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Method for catalytic oxidation of tert-butanol

A technology for catalytic oxidation and tert-butanol, used in chemical instruments and methods, preparation of peroxy compounds, preparation of organic compounds, etc.

Active Publication Date: 2012-05-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no relevant report on the application in the oxidation of tert-butanol

Method used

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  • Method for catalytic oxidation of tert-butanol
  • Method for catalytic oxidation of tert-butanol
  • Method for catalytic oxidation of tert-butanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] Take 20 grams of titanium silicon molecular sieve TS-1, the ammonium nitrate palladium complex solution with a concentration of 0.01g / ml (based on palladium atoms), and an appropriate amount of hydrazine hydrate and cetyltrimethylammonium bromide and add to the tetrapropyl Stir and mix uniformly in an aqueous solution of ammonium hydroxide (10% by mass), in which titanium silicon molecular sieve (g): cetyltrimethylammonium bromide (mole): tetrapropylammonium hydroxide (mole): hydrated Hydrazine (mole): ammonium nitrate palladium complex (g, in terms of palladium): water (mole)=100:0.005:0.5:3.0:2.0:1000. Then it was put into a stainless steel sealed reactor and hydrothermally treated at a temperature of 150°C and autogenous pressure for 48 hours. The resultant was filtered, washed with water, dried naturally, and dried at 180°C for 3 hours to obtain micropores containing precious metals. Titanium silicon material A. After characterization, its composition can be express...

Embodiment 2

[0076] Take 20 grams of titanium silicon molecular sieve TS-1, a palladium chloride solution with a concentration of 0.01g / ml (based on palladium atoms), and an appropriate amount of hydrazine hydrochloride and polypropylene, add them to the aqueous solution of sodium hydroxide (15% by mass) and stir. Mix uniformly, wherein titanium silicate molecular sieve (g): polypropylene (mole): sodium hydroxide (mole): hydrazine hydrochloride (mole): palladium chloride (g, in terms of palladium): water (mole) = 100: 0.9: 1.8:0.15:0.1:4600. Then it was put into a stainless steel sealed reactor and hydrothermally treated for 24 hours at a temperature of 180°C and autogenous pressure. The resultant was filtered, washed with water, dried naturally, and dried at 110°C for 3 hours to obtain micropores containing precious metals. Titanium silicon material B. After characterization, its composition can be expressed as 8TiO in the form of oxide 2 ·100SiO 2 ·0.006PdO·0.008Pd, its low-temperature n...

Embodiment 3

[0078] Add tetraethyl orthosilicate, tetrabutyl titanate, a palladium acetate solution with a concentration of 0.01g / ml (based on palladium atoms) and Tween 80 to the aqueous solution of tetrapropylammonium hydroxide and butanediamine (quality The percentage concentration is 10%), stir and mix uniformly, where the molar composition is silicon source: titanium source: tetrapropyl ammonium hydroxide: butanediamine: palladium source: protective agent: water = 100:0.03:0.5:0.1:0.05: 0.02:550, silicon source is SiO 2 Calculated, the titanium source is TiO 2 The palladium source is calculated as Pd. Then, it is put into a sealed reactor, and hydrothermally treated at a temperature of 120° C. and autogenous pressure for 120 hours. The resultant is taken out, filtered, dried, and calcined to obtain an intermediate crystalline material. Transfer the intermediate crystalline material to the remaining filtrate, add an appropriate amount of hydrazine hydrate, and hydrothermally heat it at ...

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Abstract

The invention discloses a method of t-butanol catalytic oxidation, which is characterized in that t-butanol, solvent, oxygen, hydrogen and diluent gas at a mole ratio of 1:(0-80):(0.2-20):(0.1-10):(0-100) react in the presence of a catalyst under 0.1-3.0MPa<1> at 0-180 DEG C. The catalyst is a microporous titanium-silicon material or a compound containing the microporous titanium-silicon material. The composition of the microporous titanium-silicon material is expressed as xTiO2*100SiO2*yEmOn*zE with an oxide form, wherein x ranges from 0.001 to 50.0; the sum of y plus z ranges from 0.005 to 20.0; the ratio of y to z is smaller than 1; E is one or more metal noble metals selected from Ru, Rh, Pd, Re, Os, Ir, P and Au; m and n are numbers required for meeting the oxidation state of E; and material grains are partially or totally hollow-structured. The method has the advantages of high t-butyl hydroperoxide selectivity and good product activity stability, and facilitates industrial production and application.

Description

Technical field [0001] The present invention relates to a method for oxidizing tert-butanol, and further relates to a method for catalyzing the oxidation of tert-butanol by using a microporous titanium silicon material containing precious metals as a catalyst. Background technique [0002] Tert-butyl hydroperoxide, also known as tert-butyl peroxide (English name is Tert-buty1 HydrogenPeroxide, abbreviated as: TBHP), is widely used in vinyl monomer polymerization and copolymerization initiator, natural raw rubber and sulfur, improve diesel fuel Cetane number, tert-butyl peroxide group introduction agent, can also be used as a crosslinking agent for unsaturated polyesters at moderate and high temperatures. [0003] Nowadays, the industrial production of t-butyl hydrogen peroxide is mainly obtained by using sulfuric acid as a catalyst and hydrogen peroxide as an oxidizing agent to catalyze and oxidize tert-butyl alcohol. This method has equipment corrosion and harmful emissions, whic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C409/04C07C407/00
Inventor 林民史春风龙军朱斌舒兴田慕旭宏罗一斌汪燮卿汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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