WO2020164340A1 - 一种5-羟甲基糠醛的纯化方法 - Google Patents
一种5-羟甲基糠醛的纯化方法 Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/38—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with substituted hydrocarbon radicals attached to ring carbon atoms
- C07D307/40—Radicals substituted by oxygen atoms
- C07D307/46—Doubly bound oxygen atoms, or two oxygen atoms singly bound to the same carbon atom
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- the invention relates to the field of organic chemistry, in particular to a purification method of 5-hydroxymethyl furfural.
- HMF 5-Hydroxymethylfurfural
- HMF is mainly derived from the dehydration and conversion of six carbon sugars, and its purity is not high due to the occurrence of side reactions, which affects subsequent applications. Therefore, the establishment of high-purity 5-HMF separation and purification technology has important economic and social value.
- HMF can be prepared by dehydration of six carbon sugars, and the reaction process is as follows:
- the main impurities are humin, a macromolecular substance produced by the polymerization reaction between sugar or HMF, and also contains levulinic acid, formic acid, and HMF derivatives.
- these impurities are difficult to completely separate through differences in solubility, polarity, boiling point, etc.
- the separation and purification methods of HMF mainly include extraction, activated carbon adsorption, recrystallization and column chromatography.
- the extraction method is used, the extraction process is complicated and requires repeated extractions, and the yield and purity of HMF are low; while using activated carbon adsorption to effectively remove impurities, it will also cause a large amount of HMF loss.
- the recrystallization process using purified HMF requires the entire process to be operated at low temperature, which has high energy consumption and low efficiency.
- the column chromatography method after selecting the appropriate filler and mobile phase, HMF with higher purity can usually be obtained, but the separation speed is extremely slow and it is difficult to industrialize. Therefore, it is of great significance to develop a simple, gentle and rapid method for directly separating and purifying high-purity HMF from the reaction solution after sugar dehydration reaction to prepare HMF.
- the technical problem to be solved by the present invention is to provide a purification method of 5-hydroxymethyl furfural.
- the method provided by the present invention has a fast separation speed, and the obtained product has high purity and low HMF loss.
- the present invention provides a purification method of 5-hydroxymethyl furfural, which includes:
- the solution containing 5-hydroxymethyl furfural is pumped into the membrane separation device for filtration, the filtrate filtered through the membrane core is collected, and the solvent is removed to obtain 5-hydroxymethyl furfural.
- the membrane core in the membrane separation device is a polyamide membrane core, a polyimide membrane core, a polyurethane membrane core, a cellulose acetate membrane core, a sulfonated polysulfone membrane core, and a polyethersulfone membrane core. , Sulfonated polyethersulfone membrane core, polyvinyl alcohol membrane core or polypiperazine membrane core.
- the membrane core in the membrane separation device is a nanofiltration membrane.
- the molecular weight cut-off of the membrane core is 100-400 Da.
- the membrane component form in the membrane separation device is one or more of hollow fiber membrane, roll membrane, plate and frame membrane and tubular membrane.
- the pressure in the membrane separation is 0.5-4 MPa.
- the content of 5-hydroxymethylfurfural in the 5-hydroxymethylfurfural-containing solution is greater than 0.1wt%.
- the content of 5-hydroxymethylfurfural in the 5-hydroxymethylfurfural-containing solution is 1wt%-80wt%
- the 5-hydroxymethyl furfural solution is prepared according to the following method:
- the sugar containing the basic structural unit of the six-carbon sugar, the solvent and the catalyst are mixed and reacted to obtain a solution containing 5-hydroxymethyl furfural.
- the sugar containing the basic structural unit of six carbon sugars is one or more of glucose, fructose, maltose, sucrose, inulin, starch, galactose, cellobiose and cellulose.
- the present invention provides a method for purifying 5-hydroxymethyl furfural.
- the present invention filters the 5-hydroxymethyl furfural-containing solution by pumping it into a membrane separation device to collect and filter the membrane core. After removing the solvent from the filtrate to obtain 5-hydroxymethylfurfural, it was found through experiments that this method can very well purify the reaction liquid containing 5-hydroxymethylfurfural, the purification speed is fast, and the purity of the obtained HMF is high. And the loss of HMF is small.
- the present invention provides a purification method of 5-hydroxymethyl furfural, which includes:
- the solution containing 5-hydroxymethyl furfural is pumped into the membrane separation device for filtration, the filtrate filtered through the membrane core is collected, and the solvent is removed to obtain 5-hydroxymethyl furfural.
- the solution containing 5-hydroxymethyl furfural is pumped into the membrane separation device for filtration, the filtrate filtered through the membrane core is collected, and the solvent is removed to obtain 5-hydroxymethyl furfural;
- the filtration pressure is preferably 0.5 to 4 MPa, more preferably 1 to 3 MPa, most preferably 1.5 to 2 MPa; among them, when the purity of 5-hydroxymethyl furfural in the obtained filtrate is low, those skilled in the art can choose to pump again according to actual needs Filter again in the membrane separation device in order to obtain 5-hydroxymethyl furfural of suitable purity.
- the content of 5-hydroxymethyl furfural in the 5-hydroxymethyl furfural-containing solution is preferably greater than 0.1 wt%, more preferably 1 to 80 wt%, and more preferably 1.8 to 50 wt%; There is no special requirement for the source of hydroxymethyl furfural.
- Any solution containing 5-hydroxymethyl furfural prepared by a method known in the art that can prepare 5-hydroxymethyl furfural can be prepared according to the following method:
- the sugar of the basic structural unit of carbon sugar, the solvent and the catalyst are mixed and reacted to obtain a solution containing 5-hydroxymethyl furfural;
- the sugar containing the basic structural unit of six carbon sugar may be glucose, fructose, maltose, sucrose, and inulin , Starch, galactose, cellobiose and cellulose;
- the solvent can be water, organic solvent or a mixed solution of organic solvent and salt solution; wherein, when the solvent is water, the solvent containing 5 -An aqueous reaction solution of hydroxymethylfurfural, wherein the pH of the aqueous reaction solution containing 5-hydroxymethylfurfural is preferably greater than 3, more preferably 5-8, most preferably 6.8-7.5; when the solvent is organic
- the membrane core in the membrane separation device is preferably a polyamide membrane core, a polyimide membrane core, a polyurethane membrane core, a cellulose acetate membrane core, a sulfonated polysulfone membrane core, and a polyethersulfone membrane core.
- Membrane core sulfonated polyethersulfone membrane core, polyvinyl alcohol membrane core or polypiperazine membrane core, more preferably polyamide membrane core, polyimide membrane core, polyurethane membrane core, sulfonated polysulfone membrane core Core, polyethersulfone membrane core or sulfonated polyethersulfone membrane core; the molecular weight cut-off of the membrane core is preferably 100-400Da, more preferably 200-300Da; the present invention has no special effect on the membrane module form in the membrane separation device According to actual requirements, a suitable form can be selected according to actual needs. For example, it can be one or more of hollow fiber membranes, roll membranes, plate and frame membranes and tubular membranes; the present invention has no special requirements on the types of membrane separation devices. For example, it can be a cross-flow filter device.
- the method for purifying 5-hydroxymethyl furfural is to filter a solution containing 5-hydroxymethyl furfural into a membrane separation device, collect the filtrate filtered through the membrane core, and remove the solvent to obtain 5-hydroxymethyl It was found that this method can purify the reaction solution containing 5-hydroxymethyl furfural, so that the purity of the obtained HMF is high, and the loss of HMF is small; and the solution after sugar dehydration can be directly
- the whole process is continuous and fast, with large processing capacity, and can be directly applied to industrial applications; and the whole separation process is simple and efficient, with little contact with air, light, etc., and can be carried out at room temperature, thereby further improving the 5-hydroxymethyl The purity of furfural.
- the reaction solution containing 5-hydroxymethyl furfural can be prepared by the following method:
- the solvent is an organic solvent: add glucose to 1L saturated NaCl aqueous solution to prepare a solution with a glucose content of 10%, add 3L tetrahydrofuran and 10% catalyst, and after 15min of N 2 is passed in, at 160°C, 1.2MPa N 2 atmosphere The reaction was stirred for 1.5 hours and cooled to stop the reaction.
- the upper organic phase solution was the organic phase extract containing 5-hydroxymethyl furfural.
- Example 2 Take 2000ml of the organic solution containing 5-hydroxymethyl furfural and its derivatives prepared in Example 1 (where HMF is 2.8wt%, HMF derivative is 2.0wt%, and the organic phase is methanol), and added to the raw material tank of the cross-flow filtration experiment device In the process, it is pumped into a solvent-resistant polyurethane membrane core for filtration.
- the membrane has a molecular weight cut-off of 200Da and a pressure of 1MPa.
- the filtrate is collected.
- the solution that has not filtered through the membrane core is recycled back to the raw material tank to recover the solvent in the filtrate. Obtained HMF 85.7g.
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Abstract
本发明提供了一种5-羟甲基糠醛的纯化方法,本发明通过将含5-羟甲基糠醛的溶液泵入膜分离装置中进行过滤,收集滤过膜芯的滤液,除去溶剂,得到5-羟甲基糠醛,结果表明,该方法能够很好的对含5-羟甲基糠醛的反应液进行纯化,纯化速度快,处理量大,并且得到的HMF的纯度高,且HMF的损失少。
Description
本申请要求于2019年02月15日提交中国专利局、申请号为201910118960.0、发明名称为“一种5-羟甲基糠醛的纯化方法”的中国专利申请的优先权,其全部内容通过引用结合在本申请中。
本发明涉及有机化学领域,尤其涉及一种5-羟甲基糠醛的纯化方法。
5-羟甲基糠醛(以下简称HMF)是美国能源局发布的重要平台化合物之一,其分子中含有的高活性呋喃环、羟基和醛基等基团,使得HMF可通过加氢、酯化、卤化、聚合和水解等过程进行进一步的转化,作为高分子材料合成单体、大环化合物合成原料以及医药、农药的重要中间体原料,在各个领域具有重要的潜在应用价值,但同时这些应用也对HMF的纯度提出了很高的要求。HMF主要由六碳糖脱水转化而来,由于副反应的发生导致其纯度不高,影响后续应用。因此,建立高纯度的5-HMF分离纯化技术具有重要的经济和社会价值。
HMF可以通过六碳糖脱水制备,其反应流程如下:
该反应中,脱水后的反应体系中除HMF外,主要含有的杂质为糖或HMF之间发生聚合反应生成的大分子物质—胡敏素,同时还含有乙酰丙酸,甲酸,HMF衍生物,未反应完全的糖等,这些杂质难以通过溶解度、 极性、沸点等的差异进行彻底分离。
目前,HMF的分离纯化方法主要有萃取、活性炭吸附、重结晶以及柱层析等。采用萃取方法时,萃取过程复杂,需要反复多次萃取,HMF的收率和纯度均较低;而采用活性炭吸附在有效除去杂质的同时,也会导致大量HMF的损失。采用提纯HMF的重结晶过程则需要全程在低温下操作,能耗高,效率低。柱层析的方法在选择了恰当的填料和流动相后,通常可以得到纯度较高的HMF,但分离速度极慢,难以工业化。因此,开发一种简单温和快速的从糖脱水反应制备HMF后的反应溶液中直接分离提纯高纯度HMF的方法具有重要意义。
发明内容
有鉴于此,本发明所要解决的技术问题在于提供一种5-羟甲基糠醛的纯化方法,本发明提供的方法分离速度快,且得到的产品纯度高,HMF损失小。
本发明提供了一种5-羟甲基糠醛的纯化方法,包括:
将含5-羟甲基糠醛的溶液泵入膜分离装置中进行过滤,收集滤过膜芯的滤液,除去溶剂,得到5-羟甲基糠醛。
优选的,所述膜分离装置中的膜芯为聚酰胺膜芯、聚酰亚胺膜芯、聚亚胺酯膜芯、醋酸纤维素膜芯、磺化聚砜膜芯、聚醚砜膜芯、磺化聚醚砜膜芯、聚乙烯醇膜芯或聚哌嗪膜芯。
优选的,所述膜分离装置中的膜芯为纳滤膜。
优选的,所述膜芯的截留分子量为100~400Da。
优选的,所述膜分离装置中的膜的组件形式为中空纤维膜、卷式膜、板框式膜和管式膜中的一种或几种。
优选的,所述膜分离中的压力为0.5~4MPa。
优选的,所述含5-羟甲基糠醛的溶液中5-羟甲基糠醛的含量为大于 0.1wt%。
优选的,所述含5-羟甲基糠醛的溶液中5-羟甲基糠醛的含量为1wt%-80wt%
优选的,所述5-羟甲基糠醛的溶液按照以下方法制备得到:
将含六碳糖基本结构单元的糖、溶剂和催化剂混合反应,得到含5-羟甲基糠醛的溶液。
优选的,所述含六碳糖基本结构单元的糖为葡萄糖、果糖、麦芽糖、蔗糖、菊粉、淀粉、半乳糖、纤维二糖和纤维素中的一种或几种。
与现有技术相比,本发明提供了一种5-羟甲基糠醛的纯化方法,本发明通过将含5-羟甲基糠醛的溶液泵入膜分离装置中进行过滤,收集滤过膜芯的滤液,除去溶剂,得到5-羟甲基糠醛,通过实验发现,该方法能够很好的对含5-羟甲基糠醛的反应液进行纯化,纯化速度快,并且得到的HMF的纯度高,且HMF的损失少。
本发明提供了一种5-羟甲基糠醛的纯化方法,包括:
将含5-羟甲基糠醛的溶液泵入膜分离装置中进行过滤,收集滤过膜芯的滤液,除去溶剂,得到5-羟甲基糠醛。
按照本发明,本发明将含5-羟甲基糠醛的溶液泵入膜分离装置中进行过滤,收集滤过膜芯的滤液,除去溶剂,得到5-羟甲基糠醛;所述过滤的压力优选为0.5~4MPa,更优选为1~3MPa,最优选为1.5~2MPa;其中,当得到的滤液中5-羟甲基糠醛的纯度较低时,本领域技术人员可以根据实际需要选择再次泵入膜分离装置中再次过滤,以期得到合适的纯度的5-羟甲基糠醛。
其中,所述含5-羟甲基糠醛的溶液中5-羟甲基糠醛的含量优选为大于0.1wt%,更优选为1~80wt%,更优选为1.8~50wt%;本发明对5-羟甲基糠醛的来源没有特殊要求,本领域公知的可以制备5-羟甲基糠醛的方法制备得到的含5-羟甲基糠醛的溶液均可,如可以按照以下方法制备得到:将含六碳糖基本结构单元的糖、溶剂和催化剂混合反应,得到含5-羟甲基糠醛的溶液;其中,所述含六碳糖基本结构单元的糖可以为葡萄糖、 果糖、麦芽糖、蔗糖、菊粉、淀粉、半乳糖、纤维二糖和纤维素中的一种或几种;所述溶剂可以为水、有机溶剂或者有机溶剂与盐溶液的混合溶液;其中,当溶剂为水时,得到含5-羟甲基糠醛的水相反应液,其中,含5-羟甲基糠醛的水相反应液的pH优选为大于3,更优选为5~8,最优选为6.8~7.5;当溶剂为有机溶剂或有机溶剂和盐溶液的混合溶液时,得到含5-羟甲基糠醛的有机溶液或5-羟甲基糠醛与有机溶剂反应形成的5-羟甲基糠醛衍生物溶液;其中,对得到的含5-羟甲基糠醛的有机溶液的pH值没有特殊要求,可以直接进行过滤;且过滤后的5-羟甲基糠醛的衍生物溶液通过回收溶剂步骤即可得到5-羟甲基糠醛;所述催化剂可以为本领域公知的可用于将六碳糖制备得到5-羟甲基糠醛的催化剂。
本发明中,所述膜分离装置中的膜芯优选为聚酰胺膜芯、聚酰亚胺膜芯、聚亚胺酯膜芯、醋酸纤维素膜芯、磺化聚砜膜芯、聚醚砜膜芯、磺化聚醚砜膜芯、聚乙烯醇膜芯或聚哌嗪膜芯,更优选为聚酰胺膜芯、聚酰亚胺膜芯、聚亚胺酯膜芯、磺化聚砜膜芯、聚醚砜膜芯或磺化聚醚砜膜芯;所述膜芯的截留分子量优选为100~400Da,更优选为200~300Da;本发明对膜分离装置中的膜的组件形式没有特殊要求,可以根据实际需要选择合适的形式,如可以为中空纤维膜、卷式膜、板框式膜和管式膜中的一种或几种;本发明对膜分离装置的种类没有特殊要求,如可以为错流过滤装置。
本发明提供的5-羟甲基糠醛的纯化方法,通过将含5-羟甲基糠醛的溶液泵入膜分离装置中进行过滤,收集滤过膜芯的滤液,除去溶剂,得到5-羟甲基糠醛,结果发现,该方法能够很好的对含5-羟甲基糠醛的反应液进行纯化,使得得到的HMF的纯度高,且HMF的损失少;且可以直接对糖脱水后的溶液直接进行分离,整个过程连续快速,处理量大,可直接进行工业应用;而且整个分离过程简单高效,与空气、光照等接触少,常温下即可进行,进而进一步提高了分离得到的5-羟甲基糠醛的纯度。
下面将结合本发明实施例的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
含5-羟甲基糠醛的反应液可按以下方法制备得到:
当溶剂为水时:向1L含10%葡萄糖的水溶液加入固体酸催化剂,通入15min N
2后,在160℃、1.5MPa N
2氛围下搅拌反应1h,冷却以停止反应,过滤除去催化剂,即得到含5-羟甲基糠醛的水相反应液。
当溶剂为有机溶剂时:向1L饱和NaCl水溶液中加入葡萄糖,配成葡萄糖含量10%的溶液,加入3L四氢呋喃和10%的催化剂,通入15min N
2后,在160℃、1.2MPa N
2氛围下搅拌反应1.5h,冷却以停止反应,上层有机相溶液即为含5-羟甲基糠醛的有机相萃取液。
或者直接将葡萄糖、催化剂加入甲醇中,通入15min N
2后,在180℃、1.2MPa N
2氛围下搅拌反应2.0h,冷却以停止反应,即得到含5-羟甲基糠醛及5-羟甲基糠醛衍生物的有机溶液。
取含5-羟甲基糠醛的有机相萃取液2000ml(HMF含量1.8wt%,有机相为四氢呋喃),加入错流过滤实验装置的原料罐中,泵入可耐溶剂的聚酰亚胺膜芯中进行过滤,膜的截留分子量为200Da,压力1MPa,收集滤液,未滤过膜芯的溶液循环回到原料罐中,回收滤液中的溶剂,得到HMF 32.5g。
通过高效液相色谱(HPLC)分析HMF的纯度为98.6%,收率为99%。
实施例2:
取实施例1制备的含5-羟甲基糠醛的有机相萃取液4000ml(HMF含量1.8wt%,有机相为四氢呋喃),加入错流过滤实验装置的原料罐中,泵入耐溶剂的聚亚胺酯膜芯中进行过滤,膜的截留分子量为200Da,压力2MPa,收集滤液,未滤过膜芯的溶液循环回到原料罐中。将收集的滤液加入干净的原料罐中进行二次过滤,收集滤液,回收滤液中的溶剂,得到HMF 62.5g。
通过HPLC分析HMF纯度为99.5%,收率为96%。
实施例3:
取实施例1制备的含5-羟甲基糠醛及其衍生物的有机溶液2000ml(其中HMF2.8wt%,HMF衍生物2.0wt%,有机相为甲醇),加入错流过滤实 验装置的原料罐中,泵入耐溶剂的聚亚胺酯膜芯中进行过滤,膜的截留分子量为200Da,压力1MPa,收集滤液,未滤过膜芯的溶液循环回到原料罐中,回收滤液中的溶剂,得到HMF 85.7g。
通过HPLC分析HMF的纯度为99.8%,收率为99%。
实施例4:
取实施例1制备的含5-羟甲基糠醛的水相反应液2000ml,其HMF含量5.9wt%,pH为6.8,加入错流过滤实验装置的原料罐中,泵入聚酰胺膜芯中进行过滤,膜的截留分子量为300Da,压力1.5MPa,收集滤液,未滤过膜芯的溶液循环回到原料罐中,回收滤液中的溶剂,得到HMF121.4g。
通过高效液相色谱(HPLC)分析HMF的纯度为96.2%,收率为99%。
实施例5:
取实施例1制备的含5-羟甲基糠醛的有机相萃取液1000ml(HMF含量1.8%,有机相为四氢呋喃),尽可能除去有机溶剂,加入含20%乙醇的水溶液混合均匀,加入错流过滤实验装置的原料罐中,泵入聚酰胺膜芯中进行过滤,膜的截留分子量为300Da,压力1.2MPa,收集滤液,未滤过膜芯的溶液循环回到原料罐中,回收滤液中的溶剂,得到HMF 16.0g。
通过高效液相色谱(HPLC)分析HMF的纯度为98.8%,收率为98%。
对比例1
取实施例1制备的含5-羟甲基糠醛的有机相萃取液4000ml(HMF含量1.8%,有机相为四氢呋喃),加入错流过滤实验装置的原料罐中,泵入聚酰胺膜芯中进行过滤,膜的截留分子量为500Da,压力为1MPa,收集滤液,未滤过膜芯的溶液循环回到原料罐中。将收集的滤液加入干净的原料罐中进行二次过滤,收集滤液,回收滤液中的溶剂,得到HMF 77.9g。
通过HPLC分析HMF纯度为82.5%,收率为99.2%。
对比例2
取实施例1制备的含5-羟甲基糠醛的水相反应液4000ml(HMF含量1.8%),加入错流过滤实验装置的原料罐中,泵入聚醚砜膜芯中进行过滤,膜的截留分子量为200Da,压力为2MPa,收集滤液,未滤过膜芯的溶液 循环回到原料罐中。将收集的滤液加入干净的原料罐中进行二次过滤,收集滤液,回收滤液中的溶剂,得到HMF 80.6g。
通过HPLC分析HMF纯度为88.9%,收率为99.6%。
对比例3
取实施例1制备的含5-羟甲基糠醛的水相反应液,其HMF含量5.9wt%,向其中加入一定量的酸,调节pH至2.8,将该溶液2000ml加入错流过滤实验装置的原料罐中,泵入聚酰胺膜芯中进行过滤,膜的截留分子量为300Da,压力1.5MPa,收集滤液,未滤过膜芯的溶液循环回到原料罐中,回收滤液中的溶剂,得到HMF 122.4g。
通过高效液相色谱(HPLC)分析HMF的纯度为95.4%,收率为99%。
以上实施例的说明只是用于帮助理解本发明的方法及其核心思想。应当指出,对于本技术领域技术人员来说,在不脱离本发明原理的前提下,还可以对本发明进行若干改进和修饰,这些改进和修饰也落入本发明权利要求的保护范围内。
Claims (10)
- 一种5-羟甲基糠醛的纯化方法,包括:将含5-羟甲基糠醛的溶液泵入膜分离装置中进行过滤,收集滤过膜芯的滤液,除去溶剂,得到5-羟甲基糠醛。
- 根据权利要求1所述的纯化方法,其特征在于,所述膜分离装置中的膜芯为聚酰胺膜芯、聚酰亚胺膜芯、聚亚胺酯膜芯、醋酸纤维素膜芯、磺化聚砜膜芯、磺化聚醚砜膜芯、聚乙烯醇膜芯或聚哌嗪膜芯。
- 根据权利要求1所述的纯化方法,其特征在于,所述膜分离装置中的膜芯为纳滤膜。
- 根据权利要求1所述的纯化方法,其特征在于,所述膜芯的截留分子量为100~400Da。
- 根据权利要求1所述的纯化方法,其特征在于,所述膜分离装置中的膜的组件形式为中空纤维膜、卷式膜、板框式膜和管式膜中的一种或几种。
- 根据权利要求1所述的纯化方法,其特征在于,所述膜分离中的压力为0.5~4MPa。
- 根据权利要求1所述的纯化方法,其特征在于,所述含5-羟甲基糠醛的溶液中5-羟甲基糠醛的含量为大于0.1wt%。
- 根据权利要求1所述的纯化方法,其特征在于,所述含5-羟甲基糠醛的溶液中5-羟甲基糠醛的含量为1wt%-80wt%。
- 根据权利要求1所述的纯化方法,其特征在于,所述5-羟甲基糠醛的溶液按照以下方法制备得到:将含六碳糖基本结构单元的糖、溶剂和催化剂混合反应,得到含5-羟甲基糠醛的溶液。
- 根据权利要求9所述的纯化方法,其特征在于,所述含六碳糖基本结构单元的糖为葡萄糖、果糖、麦芽糖、蔗糖、菊粉、淀粉、半乳糖、纤维二糖和纤维素中的一种或几种。
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