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Catalyst for preparation of 2,3,3,3-tetrafluoropropene through selective hydrodechlorination

A technology of tetrafluoropropene and hydrodechlorination, which is applied in the fields of dehydrohalogenation preparation, physical/chemical process catalyst, organic chemistry, etc., can solve the problems of high reaction temperature, unavailable raw materials, increased production cost, etc. Good sintering ability, low raw material cost, and long service life

Active Publication Date: 2019-07-12
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Literature (ChemCatChem 2017, 9,824) and patent (US8058486B2) report that this step of reaction often requires a higher reaction temperature, which not only consumes high energy, but also easily leads to carbon deposition to quickly deactivate the catalyst, and has low industrial application value.
[0004] Chinese patents CN108178719.A, CN102947255.A, and CN102947254.A disclose 1,1-dichloro-2,3,3,3-tetrafluoropropene or 1-chloro-2,3,3,3-tetrafluoropropene as The raw material compound adopts the process of hydrodechlorination to prepare HFO-1234yf, but the active component of the catalyst used is the noble metal palladium, the raw material is not easy to obtain, and the catalyst is expensive, resulting in increased production costs
[0006] At present, the process of preparing HFO-1234yf by selective hydrodechlorination has the problems of unavailable raw materials and expensive catalysts

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] According to the Co / P molar ratio of 1 / 1, 7.65g of cobalt nitrate and 3.45g of diammonium hydrogen phosphate were weighed and added to the deionized aqueous solution, and then the pH of the solution was adjusted to 2-3 with concentrated nitric acid to obtain a clear solution. An equal volume of the above solution was impregnated onto 7.9g of silica, then aged at room temperature for 12h, dried at 120°C for 12h to dry the water, and baked at 500°C for 6h to obtain CoP / SiO with a loading capacity of 30%. 2 oxide precursors. 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 kept at 120°C for 1h to drive off the water adsorbed by the catalyst; (2) from 120°C to 120°C at a rate of 5°C / min 400°C, then raise the temperature from 400°C to 650°C at 1°C / m...

Embodiment 2

[0025] According to the Co / P molar ratio of 2 / 1, 15.2g of cobalt nitrate and 3.45g of diammonium hydrogen phosphate were weighed and added to the deionized aqueous solution, and then the pH of the solution was adjusted to 2-3 with concentrated nitric acid to obtain a clear solution. The same volume of the above solution was impregnated onto 11.5g of activated carbon, then aged at room temperature for 12h, dried at 120°C for 12h to dry the water, and dried under N 2 Calcined at 500 °C for 6 h under atmosphere to obtain Co with a loading of 30% 2 P / C oxide precursor. 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 kept at 120°C for 1h to drive off the water adsorbed by the catalyst; (2) from 120°C to 120°C at a rate of 5°C / min 400°C, then raise the te...

Embodiment 3

[0027] According to the Fe / P molar ratio of 1 / 1, weigh 10.6g of ferric nitrate and 3.45g of diammonium hydrogen phosphate and add them to the deionized aqueous solution, then use concentrated nitric acid to adjust the pH of the solution to 2-3 to obtain a clear solution. An equal volume of the above solution was impregnated onto 7.71g of magnesium fluoride, then aged at room temperature for 12h, dried at 120°C for 12h to dry the water, and baked at 500°C for 6h to obtain FeP / MgF with a loading capacity of 30%. 2 oxide precursors. 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 kept at 120°C for 1h to drive off the water adsorbed by the catalyst; (2) from 120°C to 120°C at a rate of 5°C / min 400°C, then raise the temperature from 400°C to 650°C at 1°C / ...

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Abstract

The invention discloses a catalyst for preparation of 2,3,3,3-tetrafluoropropene through hydrodechlorination. The problem of high cost and easy deactivation of a traditional chlorofluorocarbon hydrodechlorination catalyst are solved. The catalyst has the characteristics that the catalyst is composed of an active component and a carrier, wherein the active component is MxPy, and MxPy is one or combination of more of PdP, Co2P, CoP and FeP. The catalyst has excellent performance, high activity, good stability and low reaction temperature, the reaction energy consumption can be reduced effectively, and an industrial application value is achieved.

Description

technical field [0001] The invention relates to a catalyst, in particular to a catalyst for preparing 2,3,3,3-tetrafluoropropene. 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) and patent (US8058486B2) report that this step reaction often requires a highe...

Claims

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Application Information

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IPC IPC(8): B01J27/185C07C17/25C07C21/18
CPCB01J27/1853B01J27/1856C07C17/25C07C21/18
Inventor 田松吕剑王博秦越马辉李晨毛伟白彦波贾兆华
Owner XIAN MODERN CHEM RES INST
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