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Preparation method of furfural

A furfural and biomass technology, which is applied in the field of furfural and furfural preparation, can solve the problems of low yield, acid corrosion, and limitation, and achieve the effects of reducing production costs, no corrosion of equipment, and low cost

Inactive Publication Date: 2013-08-14
NORTHWEST NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method can only obtain 45-55% furfural, not only the yield is low, but also the acid used has strong corrosiveness to the production equipment; secondly, there are very big problems in the reuse of mineral acid and the separation of products, Therefore, the application of this method in the industrial field has been greatly limited.

Method used

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  • Preparation method of furfural
  • Preparation method of furfural

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Embodiment 1, xylose synthesis furfural

[0021] In a 15 mL standard Schlenk glass tube, add 0.5 mmol (0.075 g) of xylose, 0.3 g of PEG-OSO 3 H, 0.03 g MnCl, then 2 mL [BMIM]PF 6 , stirred and reacted at 120°C for 18 min; after the reaction was completed, it was cooled rapidly and extracted with diethyl ether (3×2 mL). After the extraction was completed, 0.5 mmol of xylose was added to the extracted mother liquor. Continue to recycle, combine the organic phases, remove the ether with a rotary evaporator at 40°C, dry in vacuo overnight, and obtain furfural with a yield of 75%.

[0022] FTIR (KBr) ( ν , cm -1 ): 3388 (-OH), 1671 (-CHO), 1520 (C=C), 1020 (C-O-C), 2848, 2806 (-CH 2 ); 1 H-NMR (400 MHz, CDCl 3 ) δ = 9.67 (s, 1H, CHO), δ = 7.71 (d, J =4.0 Hz, 1H, Furan-H-5), δ = 7.28 (d, J =6.0 Hz, 1H, Furan-H-3), δ = 6.62 (t, 1H, J =4.0 Hz, Furan-H-4); 13 C-NMR (101 MHz, CDCl 3 ) δ: 177.93, 153.06, 148.36, 121.55, 112.76.

Embodiment 2

[0023] Embodiment 2, xylose synthesis furfural

[0024] Add 0.2g PS-PEG-OSO 3 H, other is identical with embodiment 1, and the yield of furfural is 82%, and its each performance index or characterization data are with embodiment 1.

Embodiment 3

[0025] Embodiment 3, ribose synthetic furfural

[0026] In a 15 mL standard Schlenk glass tube, add 0.5 mmol (0.075 g) of ribose, 0.3 g of PEG-OSO 3 H, 0.03 g MnCl, then 2 mL [BMIM]PF 6 , stirred and reacted at 120 °C for 20 min; after the reaction was completed, it was cooled rapidly and extracted with ether (3×2 mL). After the extraction was completed, 0.5 mmol of ribose was added to the extracted mother liquor. Continue to recycle, combine the organic phases, remove ether with a rotary evaporator at 40°C, dry in vacuo overnight, and obtain furfural with a yield of 67%. Its performance indicators or characterization data are the same as in Example 1.

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Abstract

The invention provides a preparation method of furfural, and belongs to the technical field of chemical synthesis. According to the method, furfural is obtained in 1-butyl-3-methylimidazolium hexafluorophosphate ([BMIM]PF6) ionic liquid through a one-pot method by taking pentose and biomass as raw materials, taking a polymer-supported sulfonic acid (PEG (polyethylene glycol)-OSO3H, PS (polystyrene)-PEG-OSO3H) as a catalyst and taking manganese chloride as an additive. Therefore, the reaction process is greatly simplified, the production rate is improved, and the production cost is reduced; the catalyst is easy to recover and recycle, and the separation and post-treatment processes are simple; and adopted raw materials and various reagents are non-toxic, the production process is pollution-free, equipment is not corroded, and the method is environment-friendly.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis, and relates to a method for preparing furfural, in particular to a method for preparing furfural by using biomass as a raw material. Background technique [0002] Furfural, also known as 2-furfuraldehyde, is a derivative in which the hydrogen atom at the 2-position of furan is replaced by an aldehyde group. Its English abbreviation is FAL, and its molecular formula is C 5 h 4 o 2 . Its chemical structural formula is: [0003] [0004] Furfural is the most important derivative of the furan ring system and is an important product obtained from agricultural by-products. Furfural is the raw material for the production of furfuryl alcohol and the main raw material for furan resin. Furfural is also a raw material for the preparation of various pharmaceuticals and industrial products. The traditional method of preparing furfural is to hydrolyze biomass with strong mineral ac...

Claims

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Application Information

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IPC IPC(8): C07D307/48C07D307/50
CPCY02P20/584
Inventor 张彰杜斌权正军王喜存达玉霞
Owner NORTHWEST NORMAL UNIVERSITY
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