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Method for purifying 2, 5-furan dicarbaldehyde

A furandicarbaldehyde, adsorbent technology, applied in 2 fields, can solve the problems of high commercial price, large organic solvent, consumption, etc.

Active Publication Date: 2016-08-24
保定加合精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] 2,5-furandicarbaldehyde (DFF) is an important furan derivative, 2,5-furandicarbaldehyde is widely used in many fields, and its commercial price is very expensive
[0006] The methods for purifying bio-based 2,5-furandicarbaldehyde reported in the current literature consume a large amount of organic solvents through extraction and other purification methods, and need to be optimized

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Step 1. Preparation of adsorbent:

[0021] Add 100Kg boron selective adsorption resin, 5Kg vinylpyridine, 0.5Kg2,3,4,5-bis(2-butenylene) tetrahydrofurfural, 700Kg water, 2Kg polyvinyl alcohol, 1Kg peroxide in 2000L reactor Benzoyl, react at 80°C for 6 hours, then heat up to 85°C for 2 hours, then heat up to 95°C for 6 hours, filter, and dry to obtain the adsorbent;

[0022] Step 2. Adsorption and purification of 2,5-furandicarbaldehyde:

[0023] Mix 100Kg 2,5-furandicarbaldehyde crude product and 1000Kg deionized water at 90°C for 3 hours, and then adsorb it through a chromatographic column equipped with an adsorbent at a temperature of 90°C and a flow rate of 3BV / h, and then dehydrate it. The purified product of 2,5-furandicarbaldehyde was obtained. See Table 1 for the mass percentage content of 2,5-furandicarbaldehyde in the product.

Embodiment 2

[0025] Step 1. Preparation of adsorbent:

[0026] Add 100Kg boron selective adsorption resin, 1Kg vinylpyridine, 0.1Kg2,3,4,5-bis(2-butenylene)tetrahydrofurfural, 500Kg water, 1Kg polyvinyl alcohol, 0.5Kg over a 2000L reactor For benzoyl oxidation, react at 80°C for 6 hours, then heat up to 85°C for 2 hours, then heat up to 95°C for 6 hours, filter, and dry to obtain the adsorbent;

[0027] Step 2. Adsorption and purification of 2,5-furandicarbaldehyde:

[0028] Mix 100Kg 2,5-furandicarbaldehyde crude product and 500Kg deionized water at 90°C for 1 hour, and then adsorb it through a chromatographic column equipped with an adsorbent at a temperature of 80°C and a flow rate of 1BV / h, and then dehydrate it. The purified product of 2,5-furandicarbaldehyde was obtained. See Table 1 for the mass percentage content of 2,5-furandicarbaldehyde in the product.

Embodiment 3

[0030] Step 1. Preparation of adsorbent:

[0031] Add 100Kg boron selective adsorption resin, 10Kg vinylpyridine, 1Kg2,3,4,5-bis(2-butenylene) tetrahydrofurfural, 1000Kg water, 4Kg polyvinyl alcohol, 2Kg benzene peroxide in 2000L reactor Formyl, react at 80°C for 6 hours, then heat up to 85°C for 2 hours, then heat up to 95°C for 6 hours, filter, and dry to obtain the adsorbent;

[0032] Step 2. Adsorption and purification of 2,5-furandicarbaldehyde:

[0033] Mix 100Kg 2,5-furandicarbaldehyde crude product with 2000Kg deionized water at 90°C for 1 hour, and then absorb it through a chromatographic column equipped with an adsorbent at a temperature of 100°C and a flow rate of 5BV / h, and then dehydrate it. The purified product of 2,5-furandicarbaldehyde was obtained. See Table 1 for the mass percentage content of 2,5-furandicarbaldehyde in the product.

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Abstract

The invention provides a method for purifying 2, 5-furan dicarbaldehyde. The method is characterized in that crude 2, 5-furan dicarbaldehyde is mixed with deionized water under appropriate temperature, the mixture is allowed to pass a chromatographic column with absorbent for absorption under appropriate temperature and flow speed, and then dewatering is performed to obtain the purified 2, 5-furan dicarbaldehyde.

Description

technical field [0001] The invention relates to a purification method, in particular to a purification method of 2,5-furandicarbaldehyde. Background technique [0002] 2,5-furandicarbaldehyde (DFF) is an important furan derivative. 2,5-furandicarbaldehyde is widely used in many fields, and its commercial price is very expensive. As an important platform compound, 5-hydroxymethylfurfural can be obtained from carbohydrate conversion. 5-HMF can be further converted to 2,5-furandicarbaldehyde through oxidation reaction by first dehydrating to synthesize HMF intermediate, and then in situ selective oxidation to synthesize DFF without separating HMF. [0003] Furfural is used as a raw material to prepare 2,5-furandicarbaldehyde, and the product contains a small amount of 5-hydroxymethylfurfural, which requires further purification. [0004] CN104496946A provides a method for purifying 2,5-furandicarbaldehyde from dimethyl sulfoxide solution, which comprises the following steps: ...

Claims

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Application Information

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IPC IPC(8): C07D307/46
CPCC07D307/46
Inventor 王琪宇王新
Owner 保定加合精细化工有限公司
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