Preparation method of catalyst for synthesizing allyl acetate

A technology of allyl acetate and catalyst, which is applied in the field of preparation of catalysts for the synthesis of allyl acetate, can solve the problems of low space-time yield and selectivity, and achieve improved space-time yield and selectivity, good dispersibility, The effect of good technical effects

Active Publication Date: 2014-06-25
CHINA PETROLEUM & CHEM CORP +1
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AI-Extracted Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by this invention is the problem that the space-time yield and selectivity of synthetic allyl acetate catalyst are lower in the prio...
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Abstract

The invention relates to a preparation method of a catalyst for synthesizing allyl acetate, and mainly overcoming the problems of low space time yield and selectivity of a conventional catalyst for allyl acetate. The preparation method of the catalyst for synthesizing allyl acetate comprises the following steps of (a) impregnating a carrier in a solution dissolving a palladium-containing compound and a copper-containing compound to obtain a catalyst precursor I; (b) treating the catalyst precursor I with an alkali solution to obtain a catalyst precursor II; (c) impregnating the catalyst precursor I in a solution containing a stabilizer to obtain a catalyst precursor III, wherein the stabilizer is polyvinyl pyrrolidone or polyacrylic acid alkali metal salt or a mixture of the above two; (d) reducing the catalyst precursor III by using a reducing agent to obtain a catalyst precursor IV; and (e) impregnating the catalyst precursor IV with an alkali metal acetate solution, drying to obtain a finished product of the catalyst. By adopting the above technical solution, the problems are overcome relatively well; and the preparation method can be used for industrial production of allyl acetate.

Application Domain

Organic compound preparationOrganic-compounds/hydrides/coordination-complexes catalysts +2

Technology Topic

Allyl acetateAcetate salt +11

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  • Preparation method of catalyst for synthesizing allyl acetate

Examples

  • Experimental program(2)
  • Comparison scheme(2)

Example Embodiment

[0014] [Example 1]
[0015] (1) Catalyst preparation
[0016] Step (a): Take 1200ml of an aqueous solution containing chloropalladic acid and copper chloride as the immersion solution, where the palladium content in the solution is 2.75g/L, the copper content is 0.625 g/L, and the immersion solution is 1100ml with a diameter of 4-6mm Spherical silica support obtains catalyst precursor I;
[0017] Step (b): Add 27.5 g of sodium silicate nonahydrate to 100 ml of aqueous solution and add it to the catalyst precursor I, mix well, let stand for 24 hours, and then dry at 80°C for 8 hours to prepare the catalyst precursor II;
[0018] Step (c): Take 100 ml of an aqueous solution containing polyvinylpyrrolidone (weight-average molecular weight of 360,000), wherein the content of polyvinylpyrrolidone is 100g/L, impregnate the catalyst precursor II to obtain the catalyst precursor III;
[0019] Step (d): reducing the catalyst precursor III in a hydrogen atmosphere, the hydrogen flow rate is 0.2 ml/min, the pressure is 0.5Mpa, and the reduction temperature is 200°C to obtain the catalyst precursor IV;
[0020] Step (e): immerse the potassium acetate aqueous solution to make the potassium acetate content 50g/L, and dry to obtain the finished catalyst.
[0021] For comparison, the preparation conditions of the catalyst are listed in Table 1.
[0022] (2) Catalyst characterization
[0023] An X-ray diffractometer was used to analyze and characterize the palladium-gold crystal grain size in the catalyst, and an inductively coupled plasma spectrometer (ICP) was used to measure the content of each element in the catalyst. The data obtained are listed in Table 2.
[0024] (3) Catalyst evaluation
[0025] Evaluation with fixed bed reactor, the specific conditions are:
[0026] Catalyst filling volume: 400ml;
[0027] The composition of the reaction raw materials (in terms of mole percentage): 41% propylene, 43% nitrogen, 10% acetic acid and 6% oxygen;
[0028] Raw material volumetric space velocity: 2000hr -1;
[0029] Reaction pressure: 0.7MPa;
[0030] Reaction temperature: 140°C;
[0031] Response time: 500hr;
[0032] Analyze the content of each component in the reaction product by gas chromatography, and then calculate the space-time yield of the catalyst. The experimental data obtained are listed in Table 2.

Example Embodiment

[0033] [Example 2] to [Example 11]
[0034] In addition to the type of palladium-containing compound and copper-containing compound, the content of palladium-containing compound and copper-containing compound, the type of stabilizer, the concentration of stabilizer, the weight average molecular weight of stabilizer, the weight ratio of stabilizer, the type of reducing agent and the reduction Except for the temperature change, the other steps are the same as in Example 1. For comparison, the preparation conditions of the catalyst are listed in Table 1, and the physical properties of the catalyst and the space-time yield and selectivity data of the catalyst are listed in Table 2.

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