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A technology of hydroxymethylfurfural and formic acid, which is applied in the preparation of organic compounds, the separation/purification of carboxylic acid compounds, and the preparation of carboxylate salts. It can solve problems such as environmental pollution and resource waste, reduce side reactions, and increase yields. rate, the effect of increasing the mass transfer rate
Inactive Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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[0007] In the process of hydrolyzing lignocellulose to produce glucose under high temperature conditions, the by-products of formic acid and acetic acid are produced at the same time, so the obtained glucose solution contains formic acid and acetic acid at the same time. Cause serious environmental pollution, also can cause the waste of precious resources, in the existing technology of producing 5-hydroxymethyl furfural by glucose solution, also do not have the report about being able to recover formic acid and acetic acid simultaneously from the reaction solution
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Embodiment 1
[0039] The crushed corn stalks and water were injected into the hydrolysis tank according to the mass ratio of 1:1. The pre-hydrolysis temperature was 240°C and the pre-hydrolysis time was 20 min. %.
[0040] Add sodium sulfate in gained solution, control concentration is 3wt%.
[0041] The composite extractant used is a mixed solvent of benzene, ethyl acetate and 1,1,1-trichloroethane, wherein benzene accounts for 40wt%, ethyl acetate accounts for 20wt%, and 1,1,1-trichloroethane accounts for 40wt% %.
[0042] The feed ratio of extractant and glucose solution is 3:1 (volume ratio), and the feed rate of extractant and glucose solution is equal to the ultrasonic reactor volume (that is, the feed volume space velocity is 1 h -1 , that is, the reaction time is 1 h), pump the extractant and glucose solution into the ultrasonic reactor respectively, and quickly mix with the circulating material in the ultrasonic reactor to react-extraction process, the rate of the circulating mat...
Embodiment 2
[0045] According to the method of Example 1, the difference is that the feed rate is twice the volume of the ultrasonic reactor, that is, the reaction time is 0.5 h.
[0046] The experimental results showed that the conversion rate of glucose was 77wt%, the yield of 5-hydroxymethylfurfural was 60.4wt%, the recovery rate of acetic acid was 93.6wt%, and the recovery rate of formic acid was 90.2wt%.
Embodiment 3
[0048] According to the method of Example 1, the difference is that the feed rate is 0.67 times the volume of the ultrasonic reactor, that is, the reaction time is 1.5 h.
[0049] The experimental results showed that the conversion rate of glucose was 99%, the yield of 5-hydroxymethylfurfural was 81.9%, the recovery rate of acetic acid was 93.6%, and the recovery rate of formic acid was 90.2%.
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Abstract
The invention relates to a method for producing 5-hydroxymethyl furfural. The method comprises the following steps: hydrolyzing a biomass material from which hemicellulose is removed to obtain a mixed liquid of glucose, acetic acid and formic acid; feeding the mixed liquid to an ultrasonic reactor, and reacting with an extracting agent and a catalyst in a contact manner; cooling and layering a reaction effluent to obtain an upper-layer water phase and a lower-layer extracting phase, feeding the lower-layer extracting phase to an extracting agent regeneration tower to separate; obtaining regenerated extracting agent and a little of water from an overhead product in a phase splitting manner; feeding a tower kettle product to a product tower, and separating to obtaining 5-hydroxymethyl furfural; feeding an acetic acid and formic acid mixture obtained from the tower top into an acetic acid refining tower, and separating to obtain formic acid and acetic acid. According to the method, 5-hydroxymethyl furfural instantly reaches balance between the extracting agent and water phases by virtue of the ultrasonic reactor; the yield of 5-hydroxymethyl furfural is increased; the technological process is simple; meanwhile, 5-hydroxymethyl furfural, acetic acid and formic acid are recycled; no liquid waste is discharged; and the production process is a green environment-friendly process.
Description
technical field [0001] The invention belongs to the field of chemical industry and relates to the production technology of 5-hydroxymethylfurfural, in particular to a process for continuously producing 5-hydroxymethylfurfural by using an ultrasonic reactor. Background technique [0002] Biomass is an inexhaustible renewable resource and the only renewable carbon source. After decades of exploration, people have reached a consensus: the production of bio-based chemicals from biomass and the gradual replacement of fossil resources are currently the most feasible, best or only option. How to efficiently prepare bio-based platform chemicals from biomass sugar platform has become a research hotspot of scholars all over the world. [0003] 5-Hydroxymethylfurfural has a boiling point of 183°C and a melting point of 35.2°C under normal pressure. There are functional groups such as aldehyde groups, dienes, and cyclic ethers in its molecular structure, so it has the properties of ald...
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