CN104724677A - Aluminum oxide regenerant for preparing hydrogen peroxide through anthraquinone process - Google Patents
Aluminum oxide regenerant for preparing hydrogen peroxide through anthraquinone process Download PDFInfo
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- CN104724677A CN104724677A CN201510104021.2A CN201510104021A CN104724677A CN 104724677 A CN104724677 A CN 104724677A CN 201510104021 A CN201510104021 A CN 201510104021A CN 104724677 A CN104724677 A CN 104724677A
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- Prior art keywords
- aluminum oxide
- sodium salt
- hydrogen peroxide
- basic sodium
- anthraquinone
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3433—Regenerating or reactivating of sorbents or filter aids other than those covered by B01J20/3408 - B01J20/3425
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses an aluminum oxide regenerant for preparing hydrogen peroxide through an anthraquinone process. The aluminum oxide regenerant comprises the following components: aluminum oxide and basic sodium salt, wherein the adding amount of the basic sodium salt is 10-20% of the total mass; the basic sodium salt meets the condition that the pH value is 9-11 in 1g/ml water solution by taking the basic sodium salt as a solute; and the basic sodium salt comprises sodium oxide, wherein the content of the sodium oxide is 1-4% of that of the basic sodium salt. The technical solution of the invention is excellent in regenerative activity, the organic residual quantity is greatly reduced, the environment pollution is reduced, a positive contribution for reducing emission in the hydrogen peroxide production, eliminating the pollution and reducing the consumption is made and a favorable condition for the sustainable development of the hydrogen peroxide is created.
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, now annual not lower 70,000 tons, visible its be how very grave disaster to the pollution of environment? owing to cannot effectively administer this pollution always, so far become situation out of control, 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 and basic sodium salt, and the addition of basic sodium salt is the 3-30% accounting for total mass; Described basic sodium salt meets with the pH value in the aqueous solution of its 1g/ml being solute for 9-11, is metering unit in this basic sodium salt with NaO, and the mass ratio that the content of this metering unit accounts for basic sodium salt is 1%-20%.
Further setting is described aluminum oxide is gama-alumina.
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 and basic sodium salt, and the addition of basic sodium salt is the 3-30% accounting for total mass; Described basic sodium salt meets with the pH value in the aqueous solution of its 1g/ml being solute for 9-11, is metering unit in this basic sodium salt with NaO, and the mass ratio that the content of this metering unit accounts for basic sodium salt is 1%-20%.
Aluminum oxide described in the present embodiment is preferably gama-alumina.
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)
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
The sodium oxide content of 5% 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
Therefore, the alkali formula double salt addition selecting 20% is good.
Claims (4)
1. the anthraquinone aluminum oxide regenerator preparing hydrogen peroxide, it is characterized in that comprising following component: aluminum oxide and basic sodium salt, the addition of basic sodium salt is the 3-30% accounting for total mass;
Described basic sodium salt meets with the pH value in the aqueous solution of its 1g/ml being solute for 9-11, is metering unit in this basic sodium salt with NaO, and the mass ratio that the content of this metering unit accounts for basic sodium salt is 1%-20%.
2. the anthraquinone aluminum oxide regenerator preparing hydrogen peroxide according to claim 1, is characterized in that: the addition of basic sodium salt is the 20-30% accounting for total mass
;be that the content of metering unit accounts for the mass ratio of basic sodium salt for 5%-20% with NaO.
3. the anthraquinone aluminum oxide regenerator preparing hydrogen peroxide according to claim 1, is characterized in that: the addition of basic sodium salt is the 3-10% accounting for total mass, is that the content of metering unit accounts for the mass ratio of basic sodium salt for 1%-20% with NaO.
4. the anthraquinone aluminum oxide regenerator preparing hydrogen peroxide according to claim 1, is characterized in that: described aluminum oxide is gama-alumina.
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| CN201510104021.2A CN104724677A (en) | 2015-03-10 | 2015-03-10 | Aluminum oxide regenerant for preparing hydrogen peroxide through anthraquinone process |
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| CN201510104021.2A CN104724677A (en) | 2015-03-10 | 2015-03-10 | Aluminum oxide regenerant for preparing hydrogen peroxide through anthraquinone process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111282557A (en) * | 2020-03-03 | 2020-06-16 | 王晶晶 | Regeneration method of waste alumina in hydrogen peroxide production |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1483664A (en) * | 2002-09-20 | 2004-03-24 | 中国石油化工股份有限公司巴陵分公司 | Stredford process peroxyl production work liquid post treatment method |
| 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 |
| CN104555937A (en) * | 2014-12-29 | 2015-04-29 | 何国炎 | Alumina regenerant for preparing hydrogen peroxide by anthraquinone process |
-
2015
- 2015-03-10 CN CN201510104021.2A patent/CN104724677A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1483664A (en) * | 2002-09-20 | 2004-03-24 | 中国石油化工股份有限公司巴陵分公司 | Stredford process peroxyl production work liquid post treatment method |
| 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 |
| CN104555937A (en) * | 2014-12-29 | 2015-04-29 | 何国炎 | Alumina regenerant for preparing hydrogen peroxide by anthraquinone process |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111282557A (en) * | 2020-03-03 | 2020-06-16 | 王晶晶 | Regeneration method of waste alumina in hydrogen peroxide production |
| CN111282557B (en) * | 2020-03-03 | 2021-03-16 | 王晶晶 | Regeneration method of waste alumina in hydrogen peroxide production |
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Application publication date: 20150624 |