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Method for preparing acrylic acid from glycerin as raw material

A technology of acrylic acid and glycerin, which is applied in the preparation of carboxylates, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of catalyst deactivation, low yield of acrylic acid, and reduction of catalytic active centers, so as to simplify the process and save cost, and the effect of extending the service life

Inactive Publication Date: 2011-11-23
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, the highly active reducing species can also easily cause the reduction of the catalytic active center, leading to the deactivation of the catalyst.
Using V-P-O crystal oxide material as the catalyst (J.Catal.2009, 268, 260-267), the reaction conditions are 300°C and 0.1MPa, under an oxidizing atmosphere, the conversion rate of glycerin is 100%, and the selectivity of acrolein is 66%. , the selectivity of hydroxyacetone is 4%, the selectivity of acrylic acid is 3%, the carbon balance is 93%, there is no carbon deposit on the catalyst, but the yield of acrylic acid is low

Method used

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  • Method for preparing acrylic acid from glycerin as raw material

Examples

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Embodiment 1

[0019] Put 38.1 grams of copper nitrate hexahydrate, 1.1 grams of cerium nitrate hexahydrate and 50.5 grams of ferric nitrate nonahydrate into a beaker, add 10 mL of deionized water, place in a water bath at 60°C, heat to dissolve, stir well, and then evaporate to dryness. Drying at 120°C for 12 hours, and calcining at 500°C for 4 hours in an air atmosphere, the prepared oxo-salt catalyst is Cu 1.03 Ce 0.02 Fe 1.00 o z .

[0020] 2mL oxo acid salt catalyst Cu 1.03 Ce 0.02 Fe 1.00 o z Mix it with 4mL of quartz sand and transfer it into a glass reactor with an inner diameter of 15mm, and use quartz fibers to fix the catalyst up and down. Nitrogen is introduced, and the reaction is heated to 310°C for activation for 1 hour, and then the mixed gas with a molar ratio of glycerin: water: nitrogen: oxygen = 10:12:8.25:0.125 is preheated at 290°C and then passed into the reactor. Airspeed is 100h -1 , the reaction temperature is 310°C. The reacted product was collected with ...

Embodiment 2

[0022] Put 10.0 g of titanium dioxide sol, 38.6 g of cobalt nitrate hexahydrate, and 1.5 g of zinc nitrate hexahydrate into a beaker, add 10 mL of deionized water, place in a 60°C water bath, heat and stir thoroughly, and then evaporate to dryness. Drying at 120°C for 12 hours, and calcining at 650°C for 4 hours in an air atmosphere, the prepared oxo-salt catalyst is Co 1.06 Zn 0.04 Ti 1.00 o z . The catalytic reaction conditions are the same as in Example 1. The reaction results are shown in Table 1.

Embodiment 3

[0024] Put 154.5 grams of ammonium heptamolybdate, 1.5 grams of nickel nitrate hexahydrate, and 43.4 grams of ferric nitrate nonahydrate into a beaker, add 10 mL of deionized water, place in a water bath at 60°C, heat and stir thoroughly, and then evaporate to dryness. Dry at 120°C for 12 hours, and bake at 550°C for 4 hours in the air atmosphere, the prepared oxo acid salt catalyst is Fe0.86 Ni 0.04 Mo 1.00 o z . The catalytic reaction conditions are the same as in Example 1. The reaction results are shown in Table 1.

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Abstract

A method for preparing acrylic acid from glycerin as a raw material. The method is characterized in that glycerin aqueous solution with mass concentration of 10 to 95% and mixed gas of inert gas and oxygen gas are mixed and then are fed into a reactor loaded with a solid catalyst to undergo a catalytic oxidation dehydration reaction so that glycerin is transformed into acrylic acid. The method adopts a single catalyst and a single reactor, and specifically adopts an oxysalt as a catalyst, wherein the oxysalts have double-function of oxidation and dehydration, prepares directly acrylic acid from glycerin, and realizes respectively a glycerin transformation rate of 100% and acrylic acid selectivity of 77%, thus improves acrylic acid selectivity and simplifies catalyst use processes.

Description

technical field [0001] The present invention relates to a method for preparing acrylic acid with glycerol as a raw material. Specifically, after mixing a certain concentration of glycerin aqueous solution with inert gas and oxygen in a certain molar ratio in a preheating zone, the glycerol is then passed through a reactor filled with a solid catalyst. Oxidation and dehydration reactions take place in the reactor, and the reaction does not require the separation of acrolein to directly generate acrylic acid. Background technique [0002] Biodiesel is an important renewable energy source, mainly using animal fat or vegetable oil as raw material, and it is produced through transesterification reaction, and the by-product glycerol accounts for about 10% of the output. With the increase of biodiesel production capacity, the market supply of by-product glycerin will also continue to expand; at the same time, glycerin can also be obtained from multiple biomass methods such as sugar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C57/065C07C57/05C07C51/377C07C51/21
Inventor 王峰徐杰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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