Catalyst for synthesizing acrylic acid (ester) by taking formaldehyde and acetic acid as raw materials and preparation method thereof

A catalyst and acrylic acid technology, which is applied in the preparation of carboxylate esters, organic compounds, carboxylate salts, etc. It can solve the problems of low activity, high aldehyde-acid ratio, and pollution.

Active Publication Date: 2014-03-05
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

This type of catalyst also has low activity, high aldehyde-acid ratio and pollution to the environment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Example 1: with γ-Al 2 o 3 Preparation of Composite Catalytic Materials Supporting CsO Oxide

[0010] Grinding and sub-sieving 40g of γ-Al2O3 particles of 20-30 meshes, 11.55g of alkali metal salt cesium carbonate dissolved in a certain amount of water and adding the weighed γ-Al2O3 particles. After soaking and sonicating for 2 hours, let it stand for 12 hours. Then it was dried at 120°C for 6h, and the temperature was programmed to rise at 550°C for 6h to finally obtain the CsO composite catalytic material supported by γ-Al2O3. Cesium (calculated as cesium oxide) accounts for 25% of the mass of the carrier. By changing the amount of cesium carbonate added, catalytic materials with different loads can be prepared. A fixed-bed reactor is used at 300°C and the ester-aldehyde ratio is 6 to continuously produce acrylic acid (ester), the single-pass conversion rate of formaldehyde reaches 35%, and the selectivity of acrylic acid reaches 82%.

Embodiment 2

[0011] Example 2: with γ-Al 2 o 3 Preparation of Ba / V Composite Catalytic Material Supported as Carrier

[0012] Crush and sieve out 100g of γ-Al2O3 particles of 20-30 mesh, take 17.5g of barium nitrate and dissolve in a certain amount of water, 6.425g of ammonium metavanadate in an appropriate amount of water, mix the solution (add an appropriate amount of lye to dissolve) Add γ-Al2O3 particles. After soaking and sonicating for 2 hours, let it stand for 12 hours. Then it was dried at 120°C for 6h, and the temperature was programmed to rise at 550°C for 6h to finally obtain the Ba / V composite catalytic material supported by γ-Al2O3. Among them, vanadium (calculated as vanadium pentoxide) accounts for 5% of the mass of the carrier, and barium (calculated as barium oxide) accounts for 10% of the mass of the carrier. By changing the addition amount of ammonium metavanadate and barium nitrate, catalytic materials with different loads can be prepared. A fixed-bed reactor is us...

Embodiment 3

[0013] Embodiment 3: the preparation of the catalyst support that contains ZSM-5 type molecular sieve

[0014] 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 it in 200ml of 10wt% nitric acid solution under heating and stirring, knead the solution and the mixed powder to form a plastic paste, then extrude it, dry it at 120°C for 12 hours, and then bake it at 550°C for 5 hours to obtain a molecular sieve-containing Catalyst support for ZSM-5. By changing the type of molecular sieve added, catalyst supports containing different molecular sieves can be prepared. A fixed-bed reactor is used at 370°C and the ester-aldehyde ratio is 4 to continuously produce acrylic acid (ester). The single-pass conversion rate of formaldehyde reaches 31%, and the selectivity of acrylic acid re...

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PUM

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Abstract

The invention provides a catalyst for synthesizing acrylic acid (ester) by taking formaldehyde and acetic acid as raw materials and a preparation method thereof. The method is characterized by comprising the following steps: 1, selecting one or more than one oxide of cesium (Cs), barium (Ba), strontium (Sr), magnesium (Mg), antimony (Sb) and bismuth (Bi) according to the fact that the selected oxide accounts for 2% to 30% of total mass of a carrier, and selecting one or more than one oxide of vanadium (V), phosphorus (P) and molybdenum (Mo) as an auxiliary agent according to the fact that the selected oxide accounts for 0.1% to 20% of total mass of the carrier; 2, selecting gamma-Al2O3, SiO2 or a molecular sieve as the carrier of the catalyst; and 3, depolymerizing paraformaldehyde in methanol, ethanol, isopropyl alcohol and the like by using sodium hydroxide or potassium hydroxide, adding the depolymerization solution of the paraformaldehyde into the acetic acid according to the acid-aldehyde molar ratio being 2-6, evenly mixing the mixture and then directly pumping the mixture into a reaction kettle through a sample injection pump; and performing catalytic synthesis at a reaction temperature within 200 DEG C to 400 DEG C and under the micro-positive pressure by using a fixed bed reaction device for synthesizing the acrylic acid (ester). The two target products, namely, the acrylic acid and the corresponding ester, are contained in the synthesized catalyst under a proper condition, wherein the total yield of the acrylic acid (ester) can reach more than 35%; and the by-product is less in variety and low in content. The catalyst is low in cost and environment-friendly by taking the formaldehyde and the acetic acid as the raw materials. The catalyst applied to an acrylic acid (ester) synthesis technology is simple in process and easy to industrialize.

Description

Technical field: [0001] The invention relates to a catalyst for synthesizing acrylic acid (ester) with formaldehyde (paraformaldehyde and paraformaldehyde) and acetic acid as raw materials and a preparation method thereof. Background technique: [0002] Acrylic acid and its esters are important chemical raw materials. One of its uses is to condense with alcohols to generate corresponding esters, mainly including methyl acrylate (MA), ethyl acrylate (EA), butyl acrylate (BA) and octyl acrylate (2-EHA). It accounts for about 62% of the total consumption of acrylic acid. Acrylic acid occupies a very important position in the field of fine chemicals. By the late 1970s, polypropylene and acrylic acid copolymers produced with acrylic acid were used as dispersants, flocculants and thickeners. Acrylic acid can also be copolymerized with other functional monomers to produce a variety of important polymers with various industrial uses, such as super absorbent resins, oil field addi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/04B01J23/22B01J29/40B01J29/08B01J23/28B01J23/18B01J27/18C07C57/04C07C51/353C07C69/54C07C67/343
Inventor 李春山张国梁李聃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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