Silicon tungsten, phosphorus heteropoly tungstic acid load type catalyzer used for esterification reaction, manufacturing method and application thereof

A supported catalyst, phosphotungstic heteropolyacid technology, applied in physical/chemical process catalysts, molecular sieve catalysts, preparation of organic compounds, etc., can solve problems such as unsatisfactory ester yield and long reaction time

Inactive Publication Date: 2008-01-23
BEIJING INSTITUTE OF CLOTHING TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

To achieve higher yields of esters, the required reaction time is v

Method used

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  • Silicon tungsten, phosphorus heteropoly tungstic acid load type catalyzer used for esterification reaction, manufacturing method and application thereof
  • Silicon tungsten, phosphorus heteropoly tungstic acid load type catalyzer used for esterification reaction, manufacturing method and application thereof
  • Silicon tungsten, phosphorus heteropoly tungstic acid load type catalyzer used for esterification reaction, manufacturing method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 10%SiW 12 Preparation of / beta zeolite catalyst

[0023] Weigh silicotungstic acid H with Keggin structure 3 SiW 12 o 40 xH2O 2g, dissolved in deionized water, weighed 18g of Hβ zeolite roasted at 400°C for 2 hours, (wherein Na 2 O≤0.2wt.%, total acid≥4.0×10 20 Sites / g, specific surface 607m 2 / g, the crystal grain is about 0.2μm), mixed with silicotungstic acid solution, the impregnation medium is deionized water, and the liquid-solid ratio (ratio of impregnation solvent volume to carrier mass) is 2.5ml / g. Shake and impregnate continuously in a constant temperature oscillator under normal temperature and pressure, carry out temperature program drying after 24 hours, rise to 120°C in 10 hours, continue drying at 120°C for 2 hours, and roast at 200°C for 2 hours to obtain 10% SiW 12 / beta zeolite catalyst. The obtained catalyst was characterized by IR and XRD, and the curve 9 in Fig. 2 is the IR spectrum of the catalyst. Since Keggin-type heteropolyacids have cha...

Embodiment 2

[0025] 20%SiW 12 Preparation of / beta zeolite catalyst

[0026] The amount of silicotungstic acid is 2g, the amount of Hβ zeolite is 8g, and the rest of the processing conditions and proportions are the same as in Example 1, that is, 20% SiW 12 / beta zeolite catalyst. Curve B in Figure 4 is the XRD pattern of the catalyst. In the figure, it can be observed that the XRD of the carrier Hβ zeolite has characteristic diffraction peaks at 2θ of 7.8°, 13.6°, 21.41°, 22.43°, 26.92°, and 29.60°. Dispersed on the surface of silica gel, so Keggin-type heteropolyacid characteristic diffraction peaks cannot be observed.

Embodiment 3

[0028] 30%SiW 12 Preparation of / beta zeolite catalyst

[0029] The amount of silicotungstic acid is 3g, the amount of Hβ zeolite is 7g, and the remaining processing conditions and proportions are the same as in Example 1, that is, 30% SiW 12 / beta zeolite catalyst. Curve C in Figure 4 is the XRD pattern of the catalyst. In addition to the characteristic diffraction peaks at 2θ of 7.8°, 13.6°, 21.41°, 22.43°, 26.92°, and 29.60° in the XRD of the carrier Hβ zeolite, due to the increase in loading, the Keggin structure heteropolyacid Characteristic peaks began to appear, and four characteristic peaks at 2θ of 8.28°, 8.90°, 10.27° and 28.9° were observed. Thanks to SiW 12 The interaction with the carrier makes the diffraction peaks of the carrier between 2θ=10-60° become diffuse or disappear. For example, the XRD diffraction peak at 7.8° appears branched, which is obviously the heteropoly acid at 8.28°. XRD diffraction peaks. These spectra show that SiW 12 It is highly dis...

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Abstract

The invention is a silicotungstic and phosphotungstic heteropoly acid load catalyst used for esterification reaction, which comprises the following components: Keggin structure silicotungstic acid H3SiW12O40.xH2O and phosphotungstic H3PW12O40.xH20, the content occupies 10 to 50 quality per centage of the amount of the catalyst; the carrier is H Beta zeolite. The invention adopts soaking method to prepare the solid silicotungstic and phosphotungstic heteropoly acid catalyst load on the H Beta zeolite, which can be used for catalyzing the esterification reaction of etic acid, isobutanol, isobutanol and ethanol, but also can be used for catalyzing esterification reaction of lactic acid and isobutanol to synthesis n-butyl acetate, isobutyl acetate, ethyl acetate and N-Butyl Lactate. The invention has the advantages of good stability, high activity and good selectivity, but also can used as inhomogeneous catalyst which is easy to be separated with reaction product and can use the prepared and formed catalyst powder in the continuous operating fixed bed reactor. The invention is used in the techinics of esterification reaction catalyzing rectifying.

Description

technical field [0001] The invention relates to a silicon tungsten and phosphotungstic heteropolyacid supported catalyst used for esterification in the field of organic synthesis, a preparation method and application. technical background [0002] Carboxylate is a kind of basic organic chemical raw material, which is widely used in spices, flavors, plasticizers, solvents, resins, paints, cosmetics, medicines, surfactants and organic synthesis intermediates, etc., and has a broad market at home and abroad need. At present, organic acids and alcohols are used in industry as raw materials, and concentrated sulfuric acid is used as a catalyst to synthesize them through batch reactions. The use of concentrated sulfuric acid as an esterification catalyst has the disadvantages of corroding equipment, polluting the environment, and long post-treatment procedures. Therefore, replacing traditional catalysts for esterification with solid catalysts has become an important field of cata...

Claims

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Application Information

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IPC IPC(8): B01J29/076B01J27/188C07C67/08
Inventor 杜迎春
Owner BEIJING INSTITUTE OF CLOTHING TECHNOLOGY
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