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Method for preparing furfurylideneacetone and di-furfurylideneacetone from furfural

A technology of difurfurylidene acetone and furfurylidene acetone, which is applied in the chemical field, can solve the problems of non-toxicity, strong corrosion and pollution, and achieve the effect of simple separation and purification process, high overall yield and mild reaction conditions

Active Publication Date: 2012-02-08
GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are only a small number of literatures reporting the preparation method of furfurylidene acetone, and the preparation process using liquid alkali such as NaOH, KOH or ammonia water as the catalyst is mostly used, but this process has strong corrosiveness and pollution, and is not a green production process
And for the preparation method of difurfurylidene acetone, do not see relevant literature and patent report yet

Method used

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  • Method for preparing furfurylideneacetone and di-furfurylideneacetone from furfural
  • Method for preparing furfurylideneacetone and di-furfurylideneacetone from furfural
  • Method for preparing furfurylideneacetone and di-furfurylideneacetone from furfural

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 4.8g furfural (0.05mol), 2.9g acetone (0.05mol) and 1.06g 20%-MgO / NaY catalyst are mixed with 95.4g (105ml) volumetric concentration in aqueous ethanol solution of 50%, furfural concentration is 4.6wt%, put Into a three-necked flask reactor equipped with a reflux column, heated to 100°C in an oil bath, and reacted for 8 hours. After the reaction is finished, cool for 30 minutes, vacuum filter, separate the catalyst, and collect the reaction solution. The collected reaction solution was transferred to a refrigerator set at -3°C for 8 hours, then suction filtered, and the crystals on the filter paper were collected, air-dried at room temperature for a period of time, and weighed to obtain 2.45 g of difurfurylideneacetone.

[0040] Transfer the remaining reaction liquid to a rotary hair dryer, fully recover ethanol at 60°C, and remove the ethanol solution in the recovery bottle when the reaction liquid becomes yellow and turbid. Then raise the temperature to 120°C, contin...

Embodiment 2

[0042] 4.8g furfural (0.05mol), 2.9g acetone (0.05mol) and 1.06g 20%-MgO / NaY catalyst and 95.4g (105ml) volume concentration are 40% ethanol aqueous solution mixing, furfural concentration is 4.6wt%, in Reaction at 100°C for 8h. The remaining steps were the same as in Example 1, 2.54 g of difurfurylidene acetone and 1.68 g of difurfurylidene acetone were collected, and the total yield was 54.8%.

Embodiment 3

[0044] Get 4.8g furfural (0.05mol), 5.8g acetone (0.1mol) and 1.06g 50%-MgO / NaY catalyst and 95.4g (105ml) volume concentration is the ethanol aqueous solution mixing of 50%, furfural concentration is 4.5wt%, in The reaction was carried out at 100° C. for 8 hours, and the remaining steps were the same as in Example 1. 2.35 g of difurfurylidene acetone and 1.78 g of difurfurylidene acetone were collected, and the total yield was 38.9%.

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Abstract

The invention discloses a method for preparing furfurylideneacetone and di-furfurylideneacetone from furfural by catalyzing with a solid alkali catalyst and a separating process. In the process, furfurylideneacetone and di-furfurylideneacetone are prepared by undergoing an aldol condensation reaction on furfural and acetone serving as raw materials and taking 'water-alcohol' or 'water-methanol' as a solvent under the catalyzing action of solid alkali. Di-furfurylideneacetone can be directly separated by refrigerating a reaction liquid at low temperature and crystalizing; and furfurylideneacetone can be further separated out by rotationally evaporating a residual liquid in vacuum and crystalizing. The purities of the two products are over 98percent, and the total yield is up to 55.4 percent. The method has the advantages of mild reaction conditions, simple separation and extraction processes, high overall yield, capability of realizing comprehensive utilization of two kinds of products, environmentally-friendly production process and high economic benefit and environmental benefit.

Description

Technical field: [0001] The invention relates to the technical field of chemistry, in particular to a method for preparing furfurylidene acetone and dipfurylidene acetone from furfural catalyzed by a solid base catalyst. technical background [0002] Furfurylidene acetone [4-(2-furyl)-3-buten-2-one], referred to as FA, is a resin monomer that can be used to manufacture chemically resistant plastic concrete, furan mastic, and furan epoxy Resin and other chemical industry, metallurgy and construction fields, but also an important organic chemical product and spice fine chemical intermediate. [0003] Difurylidene acetone [1,5-bis-(2-furan)-1,4-pentadien-3-one], referred to as F2A, is a rubber crosslinking agent called VP-4, which can Used as a co-crosslinking agent for rubber and plastic peroxides (also called peroxide activators or co-curing agents), mainly used for the activation of peroxide crosslinked products, and the crosslinking speed and mechanical strength are higher...

Claims

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Application Information

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IPC IPC(8): C07D307/46
Inventor 章青黄晓明刘琪英马隆龙王铁军
Owner GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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