CN201276512Y - Apparatus for separating gamma-terpinene and p-cymene by eucalyptus oil climbing film fractionating tower - Google Patents
Apparatus for separating gamma-terpinene and p-cymene by eucalyptus oil climbing film fractionating tower Download PDFInfo
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- CN201276512Y CN201276512Y CNU2008200812998U CN200820081299U CN201276512Y CN 201276512 Y CN201276512 Y CN 201276512Y CN U2008200812998 U CNU2008200812998 U CN U2008200812998U CN 200820081299 U CN200820081299 U CN 200820081299U CN 201276512 Y CN201276512 Y CN 201276512Y
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- eucalyptus oil
- eucalyptus
- terpinene
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- HFPZCAJZSCWRBC-UHFFFAOYSA-N p-cymene Chemical compound CC(C)C1=CC=C(C)C=C1 HFPZCAJZSCWRBC-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 239000010642 eucalyptus oil Substances 0.000 title claims description 12
- 229940044949 eucalyptus oil Drugs 0.000 title claims description 12
- YKFLAYDHMOASIY-UHFFFAOYSA-N γ-terpinene Chemical compound CC(C)C1=CCC(C)=CC1 YKFLAYDHMOASIY-UHFFFAOYSA-N 0.000 title abstract description 20
- 230000009194 climbing Effects 0.000 title 1
- 238000005194 fractionation Methods 0.000 claims abstract description 16
- 238000010992 reflux Methods 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract 5
- 230000000630 rising effect Effects 0.000 claims description 5
- 238000003466 welding Methods 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims 3
- 241000282326 Felis catus Species 0.000 claims 1
- 238000009413 insulation Methods 0.000 claims 1
- 230000000452 restraining effect Effects 0.000 claims 1
- 239000011800 void material Substances 0.000 claims 1
- WEEGYLXZBRQIMU-UHFFFAOYSA-N 1,8-cineole Natural products C1CC2CCC1(C)OC2(C)C WEEGYLXZBRQIMU-UHFFFAOYSA-N 0.000 abstract description 13
- WEEGYLXZBRQIMU-WAAGHKOSSA-N Eucalyptol Chemical compound C1C[C@H]2CC[C@]1(C)OC2(C)C WEEGYLXZBRQIMU-WAAGHKOSSA-N 0.000 abstract description 13
- 229960005233 cineole Drugs 0.000 abstract description 13
- 238000000034 method Methods 0.000 abstract description 10
- 239000000341 volatile oil Substances 0.000 abstract description 8
- 239000010779 crude oil Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000009833 condensation Methods 0.000 abstract description 2
- 230000005494 condensation Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 244000166124 Eucalyptus globulus Species 0.000 abstract 2
- 241000219927 Eucalyptus Species 0.000 description 13
- GRWFGVWFFZKLTI-IUCAKERBSA-N (-)-α-pinene Chemical compound CC1=CC[C@@H]2C(C)(C)[C@H]1C2 GRWFGVWFFZKLTI-IUCAKERBSA-N 0.000 description 4
- 241000233855 Orchidaceae Species 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- MVNCAPSFBDBCGF-UHFFFAOYSA-N alpha-pinene Natural products CC1=CCC23C1CC2C3(C)C MVNCAPSFBDBCGF-UHFFFAOYSA-N 0.000 description 2
- 229930007927 cymene Natural products 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- GRWFGVWFFZKLTI-UHFFFAOYSA-N rac-alpha-Pinene Natural products CC1=CCC2C(C)(C)C1C2 GRWFGVWFFZKLTI-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 description 1
- 241000723346 Cinnamomum camphora Species 0.000 description 1
- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Natural products C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000001754 anti-pyretic effect Effects 0.000 description 1
- 239000002221 antipyretic Substances 0.000 description 1
- 229930008380 camphor Natural products 0.000 description 1
- 229960000846 camphor Drugs 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- -1 cyclic monoterpene Chemical class 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 235000001510 limonene Nutrition 0.000 description 1
- 229940087305 limonene Drugs 0.000 description 1
- 229930003658 monoterpene Natural products 0.000 description 1
- 235000002577 monoterpenes Nutrition 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000001256 steam distillation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
本实用新型属于生产桉叶精油的分馏塔。它在普通分馏塔分凝器与分馏塔顶之间设置换热面积为50-70%的冷凝回流通道,即在管板塔盘上均匀设置与塔的气体流向一致的换热管束,管束的布管面积为塔盘面积的35%。本实用新型保持了原工艺条件,降低了γ-松油烯和对伞花烃的挥发量,扩大了桉原油中各组份的相对挥发度,使一次分馏桉叶素含量达到了80%以上,分离度高,成本低,避免了新增设备造成的材料耗费,尤其在生产上已取得了良好的效果。
The utility model belongs to a fractionation tower for producing eucalyptus essential oil. It sets a condensation reflux channel with a heat exchange area of 50-70% between the decondenser of the ordinary fractionation tower and the top of the fractionation tower, that is, uniformly arranges heat exchange tube bundles consistent with the gas flow direction of the tower on the tube plate tray. The pipe layout area is 35% of the tray area. The utility model maintains the original process conditions, reduces the volatilization of γ-terpinene and p-cymene, expands the relative volatility of each component in eucalyptus crude oil, and makes the content of eucalyptol in one fractionation reach more than 80%. , high separation, low cost, avoiding material consumption caused by new equipment, especially in production has achieved good results.
Description
技术领域 technical field
本实用新型属于生产桉叶精油的升膜式分馏塔。The utility model belongs to a rising film type fractionation tower for producing eucalyptus essential oil.
背景技术 Background technique
桉叶油是用桉树叶经水蒸汽蒸馏后得到的挥发油,桉叶素是重要的环单萜氧化物,沸点176℃,常温下为无色液体,具有类樟脑的强烈的清凉香气。具有解热,抗菌消炎作用。我国目前生产的桉叶油一般作为原料出口,主要产品是80%的桉叶油。除其他的理化指标外,最重要的一个指标是桉叶素的含量必须达到80%以上。一般用兰桉叶蒸馏得的桉叶油中桉叶素含量在60%左右,使用目前再沸器加热的桉叶油升膜分馏塔,一次获得纯兰桉油桉叶素的含量80%以上并不困难。由于直干兰桉生长迅速,木材好,出油率高,现已取代兰桉成为云南生产桉叶油的重要原料。在直干兰桉蒸馏的桉叶原油各成分百分比中,α-蒎烯11~13%、苧烯6~8%、桉叶素60~63%,γ-松油烯3~5%、对伞花烃1.5~3%,其中,α-蒎烯含量比纯兰桉明显偏少,而γ-松油烯和对伞花烃大幅增高。在这种改变中,γ-松油烯和对伞花烃与桉叶素组分结构相似,分子量相近,沸点相差小,它导致在分馏过程中,随着气液组分中摩尔分数的改变,各组分的相对挥发度差别太小,形成了接近恒沸点的体系,一次分馏桉叶素含量只能达到76~79%之间,很难一次获得80%含量的合格品。要使桉叶素含量达到80%以上,如果按传统方法解决,或者增加塔板数而使分馏塔加高最少1.5倍以上,即使原来6米塔节增加到15米以上,成为庞大复杂的设备;或是用超大回流比缓慢多截除一些头段蒎烯,时间将延长一倍左右,增大了能耗、降低了效率、香气品质下降,而目前常用一个方法是将第一次分馏取得的精油再次进行分馏或用纯兰桉分馏的精油渗兑。Eucalyptus oil is a volatile oil obtained by steam distillation of eucalyptus leaves. Eucalyptol is an important cyclic monoterpene oxide with a boiling point of 176°C. It is a colorless liquid at room temperature and has a strong and cool aroma like camphor. Has antipyretic, antibacterial and anti-inflammatory effects. The eucalyptus oil currently produced in my country is generally exported as a raw material, and the main product is 80% eucalyptus oil. In addition to other physical and chemical indicators, the most important indicator is that the content of eucalyptol must reach more than 80%. Generally, the content of eucalyptol in eucalyptol oil obtained by distilling eucalyptus leaves is about 60%. Using the eucalyptus oil rising film fractionation tower heated by the current reboiler, the content of eucalyptol in pure eucalyptus oil is more than 80% at one time. It's not difficult. Due to the rapid growth of direct-dried Eucalyptus eucalyptus, good wood and high oil yield, it has replaced Eucalyptus orchid as an important raw material for the production of eucalyptus oil in Yunnan. In the eucalyptus crude oil distilled from straight-dried Eucalyptus orchids, α-pinene 11-13%, limonene 6-8%, eucalyptol 60-63%, γ-terpinene 3-5%, p- The content of cymene is 1.5-3%. Among them, the content of α-pinene is significantly less than that of pure Eucalyptus, while the content of γ-terpinene and p-cymene are greatly increased. In this change, the structure of γ-terpinene and p-cymene is similar to that of eucalyptol, the molecular weight is similar, and the difference in boiling point is small, which leads to the change of mole fraction in gas-liquid components during the fractionation process , the relative volatility difference of each component is too small, forming a system close to the constant boiling point, the eucalyptol content of one fractionation can only reach between 76% and 79%, and it is difficult to obtain a qualified product with 80% content at one time. To make the content of eucalyptol reach more than 80%, if it is solved according to the traditional method, or the number of trays is increased to increase the height of the fractionation tower by at least 1.5 times, even if the original 6-meter tower section is increased to more than 15 meters, it will become a huge and complicated equipment. ; Or use super large reflux ratio to slowly cut off some head pinenes, the time will be extended by about one time, which will increase energy consumption, reduce efficiency, and reduce aroma quality. At present, a commonly used method is to obtain The essential oil is fractionated again or infiltrated with pure eucalyptus fractionated essential oil.
发明内容 Contents of the invention
本实用新型的目的是在维持原有工艺条件下,并且基本不改变原有设备,通过一次分馏流程来降低γ-松油烯和对伞花烃的挥发,以扩大直杆兰桉原油中桉叶素的相对挥发度,有效地提高桉叶素在精油中的含量。The purpose of this utility model is to reduce the volatilization of γ-terpinene and cymene through a fractionation process while maintaining the original process conditions and basically without changing the original equipment, so as to expand the concentration of eucalyptus in the crude oil of straight eucalyptus orchids. The relative volatility of leaf elements can effectively increase the content of eucalyptol in essential oils.
本实用新型通过以下方式实现:The utility model is realized in the following ways:
(1)在分馏塔的分凝器(105)与分馏塔顶(108)之间设置换热面积为升膜再沸器(101)截面积50-70%的冷凝回流通道(107),即在管板塔盘上均匀设置与塔的气体流向一致的换热管束(107-4),管束(107-4)的布管面积为塔盘面积的35%;(1) between the fractional condenser (105) and the fractionation tower top (108) of the fractionating tower, the heat exchange area is set to be the condensation reflux channel (107) of 50-70% cross-sectional area of the rising film reboiler (101), namely A heat exchange tube bundle (107-4) consistent with the gas flow direction of the tower is evenly arranged on the tube plate tray, and the tube layout area of the tube bundle (107-4) is 35% of the area of the tray;
(2)冷凝回流通道(107)到分凝器(105)联通装置是一个两端用与原塔相同的法兰盘焊接高度不低于塔径50%一个保温良好的空塔节(106)。(2) The connecting device between the condensing return channel (107) and the partial condenser (105) is a well-insulated empty tower section (106) with flanges welded at both ends and the height not lower than 50% of the tower diameter. .
所述的塔径为500mm时,25的管子数目为145~150根,同时管子的长度与塔径的比为1∶(1~1.2)。When the tower diameter is 500mm, The number of 25 tubes is 145-150, and the ratio of the length of the tubes to the diameter of the tower is 1: (1-1.2).
所述的管束在管板上的排列方式为等边三角形,正方形,或同心圆形。The arrangement of the tube bundles on the tube sheet is an equilateral triangle, a square, or a concentric circle.
在以上方式中,由于一般通径小于塔径通道15%左右填料塔压降就会明显增加,所以本实用新型的布管面积不小于塔盘面积的35%。其次,换热面积在加热面积的50-70%之间,可以最大的减少塔体总的阻力和压降,避免能耗升高。再次,装置通道过短,无法有效换能降低γ-松油烯和对伞花烃的气体分子热运动;装置通道过长,将过度冷却,将不必要的分子成分也带到塔釜中,因而我们将该装置长度控制在1∶1~1.2之间。In the above method, because the general diameter is less than about 15% of the tower diameter channel, the pressure drop of the packed tower will obviously increase, so the pipe layout area of the utility model is not less than 35% of the tray area. Secondly, the heat exchange area is between 50-70% of the heating area, which can minimize the total resistance and pressure drop of the tower body and avoid the increase of energy consumption. Again, the channel of the device is too short to effectively convert energy to reduce the thermal movement of gas molecules of γ-terpinene and p-cymene; the channel of the device is too long, which will cause excessive cooling and bring unnecessary molecular components into the tower kettle. Therefore, we control the length of the device between 1:1 and 1.2.
本实用新型已经在生产上取得了良好的效果。实践证明:本装置基本保持了原有工艺条件,γ-松油烯和对伞花烃易于在此过程中被液化富集,较大幅度地降低了γ-松油烯和对对伞花烃的挥发,使大部γ-松油烯、对聚伞花烃富集到脚油中,扩大了直杆兰桉原油中各组份的相对挥发度,使一次分馏结果桉叶素含量都在80~83%之间,有效地提高了桉叶素在精油中的含量,保证了桉叶精油的一次合格率。提高桉叶油分馏塔效率,降低了成本,降低了能耗保证了香气品质,避免了设备投资造成的材料耗费。The utility model has achieved good results in production. Practice has proved that: the device basically maintains the original process conditions, γ-terpinene and p-cymene are easy to be liquefied and enriched in this process, and the γ-terpinene and p-cymene are greatly reduced. The volatilization of most of γ-terpinene and p-cymene enriches the foot oil, expands the relative volatility of each component in the crude oil of Eucalyptus orchid, and makes the content of eucalyptol in the result of a fractionation Between 80% and 83%, the content of eucalyptol in the essential oil is effectively increased, and the first pass rate of the eucalyptus essential oil is guaranteed. Improve the efficiency of the eucalyptus oil fractionation tower, reduce the cost, reduce the energy consumption, ensure the aroma quality, and avoid the material consumption caused by equipment investment.
附图说明 Description of drawings
图1为本实用新型整体示意图。其中包括,桉叶油蒸发釜100、再沸器101、填料及塔节102、103、回流分配器104、分凝器105、空塔节106、冷凝回流通道107、塔顶及导流管108、螺旋板冷凝器109、蛇管冷凝器110。Fig. 1 is the overall schematic diagram of the utility model. Including,
图2(a)为本实用新型冷凝回流通道结构图。Fig. 2(a) is a structural diagram of the condensate return channel of the utility model.
图2中(b)、(c)分别是本实用新型冷凝回流通道俯视图和空塔节俯视图。其中,107-1是设备接口法兰盘、107-2是冷却水进口、107-3是冷凝水出口、107-4是换热管束、106是空塔节、106-1是空塔节106与分凝器105的连接法兰。(b) and (c) in Fig. 2 are respectively the top view of the condensate return channel and the top view of the empty tower section of the utility model. Among them, 107-1 is the equipment interface flange, 107-2 is the cooling water inlet, 107-3 is the condensed water outlet, 107-4 is the heat exchange tube bundle, 106 is the empty tower section, 106-1 is the
以下结合附图做进一步说明。Further description will be made below in conjunction with the accompanying drawings.
具体实施方式 Detailed ways
在原有的分馏塔分凝器105与分馏塔顶之间固定安装换热面积为50-70%的冷凝回流通道107,即在塔径为500mm上安装管板塔盘,将145根25的管子作为换热管束107-4固定在管板上,管束107-4在管板上的排列方式为等边三角形。同时管子的长度与塔径的比为1∶1.2。管束107-4与塔内气体流向均为沿塔的纵向垂直,管束的布管面积为塔盘面积的35%。管板与壳体焊接在一起。Between the original
冷凝回流通道107到分凝器105联通装置是一个两端用和原塔相同的法兰盘焊接高度不低于塔径50%一个保温良好的空塔节106,其作用是将上升气体进行重新平衡分布,均匀地输送到装置中换能。如果没有这一装置,容易造成原塔体通道堵塞。The connecting device between the
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CN101307058B (en) * | 2008-05-21 | 2010-07-07 | 云南绿宝香精香料股份有限公司 | Device for separating gamma-terpinene and p-cymene eucalyptus oil film-lifting fractionator |
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CN101307058B (en) * | 2008-05-21 | 2010-07-07 | 云南绿宝香精香料股份有限公司 | Device for separating gamma-terpinene and p-cymene eucalyptus oil film-lifting fractionator |
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