;
(2) After 24h of treatment, the solution was transferred to distillation kettle 2; the treated waste alumina is boiled by steam for 12h, separated by an oil-water separator 9 and then enters a waste water tank for sewage treatment.
(3) Controlling the temperature of the distillation kettle, and condensing the evaporated solvent through a first-stage condenser 3 and a second-stage condenser 4 to return to a solvent recovery tank 5 for reuse.
(4) And (3) sending distillate discharged from the bottom of the distillation kettle to a refining kettle 13, controlling the pressure and the temperature, transferring the product to a product kettle, and cooling and slicing the product by a slicer 15 to obtain a finished product of the 2-ethyl anthraquinone.
In some embodiments, the still distillate may be used to prepare a working fluid and may not be subjected to a refining process.
Example 1
Weighing 30g of deactivated alumina, crushing, soaking in 50ml of toluene and heavy aromatic hydrocarbon (volume ratio 1; weighing 30g of deactivated alumina, soaking the alumina in 50ml of toluene and heavy aromatic hydrocarbon (volume ratio 1); weighing 30g of deactivated alumina, soaking the alumina in 50ml of toluene and heavy aromatic hydrocarbon (volume ratio 1); after 24h, the experiments (1) to (3) were sampled and analyzed for the total effective anthraquinone content: 4.75%, 4.52% and 4.78%.
Example 2
Weighing 3 groups of 30g of deactivated alumina, soaking the alumina respectively by using 50ml of heavy aromatic hydrocarbon, 50ml of toluene, 50ml of heavy aromatic hydrocarbon (volume ratio is 1): 27g/l, 35g/l and 30g/mL.
Example 3
Weighing 2 groups of 30g of deactivated alumina, soaking the 2 groups of deactivated alumina in 50ml of toluene and heavy aromatic hydrocarbon (volume ratio is 1; the second group stands still, and the rest conditions are unchanged and are recorded as experiment (2); after 24h, respectively sampling and analyzing the effective anthraquinone content, and respectively: 6.7% and 6.1%.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for recovering anthraquinones from deactivated alumina, comprising the steps of:
(1) Weighing the inactivated alumina, and crushing;
(2) Adding the crushed alumina into a mixed solvent consisting of heavy aromatic hydrocarbon and toluene, and heating and soaking;
(3) After soaking, the solution is pressed out by nitrogen, then the solution is distilled, and distillate after distillation is refined to obtain the 2-ethyl anthraquinone.
2. The method according to claim 1, wherein the feed-liquid ratio of the alumina to the mixed solution is 1-2mL; the soaking temperature is 40 ℃, and the soaking time is 24 hours.
3. The method according to claim 1 or 2, wherein the mixed solvent is composed of heavy aromatic hydrocarbons and toluene in a volume ratio of 1.
4. The method according to any one of claims 1 to 3, wherein the soaking time is 20 to 24 hours.
5. A system for recovering anthraquinones from deactivated alumina by the method according to any one of claims 1 to 4, which comprises:
(1) Sending the inactivated alumina into a washing tank (1), and supplementing a mixed solvent in a solvent storage tank (6) into the washing tank (1) for soaking treatment;
(2) After soaking for a certain time, transferring the solution into a distillation kettle (2) through a filter (8), steaming the treated inactivated alumina with steam, cooling the solution by a cooler (11), then feeding the cooled solution into an oil-water separator (9), separating the solution, feeding the separated solution into a wastewater tank (10), and then treating sewage;
(3) Controlling the temperature of the distillation kettle (2), and returning the evaporated solvent to the solvent recovery tank (5) through the first-stage condenser (3) and the second-stage condenser (4) for recycling;
(4) And (3) refining distillate discharged from the bottom of the distillation kettle (2), controlling the pressure and the temperature, transferring the product to a product kettle, and cooling and slicing the product by a slicer to obtain a finished product of the 2-ethyl anthraquinone.
6. The system according to claim 5, wherein in the step (1), during the soaking treatment, the soaking treatment is performed in a standing state or a circulation auxiliary treatment is performed by a circulation pump (7).
7. The system of claim 5, wherein in the step (2), the cooking time is 10-12h.
8. The system according to claim 5, wherein in step (3), the temperature of the distillation still (2) is controlled to be 130-160 ℃.
9. The system according to any one of claims 5 to 7, wherein in the step (4), the refining is carried out by the specific steps of: and (3) conveying the distillate to a rectifying kettle (13), transferring the product to a product kettle (14) under the action of a vacuum system (16) by controlling the pressure and the temperature, and cooling and slicing the product by a pelletizing system (15) to obtain a finished product of the 2-ethyl anthraquinone.
10. The system according to claim 9, characterized in that the vacuum system (16) is controlled at a pressure of-0.1 to-0.13 MPa and a temperature of 200 ℃.
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| CN202211587076.XA CN115745770A (en) | 2022-12-08 | 2022-12-08 | Method and system for recovering anthraquinone from inactivated alumina |
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| CN202211587076.XA CN115745770A (en) | 2022-12-08 | 2022-12-08 | Method and system for recovering anthraquinone from inactivated alumina |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111437889A (en) * | 2020-04-01 | 2020-07-24 | 安徽泉盛化工有限公司 | Regeneration method of catalyst of hydrogenation system for producing hydrogen peroxide by anthraquinone process |
| CN113289694A (en) * | 2021-06-28 | 2021-08-24 | 广西田东达盛化工科技有限公司 | Method for regenerating palladium catalyst in production of hydrogen peroxide by anthraquinone process |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111437889A (en) * | 2020-04-01 | 2020-07-24 | 安徽泉盛化工有限公司 | Regeneration method of catalyst of hydrogenation system for producing hydrogen peroxide by anthraquinone process |
| CN113289694A (en) * | 2021-06-28 | 2021-08-24 | 广西田东达盛化工科技有限公司 | Method for regenerating palladium catalyst in production of hydrogen peroxide by anthraquinone process |
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