CN104555937A - Alumina regenerant for preparing hydrogen peroxide by anthraquinone process - Google Patents
Alumina regenerant for preparing hydrogen peroxide by anthraquinone process Download PDFInfo
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- CN104555937A CN104555937A CN201410833132.2A CN201410833132A CN104555937A CN 104555937 A CN104555937 A CN 104555937A CN 201410833132 A CN201410833132 A CN 201410833132A CN 104555937 A CN104555937 A CN 104555937A
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- sodium salt
- hydrogen peroxide
- basic sodium
- salt powder
- powder
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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 an alumina regenerant for preparing hydrogen peroxide by an anthraquinone process. The alumina regenerant comprises the following components: alumina powder and basic sodium salt powder, wherein the dosage of basic sodium salt powder accounts for 10-20% of the total mass; the basic sodium salt powder satisfies that the pH value of a 1 g/ml aqueous solution containing basic sodium salt powder as the solute is 9-11; the basic sodium salt powder comprises sodium oxide; the content of sodium oxide accounts for 1%-4% of basic sodium salt powder in mass percent. The alumina regenerant has excellent regenerative activity, and greatly reduces the amount of organic residues, so as to reduce the environmental pollution, make a positive contribution to emission reduction, pollution elimination and loss reduction in the production of hydrogen peroxide, and create favorable conditions for the sustainable development of hydrogen peroxide.
Description
Technical field
The present invention relates to the production technology of hydrogen peroxide (hydrogen peroxide) industrial regeneration agent, specifically refer to the anthraquinone aluminum oxide regenerator preparing hydrogen peroxide.
Background technology
Process for prepairng hydrogen peroxide by anthraquinone (hydrogen peroxide) is production method the most ripe in the world at present, its technological process be generally with 2-EAQ (EAQ) be carrier, heavy aromatics (AR) and trioctyl phosphate (TOP) be for mixed solvent, be mixed with the working fluid with definite composition, it is passed into together with hydrogen and is equipped with in the hydrogenation bed of catalyzer, 2-EAQ (EAQ) carries out hydrogenation with hydrogen under certain pressure and temperature, generate corresponding hydrogen anthraquinone (HEAQ), gained solution claims hydride.Hydride is again by the dioxygen oxidation in air, and hydrogen anthraquinone wherein reverts to original anthraquinone, simultaneously Hydrogen Peroxide, and gained solution is called oxidation solution.Utilize the difference of hydrogen peroxide solubleness in water and working fluid and the density difference of working fluid and water, with the hydrogen peroxide in pure water extraction oxidation solution, obtain aqueous hydrogen peroxide solution (being commonly called as hydrogen peroxide).This aqueous solution can obtain hydrogen peroxide product through purifying treatment.Working fluid (title raffinate) after water extraction, through postprocessing working procedures K
2cO
3solution drying and dehydrating decomposing H
2o
2with settlement separate alkali, then obtain working fluid through the activated alumina absorption in carclazyte bed except after alkali and regeneration degradation product, working fluid recirculation is used.
But activated alumina makes also to have adsorbed a large amount of working fluids in working fluid regenerative process, initial stage adsorptive capacity arrives more than 40%, working fluid is consumed in a large number, need the effective constituent of constantly supplementing working fluid to ensure the carrying out that hydrogen peroxide reacts, discarded aluminum oxide organic substance residues amount when to unload bed is still up to more than 20%, this not only increases raw materials consumption and production cost, also causes serious pollution to environment.In addition, the composition of this discarded aluminum oxide organic substance residues thing mainly contains anthraquinone, the pungent fat of tricresyl phosphate, aromatic hydrocarbons, organic degradation thing, phosphoric acid salt etc., these compositions are all not oxidizable, general is all high temperature sintering in 1300 DEG C of rotary kilns, organic residue is volatilized away, aluminum oxide obtains regeneration, but organic residue large portion in rotary kiln is steam state volatilization, this organic steam cannot be recycled so far, it is all in line sky, cause great environmental pollution, aluminum oxide is abandoned in electric furnace calcination as we get 50 grams of useless oxygen, the gas of stench fills the air at once, make people's eyes are blurred by tears, respiratory tract suffocates, people and animals flee from, flowers and plants are withered and yellow.It is to the far super hydrogen sulfide of the destruction of earth's ozone layer, is on hundred times of carbonic acid gas.The pollution China of preparing the discarded aluminum oxide reprocessing that hydrogen peroxide discharges occurred before 30 years, along with the rapid raising that hydrogen peroxide can produce, the reprocessing amount of discarded aluminum oxide also increases thereupon, and existing annual not lower 70,000 tons, it is how very grave disaster to the pollution of environment as seen.Owing to cannot effectively administer this pollution always, become situation out of control so far, under the situation of environment-protecting high-pressure, hydrogen peroxide industry is faced with the condition of limited production.
Therefore, research and develop a kind of high reactivity and will have very important significance to the anthraquinone hydrogen peroxide regenerator of preparing of the low absorption of the effective constituent of working fluid.
Summary of the invention
The object of the invention is the shortcoming and defect existed to overcome prior art, and provide a kind of high reactivity and to the low absorption of the effective constituent of working fluid and Residual organic solvent is low, the anthraquinone aluminum oxide regenerator preparing hydrogen peroxide that environment protecting is good.
For achieving the above object, technical scheme of the present invention is aluminum oxide powder and basic sodium salt powder, and the addition of basic sodium salt powder is the 10-20% accounting for total mass; Described basic sodium salt powder meets with the pH value in the aqueous solution of its 1g/ml being solute for 9-11, is metering unit with NaO in this basic sodium salt powder, and the mass ratio that the content of this metering unit accounts for basic sodium salt powder is 1%-5%.
Further setting is described aluminum oxide powder is gamma oxidation aluminium powder.
Further setting is described basic sodium salt powder is basic sodium salt powder.
Technique scheme of the present invention has very excellent regeneration activity, and greatly reduce Residual organic solvent, thus the pollution reduced environment, decontamination Loss reducing is reduced discharging to Hydrogen Peroxide Production and has made positive contribution, for the sustainable development of hydrogen peroxide creates favorable conditions, concrete effect is see the testing data in embodiment.
The anthraquinone aluminum oxide regenerator preparing hydrogen peroxide of the present invention has the following advantages:
(1) good refresh function is had to degradation product: traditional aluminum oxide is to the regeneration activity 2-3g/L of anthraquinone working fluid.And the regeneration activity of aluminum oxide regenerator of the present invention can reach 5-15g/L, total degradation substrate concentration more than decline 10g/L in working fluid can be made, be not only conducive to hydrogenation but also reduce anthraquinone consumption;
(2) aluminum oxide regenerator of the present invention carries out degree of depth absorption to the micro-alkali in working fluid, and dealkalize function surpasses traditional aluminum oxide, and its dealkalize degree of depth can reach 0.001g/L, is 6 times of traditional aluminum oxide.Dealkalize while, moisture content is also removed, and in working fluid, micro-water content drops to below 2g/L from original 3-4g/L;
(3) quality-advantage of aluminum oxide regenerator of the present invention is also embodied in working fluid viscosity, proportion, interfacial tension etc. are improved comprehensively, systemic resistance reduces, and flow increases, output increased, consume and reduce, make production step into benign cycle;
(4) aluminum oxide contained in aluminum oxide regenerator of the present invention has porous structure, and when having adsorbed extensive work liquid, alkali formula double salt in aluminum oxide regenerator of the present invention will occupy most pore structures of aluminum oxide, the adsorptive capacity of working fluid has dropped to 18% from 40%, Residual organic solvent has dropped to less than 1% from 20%, and the range of decrease is for can reach more than 90%;
(5) along with working fluid band alkali is few, the reduction of total degradation thing, effective component not easily runs off, work-ing life effectively continues, usage period can increase by 50%, the reduction by 50% of such carclazyte consumption, the more traditional use aluminum oxide of hydrogen peroxide unit output working fluid consumption decreases by more than 90%.Working fluid of this part absorption is mostly adhered to intergranular macrovoid, instead of occupies in the molecular structure hole after oxygen aluminium molecular dehydration, as long as so slightly steaming out will be discharged outside oxygen aluminum particulate.
Below in conjunction with embodiment, the present invention is described further.
Embodiment
Below by embodiment, the present invention is specifically described; only be used to further illustrate the present invention; can not be interpreted as limiting the scope of the present invention, the technician in this field can make some nonessential improvement and adjustment according to the content of foregoing invention to the present invention.
Embodiment
This anthraquinone aluminum oxide regenerator preparing hydrogen peroxide comprises following component: aluminum oxide powder and basic sodium salt powder, and the addition of basic sodium salt powder is the 10-20% accounting for total mass; Described basic sodium salt powder meets with the pH value in the aqueous solution of its 1g/ml being solute for 9-11, is metering unit with NaO in this basic sodium salt powder, and the mass ratio that the content of this metering unit accounts for basic sodium salt powder is 1%-5%.
| Component | Basic sodium salt powder | Aluminum oxide powder |
| Embodiment 1 | The mass ratio that 10wt%, NaO account for basic sodium salt powder is 5% | Aluminum oxide powder surplus |
| Embodiment 2 | The mass ratio that 20 wt%, NaO account for basic sodium salt powder is 1% | Gamma oxidation aluminium powder surplus |
| Embodiment 3 | The mass ratio that 15 wt%, NaO account for basic sodium salt powder is 2% | Gamma oxidation aluminium powder surplus |
| Embodiment 4 | The mass ratio that 17 wt%, NaO account for basic sodium salt powder is 3% | Aluminum oxide powder surplus |
Aluminum oxide powder described in the present embodiment is preferably gamma oxidation aluminium powder.
Basic sodium salt powder described in the present embodiment and aluminum oxide powder are more than 320 orders.
test example
table one,the pH value of alkali formula double salt is on the impact of regeneration activity (pH value in the aqueous solution of 1g/ml for)
| PH value | General anthraquinone | 2-EAQ | Tetrahydro-anthraquinone |
| 8 | 136g/L | 44g/L | 91g/L |
| 9 | 138g/L | 46g/L | 92g/L |
| 10 | 141g/L | 47g/L | 94g/L |
| 11 | 145g/L | 49g/L | 96g/L |
| 12 | 148g/L | 51g/L | 97g/L |
As shown in Table 1, illustrate that the pH value of alkali formula double salt is higher, regeneration activity is better, but pH value can make darkening of working fluid higher than 12, causes each tower body visor fuzzy, and all pH value are preferably the alkali formula double salt of 11.
In table two, alkali formula double salt, sodium oxide content is on the impact of regeneration activity
| Sodium oxide content (wt%) | General anthraquinone | 2-EAQ | Tetrahydro-anthraquinone |
| 1% | 136g/L | 45g/L | 91g/L |
| 2% | 138g/L | 46g/L | 92g/L |
| 3% | 143g/L | 49g/L | 94g/L |
| 4% | 148g/L | 51g/L | 97g/L |
The sodium oxide content of 3% is finally suitable for, and namely has good regeneration activity, can not damage again to working fluid.
Alkali formula double salt addition in the aluminum oxide regenerator of table three, configuration is to the relation table of regeneration activity and working fluid adsorptivity
| Alkali formula double salt addition | Regeneration activity | Traditional aluminum oxide is to working fluid adsorptive capacity | Aluminum oxide regenerator of the present invention is to the adsorptive capacity of working fluid |
| 10wt% | 8 g/L | 25% | 10% |
| 12wt% | 10 g/L | 22% | 7% |
| 15wt% | 12 g/L | 20% | 5% |
| 18 wt% | 15 g/L | 18% | 3% |
| 20 wt% | 17 g/L | 16% | 1% |
Therefore, the alkali formula double salt addition selecting 20% is good.
Claims (2)
1. the anthraquinone aluminum oxide regenerator preparing hydrogen peroxide, is characterized in that comprising following component: aluminum oxide powder and basic sodium salt powder, and the addition of basic sodium salt powder is the 10-20% accounting for total mass;
Described basic sodium salt powder meets with the pH value in the aqueous solution of its 1g/ml being solute for 9-11, is metering unit with NaO in this basic sodium salt powder, and the mass ratio that the content of this metering unit accounts for basic sodium salt powder is 1%-5%.
2. the anthraquinone aluminum oxide regenerator preparing hydrogen peroxide according to claim 1, is characterized in that: described aluminum oxide powder is gamma oxidation aluminium powder.
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| CN201410833132.2A CN104555937A (en) | 2014-12-29 | 2014-12-29 | Alumina regenerant for preparing hydrogen peroxide by anthraquinone process |
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| CN201410833132.2A CN104555937A (en) | 2014-12-29 | 2014-12-29 | Alumina regenerant for preparing hydrogen peroxide by anthraquinone process |
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| CN104555937A true CN104555937A (en) | 2015-04-29 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104724677A (en) * | 2015-03-10 | 2015-06-24 | 何国炎 | Aluminum oxide regenerant for preparing hydrogen peroxide through anthraquinone process |
| CN105174229A (en) * | 2015-08-28 | 2015-12-23 | 陕西开达化工有限责任公司 | Composite activated regenerant for hydrogen peroxide working fluid of anthraquinone process and preparation method thereof |
| CN109956489A (en) * | 2019-04-30 | 2019-07-02 | 刘�文 | The recovery method of waste activated alumina during process for prepairng hydrogen peroxide by anthraquinone |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101066751A (en) * | 2006-05-01 | 2007-11-07 | 三菱瓦斯化学株式会社 | Method for activating hydrogenation catalyst and method for producing hydrogen peroxide including same |
| CN101455959A (en) * | 2008-12-29 | 2009-06-17 | 中国铝业股份有限公司 | Catalyst for regenerating anthraquinone degradation products and preparation method thereof |
-
2014
- 2014-12-29 CN CN201410833132.2A patent/CN104555937A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101066751A (en) * | 2006-05-01 | 2007-11-07 | 三菱瓦斯化学株式会社 | Method for activating hydrogenation catalyst and method for producing hydrogen peroxide including same |
| CN101455959A (en) * | 2008-12-29 | 2009-06-17 | 中国铝业股份有限公司 | Catalyst for regenerating anthraquinone degradation products and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 姚迎等: "《化学知识辞典》", 30 September 1995 * |
| 王俊杰等: "蒽醌法生产过氧化氢用催化剂研究进展", 《化学推进剂与高分子材料》 * |
| 皮国民: "比表面积对活性氧化铝蒽醌再生能力的影响", 《湖南有色金属》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104724677A (en) * | 2015-03-10 | 2015-06-24 | 何国炎 | Aluminum oxide regenerant for preparing hydrogen peroxide through anthraquinone process |
| CN105174229A (en) * | 2015-08-28 | 2015-12-23 | 陕西开达化工有限责任公司 | Composite activated regenerant for hydrogen peroxide working fluid of anthraquinone process and preparation method thereof |
| CN109956489A (en) * | 2019-04-30 | 2019-07-02 | 刘�文 | The recovery method of waste activated alumina during process for prepairng hydrogen peroxide by anthraquinone |
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