Preparation method of polynuclear metal phthalocyanine alkane oxidation catalyst

A technology for oxidation catalysts and phthalocyanine alkanes, which is applied in the direction of physical/chemical process catalysts, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., can solve problems such as high raw material costs and complicated preparation processes, Achieve the effects of low preparation cost, simplify the preparation process, and alleviate pollution

Active Publication Date: 2013-01-02
SHANDONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The yield of the product obtained by this method is higher, but the preparation process is complicated, and the raw material cost is higher

Method used

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  • Preparation method of polynuclear metal phthalocyanine alkane oxidation catalyst
  • Preparation method of polynuclear metal phthalocyanine alkane oxidation catalyst
  • Preparation method of polynuclear metal phthalocyanine alkane oxidation catalyst

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preparation example Construction

[0032] The preparation method of polynuclear metal phthalocyanine is carried out according to the following steps: urea, phthalic anhydride or substituted phthalic anhydride, pyromellitic anhydride, and metal sources in a certain molar ratio are used as raw materials, and ammonium molybdate is used as a catalyst , with ammonium chloride as a synthetic additive, high-boiling alkanes, alkylbenzenes or their mixtures as solvents, liquid-phase reaction → suction filtration → boiling (distilled water, dilute acid, dilute alkali, etc.) → crude catalyst product → Soxhlet Extraction→drying→finished catalyst.

[0033] The structural general formula of above-mentioned polynuclear metal phthalocyanine is as shown in formula (I), wherein: n=0,1,2...; when n=0, i=none, when n≥1, i=2,3 ...(n+1), that is, all integers between 2 and (n+1); M is the metal as the active center; X is the peripheral substituent; Y is the non-peripheral substituent; L is the axial ligand .

[0034] The structura...

Embodiment 1

[0037] Binuclear iron-iron phthalocyanine alkane oxidation catalyst (general structural formula is shown in formula (I), wherein, n=0; M 1 = M 2 =Fe;X=Y=H,H;L 1 ~ L 4 = none) is prepared in the following steps:

[0038] Step 1: Mix 15g of phthalic anhydride, 19g of urea, 3.7g of tetrahydrate and ferrous chloride, 2.7g of pyromellitic anhydride, 0.5g of ammonium molybdate catalyst, 2.1g of ammonium chloride additive and grind them evenly , Add 100ml decahydronaphthalene solvent to obtain a reaction mixture. Firstly, the temperature of the reaction mixture was raised to 150° C., reacted for 30 minutes, then raised to the boiling point of the solvent, maintained at the boiling point for 4 hours, and then cooled to 80° C. to obtain a product mixture.

[0039] The second step: the product mixture is suction filtered, and the solvent is recovered to obtain a primary filter cake. Boil the primary filter cake with distilled water, dilute hydrochloric acid, and dilute NaOH solutio...

Embodiment 2

[0042] Trinuclear iron-iron-iron phthalocyanine alkane oxidation catalyst (structure general formula is shown in formula (I), wherein, n=1; M 1 = M 2 = M 3 =Fe;X=Y=H,H;L 1 ~ L 6 = none) is prepared in the following steps:

[0043] Step 1: Mix 18g of phthalic anhydride, 29g of urea, 5.6g of tetrahydrate and ferrous chloride, 5.4g of pyromellitic anhydride, 0.8g of ammonium molybdate catalyst, 2.1g of ammonium chloride additive and grind them evenly , Add 100ml decahydronaphthalene solvent to obtain a reaction mixture. Firstly, the temperature of the reaction mixture was raised to 150° C., reacted for 30 minutes, then raised to the boiling point of the solvent, maintained at the boiling point for 4 hours, and then cooled to 80° C. to obtain a product mixture.

[0044] The second step: the product mixture is suction filtered, and the solvent is recovered to obtain a primary filter cake. Boil the primary filter cake with distilled water, dilute hydrochloric acid, and dilute ...

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Abstract

The invention relates to a preparation method of a polynuclear metal phthalocyanine alkane oxidation catalyst. The preparation method comprises steps of: using phthalic anhydride or substituted phthalic anhydride, urea, pyromellitic dianhydride and metal sources in a certain molar ratio as raw materials; reacting in a high boiling point solvent; and then conducting acid digestion, alkali cooking, washing, suction filtration, Soxhlet extraction and drying to obtain the polynuclear metal phthalocyanine. Compared with the disclosed preparation method of polynuclear metal phthalocyanine, the method provided by the invention has simple process, yield of finished catalyst product higher than 60%, little volatile solvent and solid waste emission. The catalyst has a raw material conversion rate no less than 10%, if applied to the catalytic oxidation process of butane and hexane, and has a broad application prospect in the field of catalysis of alkane oxidation.

Description

technical field [0001] The invention relates to a method for preparing a polynuclear metal phthalocyanine alkane oxidation catalyst. Background technique [0002] Polynuclear metallophthalocyanines have very broad application prospects in the field of catalyzing the oxidation of low-carbon alkanes. Because of this, the research on the preparation of polynuclear metallophthalocyanines has general significance. [0003] The preparation method of the polynuclear metal phthalocyanine disclosed at present mainly contains one-step method and two-step method two classes, specifically there are following three kinds of methods: (1) urea-phthalic anhydride melting method, this method is based on phthalic anhydride , urea, pyromellitic anhydride and metal sources as the main raw materials, carry out solid phase reaction to obtain polynuclear metal phthalocyanine. The reaction temperature of this method is generally higher (usually more than 250 ℃), the consumption of urea is larger (...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/22B01J31/22
Inventor 王志亮高文斌张效龙
Owner SHANDONG UNIV OF SCI & TECH
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