WO2019062816A1 - 一种连续蒸馏工艺 - Google Patents

一种连续蒸馏工艺 Download PDF

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Publication number
WO2019062816A1
WO2019062816A1 PCT/CN2018/107972 CN2018107972W WO2019062816A1 WO 2019062816 A1 WO2019062816 A1 WO 2019062816A1 CN 2018107972 W CN2018107972 W CN 2018107972W WO 2019062816 A1 WO2019062816 A1 WO 2019062816A1
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section
distillation
steam
preheating
drying
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PCT/CN2018/107972
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English (en)
French (fr)
Inventor
齐立军
韩少威
季绍东
李凤飞
杨文江
暴海军
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晨光生物科技集团股份有限公司
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Priority to EP18860317.9A priority Critical patent/EP3690011A4/en
Priority to US16/651,770 priority patent/US11505764B2/en
Publication of WO2019062816A1 publication Critical patent/WO2019062816A1/zh

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/34Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/38Steam distillation
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/001Processes specially adapted for distillation or rectification of fermented solutions
    • B01D3/002Processes specially adapted for distillation or rectification of fermented solutions by continuous methods
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/30Fractionating columns with movable parts or in which centrifugal movement is caused
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/34Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/40Extractive distillation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D5/00Condensation of vapours; Recovering volatile solvents by condensation
    • B01D5/0033Other features
    • B01D5/0036Multiple-effect condensation; Fractional condensation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D5/00Condensation of vapours; Recovering volatile solvents by condensation
    • B01D5/0057Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
    • B01D5/006Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes with evaporation or distillation
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/027Recovery of volatiles by distillation or stripping

Definitions

  • the invention relates to a method for producing volatile essential oil, in particular to a continuous distillation process suitable for heat sensitive materials such as pepper, pepper, cilantro, cinnamon leaf and Chinese fir.
  • Pepper, pepper, cilantro, cinnamon, fir and the like contain a large amount of volatile essential oils, which are important natural plant extracts and play an important role in food, cosmetics and other fields.
  • volatile essential oils are generally extracted by steam distillation.
  • the traditional steam distillation process generally adopts tank group production, which has small processing capacity, long distillation time, low efficiency and easy loss of heat sensitive active ingredients in materials.
  • the technical problem to be solved by the present invention is to provide a continuous distillation process with large processing capacity, high yield of essential oil, and utilization of waste heat, which is particularly suitable for distillation of heat sensitive materials.
  • the technical solution adopted by the present invention is:
  • a continuous distillation process comprises the following steps: placing the material in a multi-layer distillation column, followed by preheating, squeezing, steam distillation, roasting, drying, cooling, and containing essential oil vapor condensation to obtain essential oil.
  • a further improvement of the technical solution of the present invention is that the material is subjected to extrusion and puncturing treatment during the transportation from the preheating section to the steam distillation section.
  • a further improvement of the technical solution of the present invention is that the water vapor-generating water used in the steam distillation is subjected to deoxidation treatment, and the oxygen content is reduced to 0.2 mg/L or less.
  • a further improvement of the technical solution of the present invention is that the preheating and roasting are carried out under nitrogen-passing conditions, the drying is performed by hot nitrogen gas, and the essential oil-containing steam is passed through an air heat exchanger as a heat source of hot nitrogen.
  • a further improvement of the technical solution of the present invention is that the essential oil contains essential oil by means of secondary condensation and water separation, the first condensation temperature is 20-30 ° C, and the secondary condensation temperature is -10 ° C to 5 ° C.
  • the preheating adopts indirect steam heating, the steam pressure is 0.1-0.2 Mpa; the steam distillation adopts direct steam heating, the steam pressure is 0.01-0.05 Mpa; the roasting crucible is heated by indirect steam, and the steam pressure is 0.1-0.4MPa; hot nitrogen drying temperature is 40-80 ° C, pressure is 10-40Kpa; cold air cooling section is normal temperature air, pressure is 10-40Kpa.
  • the treatment object of the present invention is a material containing a large amount of volatile essential oil, and further preferably pepper, pepper, alfalfa, cinnamon or Chinese fir.
  • the multi-layer distillation tower comprises a tower body centrally provided with a rotating shaft, and the tower body comprises a tower body, an upper head and a support, and is separated into preheating by the trays from top to bottom along the tower body.
  • each tray is provided with The feeding auger connecting the upper and lower two spaces, the lower end of the tray of the preheating section and the roasting section is provided with a conduit for indirect heat transfer of steam in contact with the lower surface of the tray, and the trays of the distillation section, the drying section and the cooling section are
  • the sandwich tray, the side of the sandwich tray is provided with a gas inlet, and the upper surface is provided with a gas outlet hole, and the inner gas of the preheating section, the distillation section, the roasting section and the drying section are connected to the collector through the pipeline, and the rotating shaft
  • a machete that acts as a dispersing material and a tumbling material following the rotation of the rotating shaft is disposed.
  • a further improvement of the technical solution of the present invention is that the drying section and the roasting section are connected by a pipeline, and the roasting section and the preheating section are connected by a pipeline, and the hot nitrogen is from the side of the sandwiched tray of the drying section.
  • the gas inlet enters the drying section first, then passes through the roasting section, and finally enters the preheating section, and finally is discharged from the top of the distillation tower into the collector, and the essential oil is recovered by the secondary condensation.
  • a further improvement of the technical solution of the present invention is that the front end of the unloading auger of the preheating section to the distillation section is equipped with a pair of roller machines with sharp cones, and the roller machine is pressed against the material for punching.
  • a further improvement of the technical solution of the present invention is that the multilayer distillation column is provided with 6-9 layers, wherein the preheating section is provided with 1 layer, the steam distillation section is provided with 2 to 4 layers of trays, and the baking section is provided with 1 layer.
  • the layer, the hot nitrogen drying section is provided with 1 to 2 layers, and the cooling section is provided with 1 layer.
  • Another object of the present invention is to protect a multi-stage distillation apparatus having the structure that the multi-layer distillation column comprises a tower body centrally provided with a rotating shaft, the tower body comprising a tower body, an upper head and a support, which are arranged along the tower body Down to the next, the tray is divided into a preheating section, a distillation section, a roasting section, a drying section and a cooling section.
  • the upper end of the tower body is provided with a feeding port communicating with the preheating section, and the lower end of the tower body is arranged to communicate with the cooling section.
  • each of the trays is provided with a feeding auger connecting the upper and lower two spaces, and the lower end of the tray of the preheating section and the roasting section is provided with a conduit for indirect heat transfer of steam in contact with the lower surface of the tray, and the distillation section
  • the trays of the drying section and the cooling section are sandwich trays, the side of the sandwich tray is provided with a gas inlet, the upper surface is provided with a gas outlet hole, the inner gas of the preheating section, the distillation section, the roasting section and the drying section Both are connected to the collector through a pipeline, and the curved shaft is provided with a dispersing material and a tumbling material which follow the rotation of the rotating shaft.
  • a further improvement of the technical solution of the present invention is that the drying section and the roasting section are connected by a pipeline, and the roasting section and the preheating section are connected by a pipeline, and the hot nitrogen is from the side of the sandwiched tray of the drying section.
  • the gas inlet enters the drying section first, then passes through the roasting section, and finally enters the preheating section, and finally is discharged from the top of the distillation tower into the collector, and the essential oil is recovered by the secondary condensation.
  • a further improvement of the technical solution of the present invention is that the front end of the unloading auger of the preheating section to the distillation section is equipped with a pair of roller machines with sharp cones, and the roller machine is pressed against the material for punching.
  • a further improvement of the technical solution of the present invention is that the multilayer distillation column is provided with 6-9 layers, wherein the preheating section is provided with 1 layer, the steam distillation section is provided with 2 to 4 layers of trays, and the baking section is provided with 1 layer.
  • the layer, the hot nitrogen drying section is provided with 1 to 2 layers, and the cooling section is provided with 1 layer.
  • the invention adopts a continuous distillation process, the distillation time is short, and all the steps are closed in the multi-layer distillation tower to avoid the loss of essential oil vapor, and the effect of high efficiency and high yield is achieved.
  • the process oil has a high yield and can reach more than 98%.
  • Preheating, squeezing, multi-stage distillation, roasting and simmering process the distillation effect is good, the material is extruded and punctured in the tower, which can improve the distillation effect, avoid the problem of essential oil emission in the pre-treatment outside the tower, and preheat
  • the essential oils produced by roasting and roasting are also recovered.
  • the effect of squeezing and puncturing is better.
  • the equipment is sealed to reduce the loss of essential oil leakage caused by poor sealing. Reduce the spillage of essential oil by sealing the feed and discharge by installing a air damper.
  • the material is conveyed by the auger between the layers, and the sealing effect is good, which can reduce the loss of the essential oil spilling into other layers.
  • the essential oil After distillation, the essential oil is often condensed and recovered in a mild and low temperature, reducing the amount of essential oil in the exhaust gas.
  • the process is suitable for the treatment of heat sensitive materials.
  • the pepper in the pepper and the piperine in the pepper are easy to be lost under high temperature conditions.
  • the steam is first deoxidized, the oxygen content in the steam is greatly reduced, and the oxidation process is reduced. Loss, other high temperature treatment processes are also carried out under nitrogen protection, which can significantly reduce the loss of heat sensitive components.
  • the process of the material is subjected to distillation treatment, followed by roasting, drying and cooling, which facilitates subsequent processing of the material after distillation.
  • Pepper, pepper, cilantro, laurel, fir and other essential oils contain other flavors and aromas.
  • the steam-distilled materials need to be solvent or supercritical. In the conventional distillation process, after steam distillation, the material will contain a large amount of water, which has a great influence on the next extraction.
  • the process can effectively control the moisture of the material after distillation by adding a drying process after distillation, and can directly carry out the next extraction operation.
  • This process uses steam after distillation as a heat source for hot air, so that the waste heat of steam can be utilized to save energy.
  • the process uses a multi-layer distillation tower to achieve continuous automated production, greatly improving production efficiency and reducing production costs.
  • Figure 1 is a schematic view showing the structure of a multilayer distillation column
  • Figure 2 is a schematic diagram of the structure of the roller machine
  • Figure 3 is a schematic view of the upper surface of the sandwich tray
  • Figure 4 is a schematic view of the structure of the catheter
  • Figure 5 is a plan view of Figure 4.
  • a continuous distillation process comprising the following steps, the material is placed in a multi-layer distillation tower, which is subjected to preheating, extrusion boring, steam distillation, roasting, drying, and cooling treatment, and the essential oil is condensed to obtain essential oil. .
  • the material is extruded and punctured during the transfer process from the preheating section to the steam distillation section, which can improve the distillation effect and avoid the problem of essential oil emission in the pretreatment outside the tower.
  • the water vapor-generating water used in the steam distillation is subjected to deoxidation treatment, and the oxygen content is reduced to 0.2 mg/L or less.
  • the steam deoxygenation method is any one of vacuum deoxidation, thermal deoxidation and chemical deaeration.
  • the preheating and roasting are carried out under nitrogen-passing conditions, and the drying is carried out by hot nitrogen gas, the purity of nitrogen is not less than 99%, and the essential oil vapor is passed through the air heat exchanger as a heat source of hot nitrogen.
  • the preheating section is heated by indirect steam, the steam pressure is 0.1-0.2Mpa; the steam distillation section is heated by direct steam, the steam pressure is 0.01-0.05Mpa; the roasting section is heated by indirect steam, the steam pressure is 0.1-0.4MPa;
  • the section hot nitrogen temperature is 40-80 ° C, the pressure is 10-40 Kpa; the cold air cooling section is normal temperature air, the pressure is 10-40 Kpa.
  • the height of the distillation section is controlled to be between one-third and two-thirds of the height of the tray, and the residence time of the material in the distillation column is 1-3 hours.
  • the essential oil is obtained by separating the essential oil vapor by two-stage condensation, the first-stage condensation temperature is 20-30 ° C, and the second-stage condensation temperature is -10 ° C to 5 ° C.
  • the multi-layer distillation tower is provided with 6-9 layers, wherein the preheating section is provided with 1 layer, the steam distillation section is provided with 2 to 4 trays, the roasting section is provided with 1 layer, and the hot nitrogen drying section is provided with 1 ⁇ 2 floors, the cooling section is set to 1 layer.
  • the specific structure of the multi-layer distillation tower comprises: a tower body, and a rotating shaft 1 is arranged at the center of the tower body, and the rotating shaft 1 is provided with a bending knife which acts as a dispersing material and a tumbling material following the rotation of the rotating shaft 1, and the bending is performed.
  • the knife 10 is placed between the trays.
  • the tower body comprises a tower body 2, an upper head 3 and a support 4, and is separated into a preheating section, a distillation section, a roasting section, a drying section and a cooling section through the tray along the tower body from the top to the bottom, and the upper end of the tower body
  • the feed port is connected with the preheating section, and the feed port at the upper end of the tower body is connected to the feed scraper 6 through the feed auger 5, and the feed auger 5 and the feed scraper 6 are disposed between
  • the air closing device 11 is provided with a discharge port communicating with the cooling section at the lower end of the tower body, and a lower scraper machine 7 is connected to the lower end of the discharge port at the lower end of the tower body, and each of the trays is provided with a material for connecting the upper and lower spaces.
  • Auger 8 is provided with a discharge port communicating with the cooling section at the lower end of the tower body, and a lower scraper machine 7 is connected to the lower end of the discharge port at the lower end of the tower
  • the lower end of the tray of the preheating section and the roasting section is provided with a conduit 9 for indirect heat transfer of steam in contact with the lower surface of the tray, and the conduit 9 of the lower surface of the tray of the preheating section and the roasting section is an inverted triangle, the conduit 9 repeatedly bent over the lower surface of the tray, that is, the conduit 9 extends from a point on the circumference of the lower surface of the tray to another point on the circumference, and then folded back, and the conduit 9 between the folded back and the conduit Keep it in parallel, so that it is repeatedly bent and finally covered on the lower surface of the tower.
  • the inlet of the conduit 9 on the lower surface of the tray of the preheating section and the roasting section is in communication with the steam conduit, and the outlet is connected to the steam condensate storage tank.
  • the trays of the distillation section, the drying section and the cooling section are sandwich trays, the side of the sandwich tray is provided with a gas inlet 12, and the upper surface is provided with a gas outlet hole 13.
  • the gas inlet 12 of the distillation section is connected to a steam line, and a steam outlet 14 is provided on the side wall of the distillation section, and the steam outlet 14 is connected to the collector.
  • the gas inlet 12 of the sandwich tray of the drying section is connected to the blower through a nitrogen gas transmission pipeline, wherein the essential oil vapor is passed through the air heat exchanger as a heat source of hot nitrogen, and the heat is not required to be set on the hot air conveying pipeline. The heat exchanger continues to heat the nitrogen to meet the requirements.
  • the drying section and the roasting section are connected by a pipeline, and the roasting section and the preheating section are connected through a pipeline, and the hot nitrogen gas enters the drying section from the gas inlet 12 on the side of the sandwich tray of the drying section, and then passes through the roasting section, and finally Entering the preheating section, it is finally discharged from the top of the distillation tower into the collector, and the essential oil is recovered by secondary condensation.
  • the collector includes a dry trap, a condenser, and a liquid collection tank that are connected in sequence.
  • the gas inlet 12 of the sandwich tray of the cooling section is supplied with cold air, and the cold air enters the cooling section through the gas outlet hole 13.
  • an exhaust port 15 is provided, the exhaust port 15 and the cyclone and The purifier is connected to the outside air.
  • the front end of the unloading auger 8 of the preheating section to the distillation section is equipped with a counter-roller with a pointed cone.
  • the counter-roller comprises two peripherally opposed rollers, the roller is arranged with a pointed cone, and the roller machine is pressed against the material. Hole handling.
  • the invention discloses a continuous distillation process, belonging to a production method of volatile essential oil, comprising the following steps: putting the material into a multi-layer distillation tower, followed by preheating, squeezing, steam distillation, roasting, drying, Cooling treatment, containing essential oil vapor condensation to obtain essential oil.
  • the invention has the advantages of large processing capacity, high yield of essential oil and utilization of waste heat, and is particularly suitable for distillation of heat sensitive materials.

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  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
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  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Fats And Perfumes (AREA)

Abstract

一种连续蒸馏工艺,包括以下步骤:将物料放入多层蒸馏塔中依次经过预热、挤压扎孔、水蒸汽蒸馏、烤粕,干燥、降温处理,含精油蒸汽冷凝分水得到精油。

Description

一种连续蒸馏工艺 技术领域
本发明涉及一种挥发性精油的生产方法,尤其是一种适用于花椒、胡椒、桉叶、桂叶、杉木等热敏性物料的连续蒸馏工艺。
背景技术
花椒、胡椒、桉叶、桂叶、杉木等含有大量的挥发性精油,是重要的天然植物提取物,在食品、化妆品等领域具有重要作用。
目前挥发性精油普遍采用水蒸气蒸馏工艺提取,传统的水蒸气蒸馏工艺一般采用罐组式生产,处理能力小,蒸馏时间长,效率低且易造成物料中热敏性有效成分的损失。
公告号为CN101721831B的专利中,公开了一种差压式固态连续蒸馏工艺,采用预热、强化蒸馏、残蒸三步处理,但主要适用于分离酒精。无法控制蒸馏后物料水分和温度,不适于含热敏性成品物料的蒸馏,也不利于蒸馏后物料的下一步溶剂提取。
目前市场上对挥发性精油的需求量越来越大,急需一种经济高效,适于大规模工业生产的连续水蒸气蒸馏精油的方法。
发明内容
本发明需要解决的技术问题是提供一种连续蒸馏工艺,处理能力大,精油得率高,余热得到利用,特别适于热敏性物料的蒸馏。
为解决上述技术问题,本发明所采用的技术方案是:
一种连续蒸馏工艺,包括以下步骤,将物料放入多层蒸馏塔中依次经过预热、挤压扎孔、水蒸汽蒸馏、烤粕,干燥、降温处理,含精油蒸汽冷凝分水得到精油。
本发明技术方案的进一步改进在于:物料在预热段至水蒸汽蒸馏段传输过程中经挤压、扎孔处理。
本发明技术方案的进一步改进在于:所述水蒸气蒸馏中用到的产生水 蒸气的水经过脱氧处理,含氧量降至0.2mg/L以下。
本发明技术方案的进一步改进在于:所述预热、烤粕都在通氮条件下进行,所述干燥采用热氮气干燥,所述含精油蒸汽通过空气换热器作为热氮气的热源。
本发明技术方案的进一步改进在于:所述含精油蒸汽经二级冷凝分水得到精油,一级冷凝温度为20-30℃,二级冷凝温度为-10℃到5℃。
本发明技术方案的进一步改进在于:预热采用间接蒸汽加热,蒸汽压力为0.1-0.2Mpa;水蒸气蒸馏采用直接蒸汽加热,蒸汽压力为0.01-0.05Mpa;烤粕采用间接蒸汽加热,蒸汽压力为0.1-0.4MPa;热氮气干燥温度为40-80℃,压力为10-40Kpa;冷风降温段为常温空气,压力为10-40Kpa。
优选的,本发明的处理对象为含有大量的挥发性精油的物料,进一步优选花椒、胡椒、桉叶、桂叶或杉木。
本发明技术方案的进一步改进在于:多层蒸馏塔包括中心设置转轴的塔体,塔体包括塔身、上封头和支座,沿着塔体由上到下依次通过塔板分隔成预热段、蒸馏段、烤粕段、干燥段和冷却段,塔体上端设置有与预热段连通的进料口,塔体下端设置与冷却段连通的出料口,每个塔板上设置有连通上下两个空间的下料绞龙,预热段和烤粕段的塔板下端设置有与塔板下表面接触实现蒸汽间接传热的导管,蒸馏段、干燥段和冷却段的塔板为夹层式塔板,夹层式塔板的侧面设置有气体入口、上表面设置有气体出孔,预热段、蒸馏段、烤粕段和干燥段的内气体均通过管路与收集器连接,转轴上设置有跟随转轴转动的起分散物料和翻腾物料作用的弯刀。
本发明技术方案的进一步改进在于:所述干燥段和烤粕段通过管路连通,所述烤粕段和预热段通过管路连通,所述热氮气由干燥段的夹层式塔板侧面的气体入口先进入干燥段,再通过烤粕段,最后进入预热段,最终从蒸馏塔顶部排出进入收集器,经二级冷凝回收精油。
本发明技术方案的进一步改进在于:所述预热段至蒸馏段的下料绞龙 前端安装带有尖锥的对辊机,对辊机对物料挤压扎孔处理。
本发明技术方案的进一步改进在于:所述多层蒸馏塔设置有6~9层,其中预热段设置有1层、水蒸气蒸馏段设置有2~4层塔板,烤粕段设置有1层,热氮气干燥段设置有1~2层,冷却段设置有1层。
本发明的另一目的是保护一种多段蒸馏的装置,其结构为:多层蒸馏塔包括中心设置转轴的塔体,塔体包括塔身、上封头和支座,沿着塔体由上到下依次通过塔板分隔成预热段、蒸馏段、烤粕段、干燥段和冷却段,塔体上端设置有与预热段连通的进料口,塔体下端设置与冷却段连通的出料口,每个塔板上设置有连通上下两个空间的下料绞龙,预热段和烤粕段的塔板下端设置有与塔板下表面接触实现蒸汽间接传热的导管,蒸馏段、干燥段和冷却段的塔板为夹层式塔板,夹层式塔板的侧面设置有气体入口、上表面设置有气体出孔,预热段、蒸馏段、烤粕段和干燥段的内气体均通过管路与收集器连接,转轴上设置有跟随转轴转动的起分散物料和翻腾物料作用的弯刀。
本发明技术方案的进一步改进在于:所述干燥段和烤粕段通过管路连通,所述烤粕段和预热段通过管路连通,所述热氮气由干燥段的夹层式塔板侧面的气体入口先进入干燥段,再通过烤粕段,最后进入预热段,最终从蒸馏塔顶部排出进入收集器,经二级冷凝回收精油。
本发明技术方案的进一步改进在于:所述预热段至蒸馏段的下料绞龙前端安装带有尖锥的对辊机,对辊机对物料挤压扎孔处理。
本发明技术方案的进一步改进在于:所述多层蒸馏塔设置有6~9层,其中预热段设置有1层、水蒸气蒸馏段设置有2~4层塔板,烤粕段设置有1层,热氮气干燥段设置有1~2层,冷却段设置有1层。
由于采用了上述技术方案,本发明取得的技术进步是:
本发明采用连续蒸馏工艺,蒸馏时间短,且所有步骤都是在多层蒸馏塔内封闭进行,避免精油蒸汽损失,达到高效率、高收率的效果。
本工艺精油得率高,可达到98%以上。采用预热、挤压扎孔、多级 蒸馏、烤粕工艺,蒸馏效果好,物料在塔内进行挤压和扎孔,可提高蒸馏效果,避免塔外前处理存在的精油散发问题,预热和烤粕产生的精油也得到回收。且将挤压扎孔设置在预热段之后,确保挤压、扎孔的效果发挥的更好。同时加强设备密封,减少因密封不严导致的精油外泄损失。通过安装闭风器对进料和出料进行密封,减少精油外溢。各层间通过下料绞龙传送物料,密封效果较好,可减少精油溢到其它层的损失。蒸馏后精油经常温和低温两级冷凝回收,减少了尾气中的精油含量。
本工艺适于热敏性物料的处理,花椒中麻素和胡椒中的胡椒碱等在高温条件下都易损失,先将制蒸汽用水先经脱氧处理,大幅降低蒸汽中含氧量,减少蒸馏过程氧化损失,其它高温处理过程也在氮气保护下进行,可显著减少热敏性成分损失。
本工艺对物料进行蒸馏处理后依次经过烤粕、烘干和冷却,便于蒸馏后物料的后续处理。花椒、胡椒、桉叶、桂叶、杉木等除精油外还含有其它风味、香味物质,经水蒸气蒸馏后的物料还需要再进行溶剂或超临界提取。常规的蒸馏工艺在水蒸气蒸馏后,物料中会含有大量的水分,对下一步的提取造成很大影响。本工艺通过在蒸馏后增加干燥工序,使蒸馏后物料的水分得到有效控制,可直接进行下一步提取操作。
本工艺使用蒸馏后蒸汽作为热风的热源,使蒸汽余热得到利用,可节约能源。
本工艺使用多层蒸馏塔,实现了连续自动化生产,大幅提高生产效率,降低了生产成本。
附图说明
图1是多层蒸馏塔的结构示意图;
图2是对辊机结构原理图;
图3是夹层式塔板的上表面示意图;
图4是导管结构示意图;
图5是图4的俯视图;
其中,1、转轴,2、塔身,3、上封头,4、支座,5、进料绞龙,6、进料刮板机,7、下料刮板机,8、下料绞龙,9、导管,10、弯刀,11、闭风器,12、气体入口,13、气体出孔,14、蒸汽出口,15、排气口。
具体实施方式
下面结合实施例对本发明做进一步详细说明:
一种连续蒸馏工艺,具体包括以下步骤,将物料放入多层蒸馏塔中依次经过预热、挤压扎孔、水蒸汽蒸馏、烤粕,干燥、降温处理,含精油蒸汽冷凝分水得到精油。
其中物料在预热段至水蒸汽蒸馏段传输过程中经挤压、扎孔处理,可提高蒸馏效果,避免塔外前处理存在的精油散发问题。
其中水蒸气蒸馏中用到的产生水蒸气的水经过脱氧处理,含氧量降至0.2mg/L以下。制蒸汽用水除氧方式为真空除氧、热力除氧和化学除氧中的任一种。
预热、烤粕都在通氮条件下进行,干燥采用热氮气干燥,氮气纯度不低于99%,含精油蒸汽通过空气换热器作为热氮气的热源。
预热段采用间接蒸汽加热,蒸汽压力为0.1-0.2Mpa;水蒸气蒸馏段采用直接蒸汽加热,蒸汽压力为0.01-0.05Mpa;烤粕段采用间接蒸汽加热,蒸汽压力为0.1-0.4MPa;干燥段热氮气温度为40-80℃,压力为10-40Kpa;冷风降温段为常温空气,压力为10-40Kpa。蒸馏段料层高度控制在塔板高度的三分之一到三分之二,物料在蒸馏塔内停留时间为1-3小时。
含精油蒸汽经二级冷凝分水得到精油,一级冷凝温度为20-30℃,二级冷凝温度为-10℃到5℃。
其中多层蒸馏塔设置有6~9层,其中预热段设置有1层、水蒸气蒸馏段设置有2~4层塔板,烤粕段设置有1层,热氮气干燥段设置有1~2层,冷却段设置有1层。
如图1~5所示,多层蒸馏塔的具体结构为:包括塔体,塔体中心设置转轴1,转轴1上设置有跟随转轴1转动的起分散物料和翻腾物料作用 的弯刀,弯刀10设置在塔板之间。塔体包括塔身2、上封头3和支座4,沿着塔体由上到下依次通过塔板分隔成预热段、蒸馏段、烤粕段、干燥段和冷却段,塔体上端设置有与预热段连通的进料口,塔体上端的进料口通过进料绞龙5与进料刮板机6连接,进料绞龙5和进料刮板机6之间设置有闭风器11,塔体下端设置与冷却段连通的出料口,塔体下端的出料口下端连接有下料刮板机7,每个塔板上设置有连通上下两个空间的下料绞龙8。
预热段和烤粕段的塔板下端设置有与塔板下表面接触实现蒸汽间接传热的导管9,预热段和烤粕段的塔板下表面的导管9横截面为倒三角形,导管9反复弯折的布满在塔板下表面,即导管9由塔板下表面一个圆周上的点为起点向圆周上另一个点延伸,然后折回,折回后的导管9与之间的一段导管保持平行布置,如此反复弯折,最终布满在塔体下表面。预热段和烤粕段的塔板下表面的导管9入口与蒸汽管道连通,出口与蒸汽泠凝水储罐连接。
蒸馏段、干燥段和冷却段的塔板为夹层式塔板,夹层式塔板的侧面设置有气体入口12、上表面设置有气体出孔13。蒸馏段的气体入口12与蒸汽管道相连,蒸馏段侧壁上设置有蒸汽出口14,蒸汽出口14与收集器连接。烘干段的夹层式塔板的气体入口12通过氮气输送管路与鼓风机连接,其中含精油蒸汽通过空气换热器作为热氮气的热源,热度达不到要求时在热风输送管路上设置有换热器,对氮气继续加热以满足要求。干燥段和烤粕段通过管路连通,烤粕段和预热段通过管路连通,热氮气由干燥段的夹层式塔板侧面的气体入口12先进入干燥段,再通过烤粕段,最后进入预热段,最终从蒸馏塔顶部排出进入收集器,经二级冷凝回收精油。收集器包括依次连接的干式捕集器、冷凝器和集液灌。冷却段的夹层式塔板的气体入口12通入冷空气,冷空气通过气体出孔13进入冷却段中,在冷却段侧壁上设置有排气口15,排气口15与旋风分离器和净化器连接后与外部空气连通。
其中预热段至蒸馏段的下料绞龙8前端安装带有尖锥的对辊机,对辊机包括两个外周相对的辊子,辊子上布置有尖锥,对辊机对物料挤压扎孔处理。
实施例1
取500kg精油含量6.5%的花椒,经单层预热段预热,蒸汽压力0.1MPa;双层水蒸馏气蒸馏段蒸馏,蒸汽压力分别是0.01Mpa、0.02Mpa;单层烤粕段烤粕,蒸汽压力0.1MPa;单层热氮气干燥段干燥,温度40℃,压力10Kpa;单层冷风段处理,含精油蒸汽经二级冷凝,一级冷凝温度30℃,二级冷凝温度5℃。共得到精油31.85L,精油得率98.0%。
实施例2
取800kg精油含量5.0%的胡椒,经单层预热段预热,蒸汽压力0.2MPa;四层水蒸馏气蒸馏段蒸馏,蒸汽压力分别是0.01Mpa、0.02Mpa、0.04Mpa、0.05Mpa;单层烤粕段烤粕,蒸汽压力0.4MPa;双层热氮气干燥段干燥,温度60℃和80℃,压力20Kpa和40Kpa;单层冷风段处理,含精油蒸汽经二级冷凝,一级冷凝温度20℃,二级冷凝温度-10℃。共得到精油39.80L,精油得率99.5%。
实施例3
取400kg精油含量12.5%的花椒,经单层预热段预热,蒸汽压力0.15MPa;三层水蒸馏气蒸馏段蒸馏,蒸汽压力分别是0.01Mpa、0.03Mpa、0.04Mpa;单层烤粕段烤粕,蒸汽压力0.3MPa;单层热氮气干燥段干燥,温度60℃,压力30Kpa;单层冷风段处理,含精油蒸汽经二级冷凝,一级冷凝温度25℃,二级冷凝温度0℃共得到精油49.55L,精油得率99.1%。
工业实用性
本发明公开了一种连续蒸馏工艺,属于挥发性精油的生产方法,包括以下步骤,将物料放入多层蒸馏塔中依次经过预热、挤压扎孔、水蒸汽蒸馏、烤粕,干燥、降温处理,含精油蒸汽冷凝分水得到精油。本发明处理能力大,精油得率高,余热得到利用,特别适于热敏性物料的蒸馏。

Claims (10)

  1. 一种连续蒸馏工艺,其特征在于:包括以下步骤,将物料放入多层蒸馏塔中依次经过预热、挤压扎孔、水蒸汽蒸馏、烤粕,干燥、降温处理,含精油蒸汽冷凝分水得到精油。
  2. 根据权利要求1所述的一种连续蒸馏工艺,其特征在于:物料在预热段至水蒸汽蒸馏段传输过程中经挤压、扎孔处理。
  3. 根据权利要求1所述的一种连续蒸馏工艺,其特征在于:所述水蒸气蒸馏中用到的产生水蒸气的水经过脱氧处理,含氧量降至0.2mg/L以下。
  4. 根据权利要求1所述的一种连续蒸馏工艺,其特征在于:所述预热、烤粕都在通氮条件下进行,所述干燥采用热氮气干燥,所述含精油蒸汽通过空气换热器作为热氮气的热源。
  5. 根据权利要求1所述的一种连续蒸馏工艺,其特征在于:所述含精油蒸汽经二级冷凝分水得到精油,一级冷凝温度为20-30℃,二级冷凝温度为-10℃到5℃。
  6. 根据权利要求1所述的一种连续蒸馏工艺,其特征在于:预热采用间接蒸汽加热,蒸汽压力为0.1-0.2Mpa;水蒸气蒸馏采用直接蒸汽加热,蒸汽压力为0.01-0.05Mpa;烤粕采用间接蒸汽加热,蒸汽压力为0.1-0.4MPa;热氮气干燥温度为40-80℃,压力为10-40Kpa;冷风降温段为常温空气,压力为10-40Kpa。
  7. 根据权利要求1所述的一种连续蒸馏工艺,其特征在于:多层蒸馏塔包括中心设置转轴(1)的塔体,塔体包括塔身(2)、上封头(3)和支座(4),沿着塔体由上到下依次通过塔板分隔成预热段、蒸馏段、烤粕段、干燥段和冷却段,塔体上端设置有与预热段连通的进料口,塔体下端设置与冷却段连通的出料口,每个塔板上设置有连通上下两个空间的下料绞龙(8),预热段和烤粕段的塔板下端设置有与塔板下表面接触实现蒸汽间接传热的导管(9),蒸馏段、干燥段和冷却段的塔板为夹层式塔板,夹 层式塔板的侧面设置有气体入口(12)、上表面设置有气体出孔(13),预热段、蒸馏段、烤粕段和干燥段的内气体均通过管路与收集器连接,转轴(1)上设置有跟随转轴(1)转动的起分散物料和翻腾物料作用的弯刀(10)。
  8. 根据权利要求7所述的一种连续蒸馏工艺,其特征在于:所述干燥段和烤粕段通过管路连通,所述烤粕段和预热段通过管路连通,所述热氮气由干燥段的夹层式塔板侧面的气体入口(12)先进入干燥段,再通过烤粕段,最后进入预热段,最终从蒸馏塔顶部排出进入收集器,经二级冷凝回收精油。
  9. 根据权利要求7所述的一种连续蒸馏工艺,其特征在于:所述预热段至蒸馏段的下料绞龙(8)前端安装带有尖锥的对辊机,对辊机对物料挤压扎孔处理。
  10. 根据权利要求7所述的一种连续蒸馏工艺,其特征在于:所述多层蒸馏塔设置有6~9层,其中预热段设置有1层、水蒸气蒸馏段设置有2~4层塔板,烤粕段设置有1层,热氮气干燥段设置有1~2层,冷却段设置有1层。
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