WO2022122028A1 - 一种麦芽酚或乙基麦芽酚升华后粗品反萃取提纯方法和装置 - Google Patents

一种麦芽酚或乙基麦芽酚升华后粗品反萃取提纯方法和装置 Download PDF

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WO2022122028A1
WO2022122028A1 PCT/CN2021/137215 CN2021137215W WO2022122028A1 WO 2022122028 A1 WO2022122028 A1 WO 2022122028A1 CN 2021137215 W CN2021137215 W CN 2021137215W WO 2022122028 A1 WO2022122028 A1 WO 2022122028A1
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maltol
sublimation
ethyl
ethyl maltol
crude product
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PCT/CN2021/137215
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English (en)
French (fr)
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秦基楼
张其军
陈金林
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安徽金禾实业股份有限公司
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Priority to CN202180065864.XA priority Critical patent/CN116348185A/zh
Publication of WO2022122028A1 publication Critical patent/WO2022122028A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D309/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings
    • C07D309/34—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
    • C07D309/36—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with oxygen atoms directly attached to ring carbon atoms
    • C07D309/40—Oxygen atoms attached in positions 3 and 4, e.g. maltol
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/04—Solvent extraction of solutions which are liquid
    • B01D11/0492—Applications, solvents used

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  • the invention relates to a method and a device for reverse extraction and purification of crude products after sublimation of maltol and ethyl maltol.
  • Chinese patent document CN108299362A discloses a method for separating impurities in crude maltol product, including: a. the hydrolyzed material is filtered and then cooled to 30°C and 35°C; b. the hydrolyzed liquid is pumped into the extraction mixer, and simultaneously, chloroform is pumped to make The hydrolyzed liquid and chloroform are fully mixed; c. The mixed liquid enters the stratifier, the light phase after the stratification enters the hydrolyzed liquid collection tank, and the lower heavy phase enters the chloroform collection tank and is put into the distillation still to recover chloroform, and the distilled material is sent to the chloroform collection tank. To the sublimation kettle for sublimation; d.
  • the crude product receiving kettle is heated in the ethyl maltol sublimation section, so that the temperature in the crude product receiving kettle is controlled between 90 and 92 ° C, and the material in the kettle is The molten liquid is directly sent to the crystallization kettle for crystallization, eliminating the two processes of freezing and centrifugal throwing in the traditional process.
  • Chinese patent document CN103113339B discloses a method for separating and purifying maltol, which includes grating reaction, addition reaction, hydrolysis reaction, chlorinated hydrolysis reaction and sublimation separation steps. Pa or less, the temperature is 110°C to 120°C, and the maltol is subjected to distillation treatment.
  • Patent document US5440053A discloses a method for recovering maltol from a water-insoluble raw material comprising maltol, comprising: contacting the raw material with an aqueous solution of a solute material, wherein the solute material is a halide of an alkali metal or an alkaline earth metal, It increases the specific gravity of the water and increases the immiscibility of the water with the alkali or alkali metals.
  • the alkaline earth metal halide is more soluble in water than the maltol at low temperatures; and the solution and the alkali metal or alkaline earth metal The halide isolates the maltol.
  • the processing objects are all primary isolates including the hydrolyzate of maltol.
  • the melting point of organic impurities is similar to that of maltol (or ethyl maltol)
  • the separation is difficult, and there is a lack of low-cost and effective means to separate the maltol or ethyl maltol obtained by sublimation. a small amount of organic impurities.
  • the technical problem to be solved by the present invention is to provide a method for stripping and purifying the crude product after sublimation of maltol or ethyl maltol, which can efficiently remove irritating impurities in the crude product after the sublimation of maltol or ethyl maltol.
  • the present invention provides a crude product back-extraction and purification method after sublimation of maltol or ethyl maltol, comprising the following steps:
  • a crude product back-extraction and purification method after sublimation of maltol or ethyl maltol comprises the following steps:
  • Step 1 After sublimation of maltol or ethyl maltol, the crude product and water are heated to 80 ⁇ 5°C for dissolving;
  • Step 2 The material obtained in step 1 is left to stand in layers, and after separating the upper aqueous solution, the temperature of the upper aqueous solution layer is lowered to 10°C-15°C;
  • Step 3 centrifugation to obtain the crystals of maltol or ethyl maltol after removal of impurities.
  • the mass ratio of maltol or ethyl maltol to water is 1:6.
  • the melting kettle includes a melting kettle, a layering tank connected with the melting kettle, a freezing kettle connected with the layering tank, and a centrifuge connected with the freezing kettle.
  • the melting kettle is an enamel melting kettle
  • the layering tank is an enamel layering tank, the upper part is a circular head, and the bottom is a cone
  • the freezing kettle is an enamel freezing kettle.
  • Figure 1 is a flow chart of the present invention.
  • 1-melting kettle 2-layering tank; 3-freezing kettle; 4-centrifuge; A-crude product; B-mother liquor reuse; C-mother liquor; D-sewage treatment; E-ethyl malt powder.
  • the melting point of maltol is 159-162°C, it can be volatilized with water vapor, sublime at 93°C, and about 1.2% by weight dissolves in water at room temperature.
  • Ethyl maltol has a melting point of 89-93°C, is volatile at room temperature, and dissolves in water by about 1.6% by weight at room temperature.
  • Maltol and ethyl maltol have low solubility at room temperature.
  • the absolute content of organic impurities in the crude product obtained after sublimation is not high, but these impurities cause maltol to not meet the quality standards in terms of odor and color. These impurities are also difficult to remove by conventional means.
  • Maltol and ethyl maltol show better solubility in polar solvents such as acetone, alcohol, etc. However, these solvents are water soluble and will dissolve not only maltol but possibly other organic impurities as well. At the same time, due to its volatile nature, if these solvents are used to purify maltol and ethyl maltol, these solvents will take away more maltol and ethyl maltol during distillation and separation, and at the same time maltol and ethyl maltol are condensed and crystallized. More impurities will be introduced later.
  • polar solvents such as acetone, alcohol, etc.
  • these solvents are water soluble and will dissolve not only maltol but possibly other organic impurities as well.
  • these solvents due to its volatile nature, if these solvents are used to purify maltol and ethyl maltol, these solvents will take away more maltol and ethyl maltol during distillation and separation
  • Maltol and ethyl maltol are insoluble in non-polar hydrocarbons, which makes extraction of maltol and ethyl maltol with these solvents difficult.
  • the impurities in the maltol are mainly non-polar impurities.
  • solubility of maltol and ethyl maltol in water varies greatly at different high temperatures and low temperatures, first Dissolve maltol and ethyl maltol in hot water under stirring conditions, then keep the temperature, after the maltol and ethyl maltol are left to stand for stratification, remove the organic phase, and then use maltol and ethyl maltol at different temperatures Solubility difference of phenol in water, cooling maltol and ethyl maltol aqueous solution, centrifugation to separate maltol and ethyl maltol.
  • This process is actually the process of returning maltol and ethyl maltol from the loaded organic phase (or impurity) to the aqueous phase.
  • the inventors obtained high-quality maltol and ethyl maltol products through such a method, without introducing new impurities, and the cost is low.
  • a crude product back-extraction purification method after the sublimation of ethyl maltol comprises the following steps:
  • the recovery rate of ethyl maltol recovered by testing was 93.2% for the crude product, and the purity of the recovered maltol was 99.2%.
  • Embodiment 2 is a diagrammatic representation of Embodiment 1:
  • a crude product back-extraction purification method after the sublimation of ethyl maltol comprises the following steps:
  • the recovery rate of the recovered ethyl maltol to the crude product was 94.5%, and the purity of the recovered maltol was 99.3%.
  • a crude product back-extraction purification method after the sublimation of ethyl maltol comprises the following steps:
  • the recovered ethyl maltol was tested and recovered, and the recovery rate to the crude product was 94.3%, and the purity of the recovered maltol was 99.1%.
  • Embodiment 4 is a diagrammatic representation of Embodiment 4:
  • a crude product back-extraction purification method after sublimation of maltol comprises the following steps:
  • the recovery rate of the recovered maltol was 92.5% for the crude product, and the purity of the recovered maltol was 99.2%.
  • Embodiment 5 is a diagrammatic representation of Embodiment 5:
  • a crude product back-extraction purification method after sublimation of maltol comprises the following steps:
  • the recovery rate of the crude product was 93.2%, and the purity of the recovered maltol was 99.3%.
  • the melting kettle adopts the enamel melting kettle with jacket and stirring;
  • the layering tank adopts the enamel layering tank (the upper circular head and the bottom conical);
  • the freezing kettle adopts the enamel freezing kettle with jacket and stirring.
  • a solvent is generally used to dissolve the sublimed product of maltol and ethyl maltol, and then the maltol and ethyl maltol in water are separated.
  • the difference between the present invention and the prior art is that the present invention uses heated water to dissolve maltol and ethyl maltol, and does not use a solvent that may be miscible with non-polar organic substances, and back-extracts maltol and ethyl maltol Once in water, the organic phase is removed.
  • This method can decolorize and purify compared with the solvent decolorization and purification method, saves the use of decolorizing agents, and consumes similar energy to the original method, and a small amount of impurities can be treated harmlessly after separation; When processing crude products, the application consumes less energy. Compared with the solvent decolorization and purification method or the sublimation method to process the crude product, the present application has a high yield.

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  • Organic Chemistry (AREA)
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Abstract

本申请公开了一种麦芽酚或乙基麦芽酚升华后粗品反萃取提纯方法，包括以下步骤：步骤1：将麦芽酚或乙基麦芽酚升华后粗品与水加热至80±5℃进行溶料；步骤2：将步骤1所获得的物料分层静置，分离上层水溶液后，将上层水溶液层温度降至10℃-15℃；步骤3：离心得到除杂后的麦芽酚或乙基麦芽酚晶体。还公开了一种提纯装置。本申请提纯技术方案产率高，产品纯度高。

Description

一种麦芽酚或乙基麦芽酚升华后粗品反萃取提纯方法和装置
本申请要求申请日为2020年12月11日，申请号为202011442712.0，发明名称为一种乙基麦芽酚升华后粗品反萃取提纯方法的中国专利申请的优先权。
技术领域
本发明涉及一种麦芽酚和乙基麦芽酚升华后粗品反萃取提纯方法和装置。
背景技术
麦芽酚和乙基麦芽酚的生产反应过程中，生成大量的副产物，其中部分与麦芽酚和乙基麦芽酚沸点接近的具有刺激性气味的杂质会在升华提纯工段随麦芽酚和乙基麦芽酚一同被蒸发出来，且与麦芽酚和乙基麦芽酚极易互溶，对其很难进行分离，造成麦芽酚和乙基麦芽酚产品质量一直难于提升。
中国专利文献CN108299362A公开了一种分离麦芽酚粗品中杂质的方法，包括：a、将水解后物料过滤后降温至30℃35℃；b、水解液泵入萃取混合器，同时泵入氯仿，使水解液和氯仿充分混合；c、混合液进分层器，分层后的轻相进水解液收集槽，下层重相进氯仿收集槽并放入蒸馏釜蒸馏回收氯仿，蒸馏后的物料送至升华釜进行升华；d、将水解收集槽中轻相物料泵入中和釜，调PH至2.5 3.5，温度降至40℃45，物料放入结晶器冷冻结晶，离心甩干后送升华釜进行升华。中国专利文献CN101993428B公开了一种乙基麦芽酚的提纯方法，其特征在于包括以下顺序步骤：(1)将乙基麦芽酚粗品进行升华；(2)溶解；(3)冷却；(4)固液分离；(5)干燥，得到成品。在这一专利文献中，乙基麦芽酚在溶解后，采用乙醇和水的混合溶液作为溶解乙基麦芽酚的溶剂，由于溶剂可以与其他有机物互溶，因此，无法完成分层的操作， 这就导致后续无法将杂质从混合物中分离。中国专利文献CN105085457A公开一种乙基麦芽酚升华结晶工艺，在乙基麦芽酚升华工段中对粗品接受釜进行加热，使粗品接受釜内温度控制在90～92℃之间，釜内的物料呈熔融的液态，直接送至结晶釜结晶，省去传统工艺中冷冻和离心甩料两道工序。中国专利文献CN103113339B公开了一种麦芽酚分离提纯方法,包括格式反应、加成反应、水解反应、氯化水解反应以及升华分离步骤，其特征在于：升华步骤采用分子蒸馏器，蒸馏真空度在0.05Pa以下，温度在110℃～120℃，对麦芽酚进行蒸馏处理。专利文献US5440053A公开了一种从包含麦芽酚的水不溶性原料中回收麦芽酚的方法，包括：使所述原料与溶质材料的水溶液接触，其中所述溶质材料是碱金属或碱土金属的卤化物，其增加了所述水的比重并且增加了所述水与所述碱金属或碱金属的不溶混性。在有效将麦芽酚从所述原料中提取到所述溶液中的条件下，碱土金属卤化物在低温下比所述麦芽酚更易溶于水；和从所述溶液和所述碱金属或碱土金属卤化物分离所述麦芽酚。
以上现有技术在分离粗品麦芽酚(或乙基麦芽酚)时，处理对象均为包括有麦芽酚的水解产物的初级分离物。在升华提纯获得麦芽酚后，由于有机杂质的熔点等与麦芽酚(或乙基麦芽酚)类似，分离的难度较大，缺乏低成本的有效手段来分离升华获得的麦芽酚或乙基麦芽酚中的少量的有机杂质。
发明内容
本发明所要解决的技术问题是提供一种麦芽酚或乙基麦芽酚升华后粗品反萃取提纯方法，该方法能够高效去除麦芽酚或乙基麦芽酚升华后粗品中的刺激性杂质。
为解决上述技术问题，本发明提供了一种麦芽酚或乙基麦芽酚升华后粗品反萃取提纯方法，包括以下步骤：
(1)向溶料釜内投入麦芽酚或乙基麦芽酚，再加入纯水，其中麦芽酚或乙基麦芽酚与水的质量比为1：6，投料结束后开蒸气加热至80±5℃进行溶料；
(2)溶料结束后，将溶料釜内的物料转至分层槽静置10min后进行分 层，将下层杂质分出后，将上层水溶液层放入冷冻釜进行降温，温度降至10℃-15℃，然后用离心机进行离心，得到除杂后的麦芽酚或乙基麦芽酚晶体，离心后的母液回步骤(1)进行溶料套用，至母液中杂质含量超指标后，排出系统。
一种麦芽酚或乙基麦芽酚升华后粗品反萃取提纯方法，包括以下步骤：
步骤1：将麦芽酚或乙基麦芽酚升华后粗品与水加热至80±5℃进行溶料；
步骤2：将步骤1所获得的物料分层静置，分离上层水溶液后，将上层水溶液层温度降至10℃-15℃；
步骤3：离心得到除杂后的麦芽酚或乙基麦芽酚晶体。
进一步的，麦芽酚或乙基麦芽酚与水的质量比为1：6。
进一步的，包括溶料釜，与溶料釜连接的分层槽，与分层槽连接的冷冻釜，与冷冻釜连接的离心机。
进一步的，溶料釜为搪瓷溶料釜；分层槽为搪瓷分层槽，上部为圆形封头，底部为锥形；冷冻釜为搪瓷冷冻釜。
为简单说明问题起见，以下对发明所述的一种麦芽酚或乙基麦芽酚升华后粗品反萃取提纯方法均简称为本方法。
本方法的优点：1、利用水与刺激性杂质不互溶的特性，利用水进行反萃取，进而能够高效的去除大量的杂质；2、为加大麦芽酚或乙基麦芽酚在水中的溶解度，采用加热的方式，大大降低了水的用量，能够实现麦芽酚或乙基麦芽酚：水＝1:6的较少使用量；较少的使用水的也便于后续的分离以及减少水的污染和浪费。3、分层后得到的麦芽酚或乙基麦芽酚水溶液中含有水溶性杂质较少，因而可以实现多次套用，降低母液废水处理难度。
附图说明
图1是本发明的的流程图。
其中1-溶料釜；2-分层槽；3-冷冻釜；4-离心机；A-粗品；B-母液回用；C-母液；D-污水处理；E-乙基麦芽粉。
具体实施方式
麦芽酚熔点是159-162℃，能随水蒸气挥发，在93℃升华，常温下约1.2％重量百分数溶解于水。乙基麦芽酚熔点89-93℃，在常温下易挥发，常温下，常温下约1.6％重量百分数溶解于水。麦芽酚和乙基麦芽酚在常温下溶解度较低。升华后获得的粗品中有机杂质绝对含量并不高，但是这些杂质导致麦芽酚在气味、颜色上均不符合质量标准。这些杂质也难以通过常规的手段去除。
麦芽酚和乙基麦芽酚在极性溶剂如丙酮，醇等中显示较好的溶解性。但是，这些溶剂是水溶性的，不仅会溶解麦芽酚，还可能溶解其他有机杂质。同时，由于易挥发，如果使用这些溶剂去提纯麦芽酚和乙基麦芽酚，这些溶剂在蒸馏分离时会带走较多的麦芽酚和乙基麦芽酚，同时麦芽酚和乙基麦芽酚冷凝结晶后会引入较多杂质。
麦芽酚和乙基麦芽酚不溶于非极性烃，这使得使用这些溶剂萃取获得麦芽酚和乙基麦芽酚是困难的。
发明人在组织麦芽酚工业化生产的实践中发现，麦芽酚中杂质主要是非极性的杂质，考虑到利用麦芽酚和乙基麦芽酚在水中的溶解度在不同高温和低温下溶解度差异较大，首先将麦芽酚和乙基麦芽酚搅拌条件下溶解于热水中，随后保持温度，将麦芽酚和乙基麦芽酚静置分层后，去除有机相，随后利用不同温度下麦芽酚和乙基麦芽酚在水中的溶解度差异，冷却麦芽酚和乙基麦芽酚水溶液，离心分离麦芽酚和乙基麦芽酚。这一过程实际上是将麦芽酚和乙基麦芽酚从负载有机相(或称杂质)返回水相的过程。发明人通过这样的方法，获得了高质量的麦芽酚和乙基麦芽酚产品，没有引入新的杂质，成本低廉。
实施例一：
参见图1，一种乙基麦芽酚升华后粗品反萃取提纯方法，包括以下步骤：
(1)向溶料釜1内投入乙基麦芽酚，再加入纯水，其中乙基麦芽酚与水的质量比为1：6，投料结束后开蒸气加热至75℃进行溶料；
(2)溶料结束后，将溶料釜1内的物料转至分层槽2静置10min后进行分层，将下层杂质分出后，将上层水溶液层放入冷冻釜3进行降温，温度 降至10℃，然后用离心机4进行离心，得到除杂后的乙基麦芽酚晶体，离心后的母液回步骤(1)进行溶料套用，至母液中杂质含量超指标后，排出系统。
经过检测回收的乙基麦芽酚，对粗品回收率为93.2％，回收的麦芽酚纯度为99.2％。
实施例二：
参见图1，一种乙基麦芽酚升华后粗品反萃取提纯方法，包括以下步骤：
(1)向溶料釜1内投入乙基麦芽酚，再加入纯水，其中乙基麦芽酚与水的质量比为1：6，投料结束后开蒸气加热至80℃进行溶料；
(2)溶料结束后，将溶料釜1内的物料转至分层槽2静置10min后进行分层，将下层杂质分出后，将上层水溶液层放入冷冻釜3进行降温，温度降至12.5℃，然后用离心机4进行离心，得到除杂后的乙基麦芽酚晶体，离心后的母液回步骤(1)进行溶料套用，至母液中杂质含量超指标后，排出系统。
经过检测回收的乙基麦芽酚，对粗品回收率为94.5％，回收的麦芽酚纯度为99.3％。
实施例三：
参见图1，一种乙基麦芽酚升华后粗品反萃取提纯方法，包括以下步骤：
(1)向溶料釜1内投入乙基麦芽酚，再加入纯水，其中乙基麦芽酚与水的质量比为1：6，投料结束后开蒸气加热至85℃进行溶料；
(2)溶料结束后，将溶料釜1内的物料转至分层槽2静置10min后进行分层，将下层杂质分出后，将上层水溶液层放入冷冻釜3进行降温，温度降至15℃，然后用离心机4进行离心，得到除杂后的乙基麦芽酚晶体，离心后的母液回步骤(1)进行溶料套用，至母液中杂质含量超指标后，排出系统。
经过检测回收的乙基麦芽酚，对粗品回收率为94.3％，回收的麦芽酚纯度为99.1％。
实施例四：
参见图1，一种麦芽酚升华后粗品反萃取提纯方法，包括以下步骤：
(1)向溶料釜1内投入麦芽酚，再加入纯水，其中麦芽酚与水的质量比为1：6，投料结束后开蒸气加热至75℃进行溶料；
(2)溶料结束后，将溶料釜1内的物料转至分层槽2静置10min后进行分层，将下层杂质分出后，将上层水溶液层放入冷冻釜3进行降温，温度降至12℃，然后用离心机4进行离心，得到除杂后的麦芽酚晶体，离心后的母液回步骤(1)进行溶料套用，至母液中杂质含量超指标后，排出系统。
经过检测回收的麦芽酚，对粗品回收率为92.5％，回收的麦芽酚纯度为99.2％。
实施例五：
参见图1，一种麦芽酚升华后粗品反萃取提纯方法，包括以下步骤：
(1)向溶料釜1内投入麦芽酚，再加入纯水，其中麦芽酚与水的质量比为1：6，投料结束后开蒸气加热至85℃进行溶料；
(2)溶料结束后，将溶料釜1内的物料转至分层槽2静置10min后进行分层，将下层杂质分出后，将上层水溶液层放入冷冻釜3进行降温，温度降至14℃，然后用离心机4进行离心，得到除杂后的麦芽酚晶体，离心后的母液回步骤(1)进行溶料套用，至母液中杂质含量超指标后，排出系统。
经过检测回收的麦芽酚，对粗品回收率为93.2％，回收的麦芽酚纯度为99.3％。
上述实施例中：
溶料釜采用带夹套及搅拌的搪瓷溶料釜；分层槽采用搪瓷分层槽(上部圆形封头，底部锥形)；冷冻釜采用带夹套及搅拌的搪瓷冷冻釜。
现有技术中一般利用溶剂来溶解麦芽酚和乙基麦芽酚升华的产物，随后分离水中的麦芽酚和乙基麦芽酚。本发明与现有技术的区别在于，本发明使用加热后的水溶解麦芽酚和乙基麦芽酚，不使用可能与非极性的有机物混溶的溶剂，将麦芽酚和乙基麦芽酚反萃取到水中后，去除有机相。这种方式能够相较于溶剂脱色提纯法进行脱色提纯，省去了脱色剂的使用，耗费的能源等与原有方式近似，少量的杂质经过分离后可以进行无害化处理；相较于升华处理粗品，本申请耗能少。本申请相较于溶剂脱色提纯法或者升华法处理粗品，收率高。
以上所述，仅为本申请的具体实施方式，在本申请的上述教导下，本领域技术人员可以在上述实施例的基础上进行其他的改进或变形。本领域技术 人员应该明白，上述的具体描述只是更好的解释本申请的目的，本申请的保护范围应以权利要求的保护范围为准。
此外，本领域的技术人员能够理解，尽管在此所述的一些实施例包括其它实施例中所包括的某些特征而不是其它特征，但是不同实施例的特征的组合意味着处于本申请的范围之内并且形成不同的实施例。例如，在下面的权利要求书中，所要求保护的实施例的任意之一都可以以任意的组合方式来使用。

Claims (4)

  1. 一种麦芽酚或乙基麦芽酚升华后粗品反萃取提纯方法，其特征在于，包括以下步骤：
    步骤1：将麦芽酚或乙基麦芽酚升华后粗品与水加热至80±5℃进行溶料；
    步骤2：将步骤1所获得的物料分层静置，分离上层水溶液后，将上层水溶液层温度降至10℃-15℃；
    步骤3：离心得到除杂后的麦芽酚或乙基麦芽酚晶体。
  2. 如权利要求1的麦芽酚或乙基麦芽酚升华后粗品反萃取提纯方法，其特征在于，麦芽酚或乙基麦芽酚与水的质量比为1：6。
  3. 一种麦芽酚或乙基麦芽酚升华后粗品反萃取的提纯装置，其特征在于，包括溶料釜，与溶料釜连接的分层槽，与分层槽连接的冷冻釜，与冷冻釜连接的离心机。
  4. 如权利要求3的麦芽酚或乙基麦芽酚升华后粗品反萃取的提纯装置，其特征在于，溶料釜为搪瓷溶料釜；分层槽为搪瓷分层槽，上部为圆形封头，底部为锥形；冷冻釜为搪瓷冷冻釜。
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