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A kind of method that formaldehyde aqueous solution and acetic acid synthesize acrylic acid

A technology of formaldehyde aqueous solution and acrylic acid, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate, etc., to achieve the effect of low process raw materials, mild production process and simple preparation process

Active Publication Date: 2017-02-08
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the current average operating rate of acetic acid plants is only 60%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: the preparation of the catalyst carrier containing molecular sieve

[0025] Take 30 grams of ZSM-5 molecular sieve with a silicon-aluminum ratio of 70, 100 grams of pseudo-boehmite powder, 5.2 grams of scallop powder, and 15 grams of SB aluminum hydroxide powder, mix well and set aside; take 5 grams of polyvinyl alcohol, Dissolve in 200 milliliters of 10wt% nitric acid solution under heating and stirring, and knead the solution and the mixed powder to form a plastic paste, then extrude into strips, dry at 120°C for 12 hours and roast at 550°C for 5 hours to obtain Catalyst carrier of molecular sieve ZSM-5.

[0026] By changing the type of molecular sieve added, catalyst supports containing different molecular sieves can be prepared.

Embodiment 2

[0027] Example 2: Preparation of phosphorus pentoxide-cesium oxide composite catalytic material supported by Y molecular sieve

[0028] Add a certain amount of diammonium hydrogen phosphate into deionized water, and after fully dissolving, add the measured cesium carbonate and fully dissolve to form a clear and transparent solution.

[0029] Weigh the quantitative Y molecular sieve, place it in a vacuum device, keep it under the vacuum degree of 0.1MPa for 1 hour, and add the impregnation solution containing ammonium dihydrogen phosphate and cesium carbonate under this vacuum degree, and after the Y molecular sieve is completely impregnated, put It was moved into a sonotrode and continued to immerse for 12 hours under 80HKz ultrasonic conditions.

[0030] Put the above impregnated body in the roasting equipment, heat to 120°C for 6 hours at a heating rate of 5°C / min in an air atmosphere to remove adsorbed water, and then heat to 350°C for 6 hours at a heating rate of 2°C / min ...

Embodiment 3

[0031] Example 3: with γ-Al 2 o 3 Preparation of Phosphorus Pentoxide-Strontium Oxide Composite Catalytic Material Supported as Carrier

[0032] The preparation method of the catalytic material in this example is the same as in Example 2, except that the carrier used is γ-Al 2 o 3 , the alkaline earth metal salt is strontium nitrate, and a small amount of nitric acid needs to be added dropwise during the dissolution process. Finally, after roasting treatment, the γ-Al 2 o 3 The phosphorus pentoxide-strontium oxide composite catalytic material supported by a carrier, wherein the phosphorus pentoxide accounts for 5% of the total mass of the catalytic material, and the strontium oxide accounts for 10% of the total mass of the catalytic material. By changing the addition amount of diammonium hydrogen phosphate and strontium nitrate, catalytic materials with different loads can be prepared.

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PUM

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Abstract

The invention discloses a catalyst suitable for synthesizing acrylic acid by an aqueous formaldehyde solution and acetic acid and a preparation and application method of the catalyst. The catalyst is mainly characterized by adopting one or more of activated carbon, aluminum sesquioxide, silicon dioxide or molecular sieve as carriers, and loading phosphorus pentoxide and one or more alkaline-earth metal oxides, wherein phosphorus pentoxide accounts for 1%-20% of the total mass of the catalyst, and the alkaline-earth metal oxides account for 5%-30% of the total weight of the catalyst. The catalyst is prepared by the steps of impregnation, temperature programmed calcination and the like, and a vacuum-ultrasonic impregnation technique is introduced during the preparation process. According to the invention, a fixed bed reactor is adopted for produce acrylic acid continuously under the suitable reaction conditions, the conversion per pass of formaldehyde is up to 35%, and the selectivity of acrylic acid is up to 55%.

Description

technical field [0001] The invention belongs to the field of preparation technology and application of catalytic materials, and relates to the reaction of formaldehyde aqueous solution and acetic acid to synthesize acrylic acid, using one or more of activated carbon, aluminum oxide, silicon dioxide or molecular sieve as a carrier, and carrying phosphorus pentoxide Composite catalyst with one or more than two kinds of alkaline earth metal oxides in strontium oxide and barium oxide and its preparation method, in particular to a preparation method of vacuum-ultrasonic impregnation combined with temperature-programmed roasting of the catalytic material, and the prepared The composite catalytic material is used for the reaction of formaldehyde aqueous solution and acetic acid to synthesize acrylic acid. Background technique [0002] Acrylic acid is mainly used as a monomer in the form of acid, salt and ester, and various acrylates can be prepared by homopolymerization or copolyme...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/08B01J27/18B01J29/40B01J29/70C07C51/353C07C57/04
Inventor 李春山李聃张国梁张洪华王红岩公茂明张锁江
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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