CN1400160A - Catalyst for producing hydrogen peroxide by using anthraquinone method - Google Patents
Catalyst for producing hydrogen peroxide by using anthraquinone method Download PDFInfo
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- CN1400160A CN1400160A CN 01125029 CN01125029A CN1400160A CN 1400160 A CN1400160 A CN 1400160A CN 01125029 CN01125029 CN 01125029 CN 01125029 A CN01125029 A CN 01125029A CN 1400160 A CN1400160 A CN 1400160A
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- China
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- sepiolite
- catalyst
- acid
- hydrogen peroxide
- anthraquinone
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Abstract
The present invention discloses a catalyst for anthraquinone method to produce hydrogen peroxide and its preparation method. The load type noble metal catalyst for anthraquinone hydrogenation uses pretreated sepiolite or sepiolite-Al2O3 as carrier, containing 0.2-0l.4 wt% of Pt. Before use the sepiolite is impregnated with acid with different concentration according to different solid-liquid ratio for a certain time, then it is undergone the processes of filtering, washing, drying, tableting, roasting and pulverizing to obtain the invented product. Said catalyst is prepared with impregnation method, and features high activity and high selectivity. Under the condition of that pressure is 0.2 MPa. temp is 45 deg.C and operating fluid space velocity is 11.4 h(-1) (volume space velocity) its hydrogenation efficiency can be up to 8-12g(H2O2)/l, and its selectivity is up to above 97%.
Description
The present invention relates to a kind of producing hydrogen peroxide by using anthraquinone method loaded noble metal catalyst and preparation method thereof.
Anthraquinone is the method that has comparative advantage in the at present domestic and international hydrogen peroxide manufacture, and technology is comparatively ripe.Forefathers once used the catalyzer of nickel catalyzator as anthraquinone hydrogenation, but because its poor stability, ran into the easy spontaneous combustion of air, easily poisoned by oxygen and hydrogen peroxide and lost efficacy after be difficult to regenerate and be eliminated gradually.From the sixties, U.S. Du Pont company, FMC Corp. and Engelhard company develop and have improved a series of with Al in succession
2O
3And SiO
2Deng the palladium catalyst that is carrier, these catalyzer have activity and selectivity preferably.The price continuous rise of Pd in recent years, and the price of Pt is steady relatively, is the sepiolite resource that reduces the running cost of enterprise and utilize China's abundant, the invention discloses a kind of sepiolite supported Pt catalyzer and is used for the anthraquinone hydrogenation reaction.
The object of the present invention is to provide a kind of catalyst for producing auricome by anthraquinone method and preparation method thereof.
Content of the present invention provides a kind of method of modifying of natural sepiolite, and prepares the hydrogen peroxide manufacture anthraquinone hydrogenation catalyst of high reactivity, highly selective with its supporting Pt.
Support of the catalyst of the present invention is pretreated sepiolite or sepiolite-Al
2O
3Active ingredient is by 0.2～0.4% weight Pt and 0.2～0.6% weight K
2O forms.
Support of the catalyst of the present invention is pretreated sepiolite or sepiolite-Al
2O
3, it is characterized in that earlier natural sepiolite being immersed in the certain density acid solution with certain solid-to-liquid ratio (weight ratio), solid-to-liquid ratio can be 1: 5～and 1: 20, acid can be nitric acid or hydrochloric acid or sulfuric acid, and acid concentration can be 0.5～5mol/l, and dipping time is 2h～72h.After dipping finishes, filter, washing, drying is with sepiolite and Al
2O
3Powder mixes by a certain percentage, compressing tablet, and calcining, pulverizing is 20～50 orders.Catalyzer adopts immersion process for preparing, and the mixing solutions of the salt of the salt of Pt and K is immersed in sepiolite-Al
2O
3On, in 100～120 ℃ of dryings, N is used in 450～600 ℃ of roastings at last
2-H
2In 450 ℃ in reduction activation, make catalyzer.
The salt of the used Pt of the present invention can be Platinic chloride or Tetrachloroplatinum.Used K salt can be saltpetre or acetic acid sylvite or Repone K or salt of wormwood.
The working fluid that catalyzer that the present invention makes adopts is for heavy aromatics and trioctyl phosphate (3: 1) dissolved 2-ethyl-anthraquinone, and working fluid and hydrogen is plug flow from up to down, under 0.2MPa, 45 ℃, and liquid air speed 11.4h
-1(volume space velocity), the hydrogenation efficiency of reaction can reach 8～12g (H
2O
2)/l, selectivity reaches more than 97%.
Embodiment 1: adopt the natural sepiolite of 50g with it under agitation in the HNO of 500ml1mol/l
3Soak 24h in the solution, filter, wash to solution near neutrality till, drying, compressing tablet, in 450～600 ℃ of following roasting 3h, it is standby to be crushed to 20～50 orders.Take the above-mentioned carrier of 15g, the mixing solutions that 15ml is contained 0.045Pt and 0.09gK is poured into wherein, and in 100～120 ℃ of dry 3h, 400～600 ℃ of roasting 3h use N at last
2-H
2, air speed 300h
-1, 450 ℃ of following reduction 3h can make required catalyzer.
The above-mentioned catalyzer of 7ml is packed in the stainless steel reactor of φ 8, under 45 ℃, 0.2MPa, liquid air speed 11.4h
-1(volume space velocity), the hydrogenation efficiency of reaction are 8.43g (H
2O
2)/l, selectivity is 97.9%.
Embodiment 2: catalyst pretreatment method is with example 1, and different is with dried sepiolite powder and Al
2O
3Powder is by compressing tablet after 2: 1 the mixed, roasting.The Preparation of catalysts method is with example 1.
Adopt this catalyzer 7ml, use the condition identical with embodiment 1, the hydrogenation efficiency of reaction is 9.00g (H
2O
2)/l, selectivity is 100%.
Embodiment 3: catalyst pretreatment method is with example 1, and different is with dried sepiolite powder and Al
2O
3Powder is by compressing tablet roasting after 1: 1 the mixed.The Preparation of catalysts method is with example 1.
Adopt this catalyzer 7ml, use the condition identical with embodiment 1, the hydrogenation efficiency of reaction is 10.27g (H
2O
2)/l, selectivity is 99.7%.
Embodiment 4: the Preparation of catalysts method is with example 1, and different is with dried sepiolite powder and Al
2O
3Powder is by compressing tablet roasting after 1: 2 the mixed.The Preparation of catalysts method is with example 1.
Adopt this catalyzer 7ml, use the condition identical with embodiment 1, the hydrogenation efficiency of reaction is 10.90g (H
2O
2)/l, selectivity is 98.3%.
Claims (6)
1. a hydrogen peroxide manufacture anthraquinone hydrogenation catalyst is characterized in that carrier is sepiolite or sepiolite-Al
2O
3, active ingredient is by 0.2～0.4% weight Pt, 0.2～0.6% weight K
2O forms.
2. Preparation of catalysts method as claimed in claim 1 is characterized in that used carrier is to soak sepiolite or the sepiolite-Al that certain hour was handled with certain density acid under certain solid-to-liquid ratio
2O
3Catalyzer adopts immersion process for preparing, and the saline solution of Pt is dipped on the above-mentioned carrier, and 100～120 ℃ of dry 3h use N at last
2-H
2, air speed 300h
-1, 450 ℃ of following reduction 3h can make required catalyzer.
3. method as claimed in claim 2 is characterized in that acid can be nitric acid or hydrochloric acid or sulfuric acid.
4. as claim 2 or 3 described methods, it is characterized in that the concentration of acid can be 0.5～5mol/l.
5. method as claimed in claim 2 is characterized in that solid-to-liquid ratio (weight ratio) can be 1: 5～1: 20.
6. method as claimed in claim 2 is characterized in that the treatment time can be 5～72h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01125029 CN1400160A (en) | 2001-08-02 | 2001-08-02 | Catalyst for producing hydrogen peroxide by using anthraquinone method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01125029 CN1400160A (en) | 2001-08-02 | 2001-08-02 | Catalyst for producing hydrogen peroxide by using anthraquinone method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1400160A true CN1400160A (en) | 2003-03-05 |
Family
ID=4665857
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 01125029 Pending CN1400160A (en) | 2001-08-02 | 2001-08-02 | Catalyst for producing hydrogen peroxide by using anthraquinone method |
Country Status (1)
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| CN (1) | CN1400160A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100445874C (en) * | 2006-02-15 | 2008-12-24 | 虹创科技股份有限公司 | Thin film pattern layer producing method |
| CN103663385A (en) * | 2012-09-21 | 2014-03-26 | 中国石油化工股份有限公司 | Method and device of producing hydrogen peroxide |
| CN109675543A (en) * | 2018-12-17 | 2019-04-26 | 新地能源工程技术有限公司 | A kind of sepiolite-alumina composite carrier and the high temperature sintering resistant type methanation catalyst using it |
| CN112717926A (en) * | 2019-10-28 | 2021-04-30 | 中国石油化工股份有限公司 | Catalyst for producing hydrogen peroxide by anthraquinone hydrogenation and preparation method and application thereof |
| CN114100608A (en) * | 2021-12-20 | 2022-03-01 | 河北工业大学 | Preparation method of thermal modified sepiolite mineral loaded Rh monatomic catalyst |
-
2001
- 2001-08-02 CN CN 01125029 patent/CN1400160A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100445874C (en) * | 2006-02-15 | 2008-12-24 | 虹创科技股份有限公司 | Thin film pattern layer producing method |
| CN103663385A (en) * | 2012-09-21 | 2014-03-26 | 中国石油化工股份有限公司 | Method and device of producing hydrogen peroxide |
| CN109675543A (en) * | 2018-12-17 | 2019-04-26 | 新地能源工程技术有限公司 | A kind of sepiolite-alumina composite carrier and the high temperature sintering resistant type methanation catalyst using it |
| CN109675543B (en) * | 2018-12-17 | 2022-01-25 | 新地能源工程技术有限公司 | Sepiolite-alumina composite carrier and high-temperature sintering resistant methanation catalyst using same |
| CN112717926A (en) * | 2019-10-28 | 2021-04-30 | 中国石油化工股份有限公司 | Catalyst for producing hydrogen peroxide by anthraquinone hydrogenation and preparation method and application thereof |
| CN114100608A (en) * | 2021-12-20 | 2022-03-01 | 河北工业大学 | Preparation method of thermal modified sepiolite mineral loaded Rh monatomic catalyst |
| CN114100608B (en) * | 2021-12-20 | 2023-11-28 | 河北工业大学 | Preparation method of heat modified sepiolite group mineral loaded Rh single-atom catalyst |
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