WO2012048550A1 - 一种防热敏精馏塔和天然物质防热敏精馏分离工艺 - Google Patents

一种防热敏精馏塔和天然物质防热敏精馏分离工艺 Download PDF

Info

Publication number
WO2012048550A1
WO2012048550A1 PCT/CN2011/071750 CN2011071750W WO2012048550A1 WO 2012048550 A1 WO2012048550 A1 WO 2012048550A1 CN 2011071750 W CN2011071750 W CN 2011071750W WO 2012048550 A1 WO2012048550 A1 WO 2012048550A1
Authority
WO
WIPO (PCT)
Prior art keywords
tower
fine
liquid
sump
column
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/CN2011/071750
Other languages
English (en)
French (fr)
Inventor
张志炳
周政
杨高东
孙徳芳
张岭
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nanjing University
Nanjing Tech University
Original Assignee
Nanjing University
Nanjing Tech University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nanjing University, Nanjing Tech University filed Critical Nanjing University
Priority to CN201180013778.0A priority Critical patent/CN102933271B/zh
Priority to US13/701,840 priority patent/US10039998B2/en
Publication of WO2012048550A1 publication Critical patent/WO2012048550A1/zh
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
    • B01D3/322—Reboiler specifications
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30

Definitions

  • the invention relates to a natural substance anti-thermal precision separation process and equipment.
  • Natural flavors include animal flavors and vegetable flavors. Among them, animal flavors are more commonly known as musk, ambergris, etc.; there are many types of plant flavors, such as essential oils, scented resins, oleoresins, and the like. Artificial flavors include some alcohols and esters. In chemical, petrochemical, book
  • the batch separation process consists mainly of batch-type fine columns, heating units, and condensing reflux units.
  • the basic process is as follows: The material to be steamed is added to the tower kettle 29 for heating and evaporation at a time, and the generated gas passes through the fine tower 25 to enter the condenser 26 to be condensed into a liquid, and a part of the condensate is refluxed to the fine tower, and returned to the tower. The kettle is further heated to evaporate, and the other portion is taken out.
  • the continuous separation device has more feed device 40 and reboiler 35 than the intermittent separation device.
  • the basic process of continuous separation is as follows: When driving, the raw materials to be steamed are added to the condensate tower to reach a certain liquid level, heating starts, the condensate obtained at the top of the tower is completely refluxed, and no feeding is required in the whole reflux stage; After the end of the stage, a part of the condensate flowing out of the condenser 34 is returned to the rest for production, and the liquid entering the tower is also partially recovered, and the remaining part enters the reboiler 35 to continue heating and evaporation, and the generated gas enters the fine stream.
  • the column 33 flows from bottom to top, and at this time, it is continuously fed to ensure a constant liquid level of the material in the column.
  • the object of the present invention is to solve the defect that the above-mentioned fine separation device is easy to cause heat sensitivity for the heat sensitive natural substance, and propose a new natural substance anti-thermal precision separation process and equipment.
  • the technology is particularly suitable for separating a substance system which is prone to heat-sensitive reaction upon heating, and can prevent degradation of the product due to the heat-sensitive reaction, thereby ensuring Maintain the excellent quality inherent in the target product.
  • An anti-heat precision fine tower as shown in Fig. 1, which is composed of a fine tower 2, a T-type condenser 4, a baffle 12, a tower kettle 3, a falling film reboiler 5, and a T-type condenser 4 It is placed directly on the top of the fine tower 2, without pipe connection in the middle, the distance is almost zero.
  • the T-type condenser 4 is provided with a circular baffle 12, and the liquid condensed in the T-type condenser 4 cannot directly enter the fine tower.
  • the fine tower 2 is a plate tower or a packed tower, preferably a packed tower; the tower tank 3 and the falling film reboiler 5 are connected by a centrifugal pump 7 into a high-speed circulation system, and the tower tank 3 is elongated and tubular.
  • the falling film type reboiler 5 is a chunky tube type.
  • the above-mentioned anti-heating precision crucible tower, the T-type condenser 4, and the fine crucible tower 2 are connected by a flange, and the refrigerant of the T-type condenser 4 enters through the duct 18 and then flows out from the duct 19.
  • the liquid collection tank 20 is disposed at the top outlet of the fine crucible tower 2, and the edge of the liquid collection tank 20 is higher than the connection port of the fine crucible tower 2 and the T-type condenser 4. There is a gap between the baffle 12 and the baffle 12, and the liquid condensed in the T-type condenser 4 can flow into the sump 4.
  • the baffle 12 is welded above the interface of the fine crucible tower 2 and the T-type condensation tower 4, and has a gap with the top of the fine crucible tower 2, so that the upward steam can pass, and at the same time
  • the diameter of the baffle 12 is larger than the inner edge of the sump 20, so that the condensed liquid in the T-type condenser 4 flows into the sump 20 without directly entering the concentrating tower 2.
  • the tower tank 3 is an elongated tubular shape, and the volume is 1/10 1/50 of the conventional tower kettle, so that the residence time of the material is correspondingly greatly shortened, and the long time is not long.
  • the ground stays in a high temperature environment.
  • the above-mentioned anti-heating precision crucible tower, the falling film type tube re-boiler 5, has a short body (high aspect ratio less than 1) cylinder, and the fluid is in the column under the action of the liquid circulation pump at the bottom of the tower
  • the average dwell time from top to bottom in each tube is very short, usually around 0.1-3 seconds. Therefore, although the temperature is the highest in the whole process, the contact time between the material and the heating wall is extremely short, so that the heat-sensitive reaction can be effectively avoided.
  • the conventional reboiler reboiler is the opposite. When the material is cooked at a high temperature for a long time, the heat-sensitive reaction is generally difficult to avoid.
  • the above-mentioned anti-heating precision crucible tower is composed of a pipe 23, a liquid collection tank 6, a pipe 16, a centrifugal pump 8, and a pipe 15, and the liquid collection tank 6 is for collecting the liquid flowing out of the liquid collection tank 20.
  • the liquid in the liquid collection tank 6 is returned to the fine tower 2 by the centrifugal pump 8 to be refluxed, and a part is taken out as a product.
  • a natural substance anti-heating fine separation process as shown in Figure 1, the whole process is continuous, it adopts the above The anti-thermal precision tower, the specific steps are as follows:
  • Step 1 Reduce the pressure in the entire fine column to the required operating pressure by the vacuum system 22 (usually control the operating pressure below the temperature sensitive point of the fine material).
  • the vacuum system 22 usually control the operating pressure below the temperature sensitive point of the fine material.
  • Step 2 The gas enters the T-type condenser 4 and condenses into a liquid. Due to the baffle 12, the liquid can only flow from the peripheral side of the baffle into the sump 20, and then enters the sump 6 through the pipe 23, and then passes through the pipe.
  • the T-type condenser 4 is placed directly above the condensing tower 2, and the gas enters from the middle of the tank of the condenser 4, Since the distance between the top of the fine column 2 and the condenser 4 is almost zero, the gas in the fine column 2 can be rapidly condensed into a liquid and cooled below the temperature sensitive temperature, due to the presence of the baffle 12, The condensed liquid can only flow from the circumferential side of the baffle 12 into the sump 20;
  • Step 3 When the whole reflux is established for a period of time, the whole tower is balanced, the part is finally taken out, the valves 9 and 10 are opened, the light component of the tower top is taken out through the valve 10, and the high-boiling heavy component in the tower tank 3 passes through the valve. 9 is produced, and at the same time, the feed is started through the pipe 1, so that the liquid level in the tower 3 is maintained at a normal level, thereby entering the continuous fine operation stage.
  • the anti-heat precision tower uses a T-type condenser, which greatly shortens the distance between the fine tower and the condenser. , thereby minimizing the residence time of the vapor phase between the top of the fine crucible and the condenser, so that the vapor rising from the fine tower to the top of the tower can be quickly condensed into a liquid and cooled below the temperature sensitive temperature. , can effectively prevent the occurrence of thermal reaction between the top of the tower and the condenser.
  • Anti-thermal precision tower shown in Figure 1
  • a circular baffle and an annular sump are designed between the T-condenser and the fine turret, so that the condensed liquid from the T-type condenser is only It can flow into the sump, thus preventing the condensate from directly entering the condensing tower, which facilitates precise control of the recirculation.
  • the anti-heat precision tower uses a slender tubular tower, which is greatly reduced in size, only the traditional tower 1/50 1/10, and due to the action of the bottom circulation pump, the average residence time of the materials in the tower is only 1/50 1/10 of the traditional tower.
  • the tower material is prevented from being cooked for a long time in the high temperature region of the tower, thereby greatly suppressing the occurrence of the heat-sensitive reaction in the tower.
  • Anti-thermal precision tower (shown in Figure 1) A falling film tube reboiler with a short and thick structure, with traditional fine design Compared with the conventional tube-type reboiler 35 in the preparation, the liquid from the top of the falling film tube reboiler will continuously update the vaporized surface, so that the surface heat transfer effect is good, the vaporization speed is fast, and the liquid and high temperature columns are simultaneously The contact time of the inner surface of the tube is extremely short, which can effectively prevent the liquid material from being heated by overheating and high temperature for a long time, thereby effectively avoiding the occurrence of heat-sensitive reaction in the heat exchanger. BRIEF DESCRIPTION OF THE DRAWINGS FIG.
  • 1 is a heat-sensitive fine separation process and equipment of the present invention, wherein 1 is a feed port, 2 is a fine sputum tower, 3 is a tower kettle, 4 is a T-type condenser, and 5 is a falling film type.
  • Boiling device 6 is a liquid collection tank, 7 and 8 are centrifugal pumps, 9, 10, 21, 24 are valves, 11, 13, 14 are tower material conveying pipes, 12 are baffles, 15, 16, 23 are towers
  • the top condensate conveying pipe, 17 is the top condensate recovery port, 18, 19 is the condensing medium conveying pipe, 20 is the sump, and 22 is the vacuum system.
  • 2 is a conventional batch fine boring equipment, wherein 25 is a fine boring tower, 26 is a condenser, 27 is a vacuum system, 28, 30, 31 are valves, and 29 is a tower kettle.
  • Figure 3 is a conventional continuous fine boring equipment, wherein 32 is a tower kettle, 33 is a fine turret, 34 is a condenser, 35 is a reboiler, 36 is a vacuum system, 37, 38, 39 are valves, 40 is a feed port .
  • Figure 4 shows the process and equipment for the separation of the two towers of the anti-thermal (the equipment diagram of the embodiments 2 and 3), 2 is the fine tower A, and T2 is the fine tower 8. detailed description
  • the mixed solution of the crude oil of eucalyptus leaves and ethanol is passed from the pipeline 1 through the condensing tower 2 into the tower kettle 3, the diameter of the sorghum tower 2 is 0.15 m, the number of theoretical trays is 40, and the total volume of the tower kettle 3 is 50 liters.
  • the aspect ratio is 3:1.
  • the vacuum system 22 is turned on, the pressure of the entire fine boring system is lowered to 400 mmHg, and the falling film reboiler 5 starts heating.
  • the volume of the falling film reboiler 5 is 500 L, and the heating of the falling film reboiler 5 is started.
  • the medium temperature was 140 °C.
  • the pump 7 is turned on to circulate the liquid material in the tower tank 3.
  • the circulation flow rate of the centrifugal pump is 40 m 3 /h, and the vapor phase generated in the falling film type reboiler 5 enters the fine tower together with the unvaporized liquid. At the bottom of the bottom, the vapor phase is separated by the fine column 2, and the vapor phase reaching the top is rapidly condensed in the T-type condenser 4 into a liquid flowing into the liquid collecting tank 20, and then enters the liquid collecting tank 6 through the line.
  • the centrifugal pump 8 is used to directly drive the condensate in the liquid collection tank into the fine column 2 for full reflux operation. When full reflux is carried out for a period of time After the balance is established, the part is finally taken out, and the valves 9 and 10 are opened, and the reflux ratio is 2/5.
  • the mixed solution of the crude oil and the ethanol of the eucalyptus leaves is started through the pipe 1, and the liquid level in the tower 3 is kept constant, and the To the continuous precision stage.
  • the purity of 1,8-cineole in the collected liquid of the tower was 99.7%, and the amount of production was 300kg/h.
  • the residence time of the material in the tower was greatly shortened, which was only conventional continuous.
  • the 1/40 1/30 of the steamed steam is 1/200 1/100 of the conventional intermittent steaming, and the heat-sensitive reaction can be almost completely avoided. Because of this, the recovery rate of 1,8-cineole qualified products can be as high as 98.5% or more, which is more than 3% higher than conventional continuous steaming, and the product smells pure, clear and transparent.
  • the two-column process was used to separate the masson pine turpentine.
  • the specific device structure and operation method are similar to those of Embodiment 1 (as shown in FIG. 4).
  • the precision tower A2 has a diameter of 0.15 m, the theoretical number of plates is 40, the total volume of the tower kettle 3 is 50 L, and the height to diameter ratio of the tower kettle is 3:1.
  • the pressure control of the fine column A2 is 40 mmHg, and the heating temperature of the falling film reboiler 5 is 140 °C.
  • the circulating flow rate of the centrifugal pump is 30 m 3 /h.
  • the top temperature of the fine tower A1 is controlled at about 90 °C, and ⁇ -pinene is produced at the top.
  • the recovery amount is 180 kg/h, and its purity can reach 98% or more.
  • the yield of terpenes can reach over 99.5%, which is more than 8 percentage points higher than conventional continuous steaming.
  • the material at the bottom of the crucible 2 crucible is separated into the fine crucible 2 by the bottom pump 7.
  • the pressure of the fine crucible 2 is controlled to 40 mmHg, and the temperature of the falling film reboiler is 150 °C.
  • the circulating flow rate of the centrifugal pump is 30 m 3 /h.
  • the top part is produced with ⁇ -pinene, the amount of production is 80kg/h, and the heavy component of turpentine is produced at the bottom, commonly known as heavy oil.
  • the purity of ⁇ -pinene can reach above 98.5, and the yield can reach over 99.0%, which is more than 7 percentage points higher than conventional continuous steaming.
  • the residence time of the materials in the two towers is greatly shortened, which is only 1/60 1/50 of the continuous steaming of the conventional two towers, which is 1/500 1/400 of the conventional intermittent steaming. , The heat-sensitive reaction of the turpentine component can be almost completely avoided.
  • Example 2 Similar to the operation of Example 2, a mixed solution of dihydromyrcenol, dihydromyrcene, and isopropyl alcohol was added to the fine boring system, and the operating pressure of the fine enthalpy 2 was controlled by a vacuum system of 20 mmHg.
  • the diameter of the diaphragm is 0.15m, the number of theoretical plates is 40), the heating temperature of the falling film reboiler 5 is 140 °C, the circulating flow rate of the centrifugal pump 7 is 40m 3 /h, and the total reflux temperature is maintained for a period of time after the temperature of the whole tower is stabilized.
  • Dihydromyrcenol was produced at the bottom of the fine tower A2 (recovery amount 300 kg/h, reflux ratio 2/5), and its purity was 95.6%. Then, it is sent to the fine turret BT2 for fine boring, and more than 99.5% of the dihydromyrcenol product can be obtained from the top of the condensing tower BT2.
  • the average residence time of the materials in the two towers is only about 1/50 of the continuous distillation of the conventional two towers, which is a routine interval. About 1/400 of steamed rice.
  • the yield of dihydromyrcenol can be as high as 92% or more, which is about 14% higher than that of conventional continuous steaming, and more than 20% higher than conventional intermittent steaming.
  • the resulting product has a pure odor and does not have any scorching odor.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Description

一种防热敏精馏塔和天然物质防热敏精馏分离工艺 发明领域
本发明涉及一种天然物质防热敏精熘分离工艺与设备。
背景技术
说
天然物质的香料等， 在化工、 食品、 医药等行业中占重要地位。 天然香料包括动物 性香料和植物性香料， 其中动物性香料较为常见的有麝香、 龙涎香等； 植物性香料种类 比较多， 如精油、 香树脂、 油树脂等。 人工香料包括一些醇类和酯类。 在化工， 石化， 书
制药， 食品等工业中， 分离装置是必不可少的。 传统的精熘分离包括间歇分离 （流程如 图 2所示） 和连续分离 （流程如图 3所示）， 间歇分离流程中主要包括间歇式精熘塔、 加 热装置、 冷凝回流装置。 其基本流程为： 一次性将要蒸熘的物料加入塔釜 29中进行加热 蒸发， 产生的气体经过精熘塔 25进入到冷凝器 26中冷凝成液体， 冷凝液一部分回流精熘 塔， 回到塔釜继续加热蒸熘， 另一部分则采出， 加热到一定时间待塔釜物料中的轻组分 完全蒸出后， 一次性将塔釜的物料放出， 期间不再补充物料。 连续分离装置比间歇分离 装置多了进料装置 40和再沸器 35。 连续分离的基本流程为： 开车时， 将待蒸熘的原料加 入精熘塔塔釜达到一定的液位， 开始加热， 塔顶所得的冷凝液全部回流， 全回流阶段不 需要补料； 全回流阶段结束后从冷凝器 34中流出的冷凝液一部分回流其余部分采出， 而 进入塔釜的液体也要部分采出， 剩余部分则进入再沸器 35中继续加热蒸发， 产生的气体 进入精熘塔 33中自下而上流动， 此时要不断进料以保证塔釜中物料的液位恒定。 目前大 多数精熘分离的流程都属于以上这两种情况。这样的流程需要对物料进行长时间的高温 加热， 对于上述这些天然物质， 大部分对热敏感， 往往会在蒸熘分离过程中由于温度过 高、 受热时间过长而发生热敏反应， 如聚合、 脱水、 氧化、 分解等， 导致结焦、 积炭、 变色、 香气受损等后果， 使产物的品质降低， 同时也造成资源的浪费。
发明内容
本发明的目的是针对热敏性的天然物质，解决上述精熘分离装置的易导致热敏这一 缺陷， 提出一种新的天然物质防热敏精熘分离工艺与设备。 该技术特别适用于分离在加 热时易发生热敏性反应的物质体系， 可以防止其由于热敏反应造成的产品降质， 从而保 持目标产品固有的优良品质。
本发明的目的可通过以下技术方案来实现：
一种防热敏精熘塔， 如图 1所示， 它由精熘塔 2、 T型冷凝器 4、 挡板 12、 塔釜 3、 降膜式再沸器 5组成， T型冷凝器 4直接置于精熘塔 2顶部， 中间不用管道连接， 距离 几乎为零， T型冷凝器 4内设有一块圆形挡板 12， T型冷凝器 4中冷凝的液体不能直 接进入到精熘塔 2， 以避免难控制的内回流， 精熘塔 2与 T型冷凝器 4之间有一环形集 液槽 20， 用来收集 T型冷凝器 4中冷凝的液体， 并引入塔外的集液罐 6中， 精熘塔 2 为板式塔或填料塔， 优选的为填料塔； 塔釜 3与降膜式再沸器 5之间通过离心泵 7连成 高速循环系统， 塔釜 3为细长管状； 降膜式再沸器 5为矮胖型列管式。
上述的防热敏精熘塔， 所述的 T型冷凝器 4， 与精熘塔 2之间通过法兰连接， T型 冷凝器 4的冷媒由管道 18进入， 再从管道 19流出。
上述的防热敏精熘塔， 所述的集液槽 20， 设置在精熘塔 2顶部出口的位置， 集液槽 20的边口高于精熘塔 2与 T型冷凝器 4的连接口，且与挡板 12之间有空隙， T型冷凝 器 4中被冷凝成的液体只能流入集液槽 4中。
上述的防热敏精熘塔， 所述的挡板 12， 焊接在精熘塔 2与 T型冷凝塔 4接口处的 上方， 与精熘塔 2顶部有一段空隙， 可让上行蒸汽通过， 同时挡板 12的直径要大于集 液槽 20的内边缘， 这样 T型冷凝器 4中冷凝的液体就会流到集液槽 20中， 而不会直接 进入精熘塔 2中。
上述的防热敏精熘塔， 所述的塔釜 3为细长的管状， 体积为传统塔釜的 1/10 1/50， 因此其中物料的停留时间也相应大幅度缩短， 不会长时间地滞留在高温环境中。
上述的防热敏精熘塔， 所述的降膜式列管再沸器 5， 外观为矮胖的 （高径比小于 1 ) 圆柱体，在塔底液体循环泵的作用下，流体在列管中每次自上而下的平均停留时间很短， 通常为 0.1-3秒左右。 因此， 虽然此处是全流程中温度最高的地方， 但由于物料与加热 壁之间的接触时间极短， 因此将有效避免热敏反应的发生。 而传统的精熘塔的再沸器则 相反， 物料在其中被长时间高温蒸煮， 则发生热敏反应是一般难以避免的。
上述的防热敏精熘塔， 所述的回流系统由管道 23、 集液罐 6、 管道 16、 离心泵 8和 管道 15组成， 集液罐 6用来收集从集液槽 20中流出的液体， 集液罐 6中的液体， 用离 心泵 8将一部分送回精熘塔 2中进行回流， 一部分则作为产品被采出。 一种天然物质防热敏精熘分离工艺， 如图 1所示， 整个工艺为连续的， 它采用上述 的防热敏精熘塔， 具体步骤如下：
步骤 1. 通过真空系统 22将整个精熘塔内压力降低至所需操作压力（通常将操作压 力控制在被精熘物的热敏温度点以下）， 开车时， 将混合物料从管道 1通过精熘塔 2进 入到塔釜 3中， 当达到一定液位时， 开启泵 7， 将塔釜 3中物料通过管道 13和 14打入 降膜式再沸器 5中进行加热， 产生的气液混合物在压差的作用下通过管道 11进入到精 熘塔 2中， 进行精熘；
步骤 2. 气体进入到 T型冷凝器 4中冷凝成液体， 由于挡板 12， 液体只能从挡板周 侧流入集液槽 20，再经过管道 23进入到集液罐 6内，然后经过管道 16和离心泵 8将集 液罐 6中的液体打进精熘塔 2中， 进行全回流， T型冷凝器 4放置在精熘塔 2正上方， 气体从冷凝器 4的罐体中间进入， 由于精熘塔 2顶部与冷凝器 4之间的距离几乎为零， 所以精熘塔 2中的气体能被迅速冷凝成液体， 并且被冷却至热敏温度以下， 由于挡板 12 的存在， 被冷凝的液体只能从挡板 12的周侧流入到集液槽 20中；
步骤 3. 当全回流进行一段时间全塔建立平衡后， 开始部分采出，打开阀门 9和 10， 塔顶轻组分熘出物通过阀门 10采出， 塔釜 3内高沸点重组分通过阀门 9采出， 同时通 过管道 1开始进料， 使塔釜 3中的液体液面保持在正常水平， 由此进入到连续精熘操作 阶段。
本发明的优点：
1.与传统精熘设备 （图 2， 图 3所示） 相比， 防热敏精熘塔 （图 1所示） 采用 T型 冷凝器， 大大缩短了精熘塔与冷凝器之间的距离， 从而最大限度地缩短了汽相在精熘塔 顶与冷凝器之间的停留时间， 这样从精熘塔中上升到塔顶的蒸汽能被迅速冷凝成液体， 并被冷却至热敏温度以下， 可有效防止塔顶和冷凝器之间热敏反应的发生。
2.防热敏精熘塔 （图 1所示） 中 T型冷凝管与精熘塔之间设计了一块圆形挡板和环 形集液槽， 这样从 T型冷凝器中冷凝回流的液体只能流入集液槽中， 从而防止了冷凝液 直接进入精熘塔中， 便于对回流进行精确控制。
3.与传统精熘设备 （图 2， 图 3所示） 相比， 防热敏精熘塔 （图 1所示） 采用了细 长管状塔釜， 其体积大大减小， 仅为传统塔釜的 1/50 1/10， 又由于塔底循环泵的作用， 使得塔釜中物料的平均停留时间也仅为传统塔釜的 1/50 1/10。 这样， 就避免了塔釜物 料在塔釜高温区域被长时间蒸煮， 从而大大抑制了塔釜内热敏反应的发生。
4.防热敏精熘塔 （图 1所示） 采用了短粗结构的降膜式列管再沸器， 与传统精熘设 备中的普通列管式再沸器 35相比， 降膜式列管再沸器自上而下的液体会不断更新汽化 表面， 使得表面传热效果良好， 汽化速度快， 同时液体与高温列管内表面的接触时间极 短， 可有效避免液相物料被过热和长时间高温加热， 也就有效避免了换热器内热敏反应 的发生。 附图说明 图 1为本发明的防热敏精熘分离工艺与设备， 其中 1为进料口， 2为精熘塔， 3为塔釜， 4为 T型冷凝器， 5为降膜式再沸器， 6为集液罐， 7、 8为离心泵， 9、 10、 21、 24为 阀门， 11、 13、 14为塔釜物料输送管道， 12为挡板， 15、 16、 23为塔顶冷凝液输送管 道， 17为塔顶冷凝液采出口， 18、 19为冷凝介质输送管道， 20为集液槽， 22为真空系 统。 图 2为传统间歇精熘设备， 其中 25为精熘塔， 26为冷凝器， 27为真空系统， 28、 30、 31为阀门， 29为塔釜。 图 3为传统连续精熘设备， 其中 32为塔釜， 33为精熘塔， 34为冷凝器， 35为再沸器， 36为真空系统， 37、 38、 39为阀门， 40为进料口。 图 4为防热敏两塔精熘分离工艺与设备 （实施例 2和 3的设备图）， 2为精熘塔 A， T2 为精熘塔8。 具体实施方式
实施例 1
将桉叶粗油与乙醇的混合溶液由管道 1经过精熘塔 2进入塔釜 3， 精熘塔 2直径为 0.15m, 理论塔板数为 40， 塔釜 3的总容积为 50L， 塔釜的高径比为 3 : 1。 开启真空系统 22, 将整个精熘系统的压力降到 400毫米汞柱， 降膜式再沸器 5开始加热， 降膜式再沸 器 5的容积为 500L, 降膜式再沸器 5的加热介质温度为 140°C。 同时开启泵 7， 使塔釜 3中的液料循环， 离心泵的循环流量为 40m3/h， 降膜式再沸器 5中产生的汽相与未被汽 化的料液一道进入精熘塔 2底部， 汽相经过精熘塔 2分离， 到达顶部的汽相在 T型冷凝 器 4中被迅速冷凝成液体流入集液槽 20后， 再通过管线进入集液罐 6。 采用离心泵 8 将集液罐中冷凝液直接打入精熘塔 2内进行全回流操作。当全回流进行一段时间全塔建 立平衡后， 开始部分采出， 打开阀门 9和 10， 回流比为 2/5， 同时通过管道 1开始进桉 叶粗油与乙醇的混合溶液， 保证塔釜 3中液体液面保持恒定， 进入到连续精熘阶段。 采 集出的塔釜液料中 1,8-桉树脑纯度为 99.7%， 采出量为 300kg/h， 与常规连续蒸熘相比， 物料在塔釜内的停留时间大幅缩短， 仅为常规连续蒸熘的 1/40 1/30， 为常规间歇蒸熘 的 1/200 1/100， 几乎完全可避免热敏反应的发生。 由于此， 1,8-桉树脑合格品的回收率 可高达 98.5%以上， 比常规连续蒸熘提高 3%以上， 而且产品气味纯正， 清澈透明。
实施例 2
采用两塔流程分离马尾松松节油。 具体设备结构和操作方法与实施例 1的类似（如 图 4所示）。 将马尾松松节油加入精熘系统精熘塔 A2。 精熘塔 A2直径为 0.15m， 理论 塔板数为 40， 塔釜 3的总容积为 50L， 塔釜的高径比为 3 : 1。 精熘塔 A2的压力控制为 40mmHg操作， 降膜式再沸器 5的加热温度为 140°C。 离心泵的循环流量为 30m3/h。 全 回流一段时间待全塔温度稳定后， 精熘塔 A1顶温控制在 90°C左右， 在顶部采出 α -蒎 烯， 采出量为 180kg/h，其纯度可达 98 %以上， α -蒎烯的收率可达 99.5%以上， 比常规 连续蒸熘提高 8个百分点以上。 精熘塔 Α2釜底部的物料通过塔底泵 7打入精熘塔 ΒΤ2 进行分离。精熘塔 ΒΤ2的压力控制为 40mmHg操作，降膜式再沸器的加热温度为 150°C。 离心泵的循环流量为 30m3/h。 其顶部采出 β -蒎烯， 采出量为 80kg/h， 底部采出松节油 的重组分， 俗称重油。 β -蒎烯的纯度可达 98.5以上， 收率可达 99.0%以上， 比常规连 续蒸熘提高 7个百分点以上。
与常规连续蒸熘相比， 物料在两个塔釜内的停留时间大为缩短， 仅为常规两塔连续 蒸熘的 1/60 1/50， 为常规间歇蒸熘的 1/500 1/400， 几乎可完全避免松节油组分的热敏 反应。
实施例 3
与实施例 2的操作方式类似， 将二氢月桂烯醇、 二氢月桂烯、 异丙醇混合溶液加 入精熘系统， 通过真空系统控制精熘塔 Α2操作压力 20毫米汞柱 （精熘塔 Α的直径 0.15m, 理论塔板数 40)， 降膜式再沸器 5的加热温度为 140°C， 离心泵 7的循环流量为 40m3/h， 全回流一段时间待全塔温度稳定后在精熘塔 A2底部采出二氢月桂烯醇 （采出 量 300kg/h,回流比 2/5 )，其含量其纯度可达到 95.6%。再将其送入精熘塔 BT2进行精熘， 从精熘塔 BT2顶部可得到 99.5%以上的二氢月桂烯醇产品。通过此抗热敏装置和工艺操 作，物料在两个塔釜内的平均停留时间仅为常规两塔连续蒸熘的 1/50左右，为常规间歇 蒸熘的 1/400左右。 因此二氢月桂烯醇的收率可高达 92%以上， 比常规连续蒸熘提高 14 个百分点左右， 而比常规间歇蒸熘提高 20%以上。 所得产品气味纯正， 没有任何焦糊异 味。

Claims

权 利 要 求 书
1. 一种防热敏精熘塔， 其特征是： 它由精熘塔（2)、 T型冷凝器（4)、 挡板（12)、 塔釜 （3 )、 降膜式再沸器 （5) 和回流系统组成， T型冷凝器 （4) 直接置于精熘塔 （2) 顶部， 中间不用管道连接， 距离几乎为零， T型冷凝器（4) 内设有一块圆形挡板（12)， T型冷凝器 （4) 中冷凝的液体不能直接进入到精熘塔 （2)， 精熘塔 （2) 与 T型冷凝器
(4) 之间有一环形集液槽 （20)， 用来收集 T型冷凝器 （4) 中冷凝的液体， 并引入塔 外的集液罐 （6) 中， 塔釜 （3 ) 与降膜式再沸器 （5 ) 之间通过离心泵 （7) 连成高速循 环系统， 塔釜 （3 ) 为细长管状； 降膜式再沸器 （5 ) 为矮胖型列管式。
2. 根据权利要求 1所述的防热敏精熘塔， 其特征是： 所述的精熘塔（2) 为板式塔 或填料塔。
3. 根据权利要求 2所述的防热敏精熘塔， 其特征是： 所述的精熘塔（2)为填料塔。
4. 根据权利要求 1所述的防热敏精熘塔， 其特征是： 所述的 T型冷凝器 （4) 与精 熘塔（2)之间通过法兰连接， T型冷凝器（4)的冷媒由管道（18)进入， 再从管道（19) 流出。
5. 根据权利要求 1所述的防热敏精熘塔， 其特征是： 所述的集液槽 （20)， 设置在 精熘塔 （2)顶部出口的位置， 集液槽 （20) 的边口高于精熘塔 （2) 与 T型冷凝器 （4) 的连接口， 且与挡板 （12) 之间有空隙， T型冷凝器 （4) 中被冷凝成的液体只能流入 集液槽 （4) 中。
6. 根据权利要求 1所述的防热敏精熘塔， 其特征是： 所述的挡板 （12)， 焊接在精 熘塔 （2) 与 T型冷凝塔 （4) 接口处的上方， 与精熘塔 （2) 顶部有一段空隙， 可让上 行蒸汽通过， 同时挡板 （12) 的直径要大于集液槽 （20) 的内边缘， T型冷凝器 （4) 中冷凝的液体只能流到集液槽 （20) 中， 而不会直接进入精熘塔 （2) 中。
7. 根据权利要求 1所述的防热敏精熘塔， 其特征是： 所述的塔釜 （3 ) 为细长的管 状， 体积为传统塔釜的 1/10 1/50。
8. 根据权利要求 1所述的防热敏精熘塔， 其特征是： 所述的降膜式列管再沸器（5 ) 外观为矮胖的圆柱体， 在塔底液体循环泵的作用下， 流体在列管中每次自上而下的平均 停留时间很短， 通常为 0.1-3秒左右。
9. 根据权利要求 1所述的防热敏精熘塔， 其特征是： 所述的回流系统由管道（23 )、
1 集液罐 （6)、 管道 （16)、 离心泵 （8) 和管道 （15 ) 组成， 集液罐 （6) 用来收集从集 液槽 （20) 中流出的液体， 集液罐 （6) 中的液体， 用离心泵 （8) 将一部分送回精熘塔 (2) 中进行回流， 一部分则作为产品被采出。
10. 一种采用权利要求 1所述的防热敏精熘塔的天然物质防热敏精熘分离工艺， 整 个工艺为连续的， 它采用权利要求 1所述的防热敏精熘塔， 其特征是具体步骤如下： 步骤 1. 通过真空系统 22将整个精熘塔内压力降低至所需操作压力， 开车时， 将混 合物料从管道 （1 ) 通过精熘塔 （2) 进入到塔釜 （3 ) 中， 当达到一定液位时， 开启泵
(7)， 将塔釜 （3 ) 中物料通过管道 （13和 14) 打入降膜式再沸器 （5 ) 中进行加热， 产生的气液混合物在压差的作用下通过管道 （11 ) 进入到精熘塔 （2) 中， 进行精熘； 步骤 2. 气体进入到 T型冷凝器 （4) 中冷凝成液体， 由于挡板 （12)， 液体只能从 挡板 （12) 周侧流入集液槽 （20)， 再经过管道 （23 ) 进入到集液罐 （6) 内， 然后经过 管道 （16)和离心泵 （8 )将集液罐 （6) 中的液体打进精熘塔 （2) 中， 进行全回流， T 型冷凝器 （4) 放置在精熘塔 （2) 正上方， 气体从冷凝器 （4) 的罐体中间进入， 由于 精熘塔 （2) 顶部与冷凝器 （4) 之间的距离几乎为零， 所以精熘塔 （2) 中的气体能被 迅速冷凝成液体， 并且被冷却至热敏温度以下， 由于挡板 （12) 的存在， 被冷凝的液体 只能从挡板 （12) 的周侧流入到集液槽 （20) 中；
步骤 3. 当全回流进行一段时间全塔建立平衡后， 开始部分采出， 打开阀门 （9)和 阀门 （10)， 塔顶轻组分熘出物通过阀门 （10)采出， 塔釜 （3 ) 内高沸点重组分通过阀 门 （9) 采出， 同时通过管道 （1 ) 开始进料， 使塔釜 （3 ) 中的液体液面保持在正常水 平， 由此进入到连续精熘操作阶段。
2
PCT/CN2011/071750 2010-10-14 2011-03-14 一种防热敏精馏塔和天然物质防热敏精馏分离工艺 Ceased WO2012048550A1 (zh)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201180013778.0A CN102933271B (zh) 2011-03-14 2011-03-14 一种防热敏精馏塔和天然物质防热敏精馏分离工艺
US13/701,840 US10039998B2 (en) 2010-10-14 2011-03-14 Anti-thermosensitization rectification tower and the rectification process thereof for separating thermosensitive natural substances

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201010506824.8 2010-10-14
CN201010506824 2010-10-14

Publications (1)

Publication Number Publication Date
WO2012048550A1 true WO2012048550A1 (zh) 2012-04-19

Family

ID=45937854

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2011/071750 Ceased WO2012048550A1 (zh) 2010-10-14 2011-03-14 一种防热敏精馏塔和天然物质防热敏精馏分离工艺

Country Status (1)

Country Link
WO (1) WO2012048550A1 (zh)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1555902A (zh) * 2003-12-31 2004-12-22 天津大学 带侧线出料和塔釜冷存料的热敏物料间歇精馏过程
CN101391152A (zh) * 2008-10-22 2009-03-25 天津大学 吸收式热泵用于双再沸器间歇萃取精馏的装置和方法
CN201280531Y (zh) * 2008-04-02 2009-07-29 山东华鲁恒升化工股份有限公司 一种制备三甲胺的生产装置

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1555902A (zh) * 2003-12-31 2004-12-22 天津大学 带侧线出料和塔釜冷存料的热敏物料间歇精馏过程
CN201280531Y (zh) * 2008-04-02 2009-07-29 山东华鲁恒升化工股份有限公司 一种制备三甲胺的生产装置
CN101391152A (zh) * 2008-10-22 2009-03-25 天津大学 吸收式热泵用于双再沸器间歇萃取精馏的装置和方法

Similar Documents

Publication Publication Date Title
US10039998B2 (en) Anti-thermosensitization rectification tower and the rectification process thereof for separating thermosensitive natural substances
CN100586523C (zh) 有机溶剂回收用的多效逆流降膜蒸发系统
CN100537507C (zh) 维生素a中间体十四醛的提纯方法及其装置
CN102125770B (zh) 刮膜式薄膜蒸发器用于处理热敏性物料的连续精馏装置和方法
CN205730426U (zh) 一种精馏塔
CN104059780B (zh) 一种用于热敏性芳香油分馏的设备
CN207197285U (zh) 一种不凝气体去除装置
CN102933271B (zh) 一种防热敏精馏塔和天然物质防热敏精馏分离工艺
CN202185162U (zh) 短程蒸馏装置
CN107754365A (zh) 一种甲醇双效精馏精制装置及工艺方法
CN202155061U (zh) 高真空蒸馏提纯装置
CN102266677B (zh) 高真空蒸馏提纯装置
CN208356129U (zh) 一种微膜蒸发器及包含微膜蒸发器的精馏系统
WO2012048550A1 (zh) 一种防热敏精馏塔和天然物质防热敏精馏分离工艺
CN108465261B (zh) 一种蒸馏塔设备
CN217459286U (zh) 一种秸秆生产木醋液的后处理装置
CN208250270U (zh) 一种用于杨梅酒加工提纯使用酒蒸馏设备
US10058796B2 (en) Evaporator and process for use thereof
CN212594079U (zh) 一种四氯化钛中低沸点杂质的气相分离装置
CN2748444Y (zh) 注射用水蒸馏塔
CN218306238U (zh) 一种粗甲酯蒸馏设备
CN202284190U (zh) 聚对苯二甲酸1,3-丙二醇酯连续生产工艺中的循环1,3-丙二醇精制塔
RU2398879C1 (ru) Способ получения ректификованного спирта
CN223468212U (zh) 一种常压型单效蒸馏水机
CN206214817U (zh) 一种分离热敏物料的精馏装置

Legal Events

Date Code Title Description
WWE Wipo information: entry into national phase

Ref document number: 201180013778.0

Country of ref document: CN

121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 11831947

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

WWE Wipo information: entry into national phase

Ref document number: 13701840

Country of ref document: US

122 Ep: pct application non-entry in european phase

Ref document number: 11831947

Country of ref document: EP

Kind code of ref document: A1