A molybdenum phosphide catalyst used for gas phase selective hydrodechlorination for preparing 2,3,3,3-tetrafluoropropene

A molybdenum phosphide catalyst and selective hydrogenation technology, which is applied in the direction of physical/chemical process catalysts, molecular sieve catalysts, dehydrohalogenation preparation, etc., can solve the problems of reduced selectivity of target products, increased reaction process costs, etc., and achieve high temperature resistance to sintering The effect of good ability and low cost of raw materials

Active Publication Date: 2019-07-05
XIAN MODERN CHEM RES INST
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Problems solved by technology

However, in the preparation methods disclosed in these several patents, although 1,1-dichloro-2,3,3,3-tetrafluoropropene or 1-chloro-2,3,3,3-tetrafluoropropene can be directly mixed with hydrogen One-step reaction to prepare 2,3,3,3-tetrafluoropropene, but in the actual reaction process, the double bond in the raw material compound will preferential...

Method used

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  • A molybdenum phosphide catalyst used for gas phase selective hydrodechlorination for preparing 2,3,3,3-tetrafluoropropene
  • A molybdenum phosphide catalyst used for gas phase selective hydrodechlorination for preparing 2,3,3,3-tetrafluoropropene
  • A molybdenum phosphide catalyst used for gas phase selective hydrodechlorination for preparing 2,3,3,3-tetrafluoropropene

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Experimental program
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Effect test

Embodiment 1

[0022] Embodiment 1: Preparation of MoP / oxide (fluoride or molecular sieve) catalyst

[0023] At room temperature, 3.52 g of ammonium heptamolybdate ((NH 4 ) 6 Mo 7 o 24 4H 2 O) and 2.63g diammonium hydrogen phosphate ((NH 4 ) 2 HPO 4 ) was added to 20 mL of deionized aqueous solution, and then the pH of the solution was adjusted to 2-3 with concentrated nitric acid to obtain a clear solution. According to the loading of 0.5%, 5%, 10%, 20%, and 30%, the above solutions are impregnated onto a certain mass of oxides, fluorides, or molecular sieves, and then aged at room temperature for 12 hours, dried at 120 ° C for 12 hours to dry the water, and Calcined at 500°C for 6h to obtain the oxide precursor of supported MoP. The phosphide catalyst was prepared by in-situ temperature-programmed reduction method. The temperature programming step mainly includes two steps: (1) in H 2 Under the atmosphere (flow rate 150mL / min), the temperature was raised from room temperature to ...

Embodiment 2

[0024] Embodiment 2: preparation MoP / activated carbon catalyst

[0025] At room temperature, 3.52 g of ammonium heptamolybdate ((NH 4 ) 6 Mo 7 o 24 4H 2 O) and 2.63g diammonium hydrogen phosphate ((NH 4 ) 2 HPO 4 ) was added to 20 mL of deionized aqueous solution, and then the pH of the solution was adjusted to 2-3 with concentrated nitric acid to obtain a clear solution. According to the loads of 5%, 10%, 20%, and 30%, the above solutions were impregnated on a certain mass of activated carbon, and then aged at room temperature for 12 hours, dried at 120°C for 12 hours, and baked at 500°C for 3 hours in a nitrogen atmosphere. Oxide precursors of MoP supported on activated carbon were obtained. The phosphide catalyst was prepared by in-situ temperature-programmed reduction method. The temperature programming step mainly includes two steps: (1) in H 2 Under the atmosphere (flow rate 150mL / min), the temperature was raised from room temperature to 120°C at 5°C / min, and k...

Embodiment 3

[0026] Example 3: Preparation of surface sulfur-modified molybdenum phosphide-supported activated carbon catalyst

[0027] Using the molybdenum phosphide loaded activated carbon catalyst obtained in Example 2, after the sample temperature program reduction was completed, the temperature was lowered to 400 ° C, and the H 2 Switch to containing 10% (volume fraction) H 2 S / H 2 . The sulfidation treatment was continued for 3 hours, and the surface sulfur-modified molybdenum phosphide-supported activated carbon catalyst was obtained, and the active phase was denoted as MoP-S.

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Abstract

A molybdenum phosphide catalyst used for gas phase selective hydrodechlorination of 2-chloro-1,1,1,2-tetrafluoro propane to prepare 2,3,3,3-tetrafluoropropene, in order to solve a problem that traditional chlorofluorocarbon hydrodechlorination catalysts are high in cost and liable to deactivate. The catalyst includes bulk phase MoP or MoP/carrier, wherein the active component MoP is formed by combining metal molybdenum and non-metal element phosphorus to form the molybdenum phosphide covalent compound having a crystal structure, the MoP is subjected to surface modification through a sulfuration manner to obtain the compound. The catalyst has advantages of excellent performance, high activity, good stability, low reaction temperature, capability of effectively reducing reaction energy consumption, and industrial application value.

Description

technical field [0001] The invention relates to a catalyst, in particular to a catalyst for preparing 2,3,3,3-tetrafluoropropene by gas-phase selective hydrogenation dechlorination. It belongs to multiple catalytic technical fields. Background technique [0002] 2,3,3,3-tetrafluoropropene, referred to as HFO-1234yf, the molecular formula is CF 3 CF=CH 2 , non-toxic, non-flammable, ODP is zero, and GWP is about 4. It is considered to be an ideal substitute for HFC-134a and one of the most promising fourth-generation low-carbon refrigerants. [0003] So far, among the many known synthetic methods of HFO-1234yf, 1,1,2,3-tetrachloropropene and anhydrous hydrogen fluoride are mainly used as raw materials to generate the target product through three-step synthesis (Chinese patent CN102603465.A). The final step is dehydrochlorination by 2-chloro-1,1,1,2-tetrafluoropropane (HCFC-244bb) in the presence of a catalyst. Literature (ChemCatChem 2017, 9,824–832) and patent (US8058486B...

Claims

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Application Information

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IPC IPC(8): B01J27/19B01J29/48B01J37/02B01J37/18B01J37/20C07C17/25C07C21/18
CPCB01J27/19B01J29/48B01J37/0201B01J37/18B01J37/20C07C17/25C07C21/18
Inventor 田松吕剑贾兆华秦越马辉李晨王博毛伟白彦波
Owner XIAN MODERN CHEM RES INST
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