Preparation method for substituted molybdophosphate crystal catalyst

A technology of phosphate crystals and catalysts, which is applied in the chemical field, can solve the problems of difficult recovery of catalysts, harsh reaction conditions, and easy pollution, and achieve the effects of low cost, mild reaction process conditions, and easy recovery

Inactive Publication Date: 2011-10-19
HARBIN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation of propylene carbonate by the cycloaddition method needs to be reacted at high temperature (170-210°C) and high pressure (6.0-12.0Mpa). Th

Method used

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Effect test

Embodiment 1

[0021] A kind of preparation method of substituted molybdophosphate crystal catalyst, this method is divided into two steps, the first step, sodium molybdate Na 2 MoO 4 2H 2 O, transition metal sulfate, phosphoric acid H3PO4 and 1,3-2 (4-pyridyl)-propane or ethylenediamine are mixed in water with a mole fraction of 2000 in a ratio of 6:2.9:30:2.6 , and stirred for 30 minutes to obtain a mixed solution; in the second step, the mixed solution obtained in the first step was sealed in a stainless steel reactor lined with polytetrafluoroethylene, and the filling degree was 60-70%, and then the reactor was placed in 165°C Heating and crystallizing in an oven for 7 days, and then naturally cooling to room temperature, the dark red polyacid crystal catalyst was obtained.

Embodiment 2

[0023] The preparation method of the substituted type molybdophosphate crystal catalyst described in embodiment 1, with 1.45 gram of sodium molybdate Na 2 MoO 4 2H 2 O, 0.52 g zinc sulfate ZnSO 4 ·H 2 O, 2 mL H 3 PO 4 , 0.38 grams of 1,3-2 (4-pyridyl)-propane was mixed in 36 milliliters of water, stirred at room temperature for 30 minutes, and the resulting mixed solution was sealed in a stainless steel reactor lined with polytetrafluoroethylene, and the filling degree was 65%. Then put the reaction kettle into a 165°C oven and heat it for 7 days, then cool it naturally to room temperature to obtain a deep red massive polyacid crystal catalyst; the polyacid crystal catalyst is a pure compound, and its chemical formula is

[0024] (H 2 bpp) 3 [Zn 3 Mo 12 VO 24 (OH) 8 (HPO 4 ) 6 (PO 4 ) 2 ]·2H 2 O) bpp = 1,3-2(4-pyridyl)-propane).

Embodiment 3

[0026]The preparation method of the substituted type molybdophosphate crystal catalyst described in embodiment 1, with 1.45 gram of sodium molybdate Na 2 MoO 4 2H 2 O, 0.56 g ferrous sulfate FeSO 4 ·H 2 O, 2 mL phosphoric acid H 3 PO 4 , 0.32 g of ethylenediamine was mixed in 36 ml of water, stirred at room temperature for 30 minutes, the resulting mixture was sealed in a stainless steel reactor lined with polytetrafluoroethylene, and the filling degree was 65%, and then the reactor was placed in a 165°C oven Heating at a constant temperature for 7 days, and then naturally cooling to room temperature, obtained the dark red massive polyacid crystal catalyst; the polyacid crystal catalyst is a pure compound, and its chemical formula is

[0027] (H 2 en) 3 (Hen)[Fe III 3 Mo 12 V o 24 (OH) 8 (HPO 4 ) 4 (PO 4 ) 4 ]·3H 2 O (en = ethylenediamine).

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Abstract

The invention relates to a preparation method for a substituted molybdophosphate crystal catalyst. The design and synthesis of a high-activity, selective, environmentally-friendly and recyclable catalyst have an important significance in the research and chemical industry fields. The preparation method provided by the invention comprises two steps: step one, mixing sodium molybdate Na2MoO4.2H2O, transition metal sulfate, phosphoric acid H3PO4 and 1,3-bis(4-pyridyl)-propane or ethylene diamine at a molar ratio of 6: 2.9: 30: 2.6 in water with the molar fraction of 2000 and stirring for 30 minutes to obtain a mixed liquid; and step two, enclosing the mixed liquid obtained in the step one in a polytetrafluoroethylene-lined stainless steel reaction kettle at a filling degree of 60-70%, then placing the reaction kettle in a 165 DEG C oven to heat and crystallize for 7 days, and then naturally cooling to room temperature to obtain the dark red polyacid crystal catalyst. The preparation method can be used for preparing the substituted molybdenum phosphate crystal catalyst.

Description

Technical field: [0001] The invention relates to a method for use in the chemical field, in particular to a preparation method for a substituted molybdophosphate crystal catalyst. Background technique: [0002] Designing and synthesizing catalysts with high activity, selectivity, environmental friendliness and recyclability is of great significance in both scientific research and chemical industry. Polyoxometalates have strong acidity, rich redox properties, and are non-toxic and non-corrosive. They are widely used in reactions such as olefin hydration, esterification and hydrolysis, alkylation, and olefin epoxidation. Used as a catalyst. Their composition, structure, acidity, and redox properties are variable and adjustable, making them ideal materials for molecular models in theoretical studies of catalytic chemistry and for artificial molecular design of catalysts. In addition, propylene carbonate is an important chemical raw material with a wide range of uses. Its mon...

Claims

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Application Information

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IPC IPC(8): B01J31/36C07D317/36
CPCY02P20/584
Inventor 于凯高嵩周百斌
Owner HARBIN NORMAL UNIVERSITY
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