CN2561484Y - Fractionating rectifying tower for supercritical carbon dioxide fluid continuous countercurrent extraction - Google Patents

Fractionating rectifying tower for supercritical carbon dioxide fluid continuous countercurrent extraction Download PDF

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Publication number
CN2561484Y
CN2561484Y CN 02228379 CN02228379U CN2561484Y CN 2561484 Y CN2561484 Y CN 2561484Y CN 02228379 CN02228379 CN 02228379 CN 02228379 U CN02228379 U CN 02228379U CN 2561484 Y CN2561484 Y CN 2561484Y
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China
Prior art keywords
tower
joint
filler
rectifying column
height
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Expired - Fee Related
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CN 02228379
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Chinese (zh)
Inventor
王先宝
耿建国
刘长华
丁霄霖
方涛
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KAIDI FINE CHEMICAL CO Ltd WUHAN
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KAIDI FINE CHEMICAL CO Ltd WUHAN
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Abstract

The utility model is a distillation column for continuous countercurrent extraction of supercritical carbon dioxide liquid, comprising a column body, a column cover, a material entrance, steam jackets and a valve. The column body is divided into 3-8 sections, the top section is connected with the column cover, the top of the column is provided with a material outlet, the last section is provided with a dioxide liquid inlet and a material outlet, a material outlet is arranged between two sections and steam jackets and steam inlet and condensation water outlet are positioned outside each section. The column is 10-32m high with all sections of the same height 3-5m and diameter of 200-500mm. The column is preferred to be 10-15m high and divided into 3 sections with all sections of same height 3-5m and diameter of 200-500mm or preferred to be 10-20m high and divided into 3-4 sections with all sections of same height 3-5m and diameter of 200-500mm. The column is filled with filler which is round and regulated filler with the same inner diameter of the column and a plurality of round and regulated filler are piled.

Description

The rectifying column of supercritical carbon dioxide fluid continuous countercurrent extraction
Technical field
The utility model relates to a kind of rectifying column of supercritical carbon dioxide fluid continuous countercurrent extraction, belongs to field of fine chemical extracting rectifying equipment, is fit to any liquid material supercritical carbon dioxide fluid continuous countercurrent extraction technology.
Background technology
The normal plate column that adopts in the Chemical Manufacture, the filler material mostly is pottery or metallic article.This extraction tower mass-transfer efficiency is low, is not suitable for supercritical fluid extraction.Industrial production requirement all can not be satisfied with the also particle dumped packings that adopt of small-sized supercritical carbon dioxide device in the laboratory more.97231194 patents belong to the most approaching technology of the present utility model.97231194 patents are a tower two joints, and temperature control is undesirable, and its filler is a triangle, and the product yield is low, and purity does not reach requirement yet.
Technology contents
The purpose of this utility model is that a kind of abundant contact mass transfer of material energy, heat transfer filler of making of design can provide desirable gas, liquid contact-making surface, mass transfer, heat transfer coefficient height, the filler volume is big, and it is big that material is handled flow, the separative efficiency height, the temperature control ideal, flux is big and resistance is little, filler voidage height, and specific surface is big, surface wettability is good, is suitable in enormous quantities, quantity-produced rectifying column.
The technical solution of the utility model is: the rectifying column of this supercritical carbon dioxide fluid continuous countercurrent extraction comprises tower body, Ta Gai, material import and export, steam jacket and valve, tower body divides 3~8 joints, tower is gone up a joint top most has the tower lid to connect, cat head has material outlet, tower next section is established carbon dioxide inlet and material outlet, in the middle of two joint towers, establish material inlet, filler is housed, every joint tower peripheral hardware steam jacket and steam inlet, condensation-water drain in the tower body.Tower height 10~32m, every joint tower body height is basic identical, is 3~5m, tower diameter 200~500mm.
Preferred tower height 10~15m, tower body divide 3 joints, the basic identical 3~5m of every joint tower body height, tower diameter 200~500mm.
Preferred tower height 15~20m, tower body divide 4 joints, and every joint tower body height is basic identical, is 3~5m, tower internal diameter 200~500mm.
Described rectifying column is established material inlet between per two joints of its body of the tower, and import department establishes distributor.
Described rectifying column, its filler are the cylindrical structured packing identical with the tower internal diameter, and a plurality of cylindrical structured packings stack.
Described rectifying column, apart from rectifying column at the bottom of next joint tower 500~800mm place establish gripper shoe, other establish support ring at the bottom of respectively saving tower, support top filler, filler adopts regular stainless steel helices, specific area 900~3000m 2/ m 3, voidage is 0.80~0.93, and filler is filled into cat head from every joint tower bottom, and the space of one section dress material distributor is respectively stayed by the intermediate material import department of two joint towers.
The utility model provides a kind of rectifying column of novel supercritical carbon dioxide fluid continuous countercurrent extraction, is particularly suitable for liquid mixture raw materials such as industrialization continuous rectification separating natural vitamin E and fatty acid methyl ester, thick ginger oil.This rectifying column voltage withstand class height, unit number of theoretical plate pressure drop are little, the separation accuracy height, and the material disposal ability is big, and the space-time yield height can realize that the separation of multi-component masses is purified.Rectifying column adopts regular corrugated wire gauze packing, and voidage is big, and specific area is big, and is convenient to clean and change, and pressure drop is little, and resistance is little, and flux is big.The rectifying column material can be taked continuous flow upstream rectifying mode, and treating capacity is big, the space-time yield height, and the product purity height, no solvent residue, three-waste free discharge, free from environmental pollution.Rectifying column can use separately, also can two-stage or plural serial stage use, for the multicomponent of liquid mixture raw material from a best approach is provided.
Description of drawings
Fig. 1 has provided general structure schematic diagram of the present utility model.Temperature sensor 1, safety valve 2, pressure sensor 3, pressure-reducing valve 4, rectifying post jamb 5, filler 7, filler support ring 8, stock distributor assembly 9, material shower nozzle 10 and 11, carbon dioxide distributor 13, filler gripper shoe 14, material outlet valve 15, steam jacket 12, steam inlet 17, steam (vapor) outlet 18, pad 19.
The specific embodiment
Rectifying column is made up of tower top cover, body of the tower, material distributor assembly, regular stainless steel wire corrugated wire gauze packing, high pressure securing member, and material is 0Cr18Ni9.Every part characteristics division is as follows: 1, establish material outlet pipe, temperature sensor and connection Screw-thread sealing plug on the tower top cover.Material outlet Guan Shangshe safety valve and pressure sensor.The tower top cover wall thickness is consistent with the body of the tower wall, according to rectifying column diameter and design pressure and decide.2. body of the tower: can be divided into 3~8 joints, the upper and lower connection Screw-thread sealing plug of establishing of every joint according to design rectifying column height.Every in addition joint is established steam jacket, and operating pressure is 0.3MPa.The inner upper and lower end of the every joint of body of the tower is established packing press ring and is filled out the bar support ring.Body of the tower next joint inside is divided into the filler gripper shoe, and material outlet valve and blowoff valve are established in the bottom.The filler gripper shoe is welded on the body of the tower by 5~8 stainless steel strips.High 3~the 5m of the every joint of body of the tower, 50~100mm establishes at the place feed carbon dioxide mouth under the filler gripper shoe.3. filler: make identical with the tower internal diameter cylindrically, each high 50~100mm, filler are the screen waviness shape.The filler voidage is 0.80~0.93, and specific area is 900~3000m 2/ m 3But in 1/2 or all long-pending less structured packings of packing ratio table of tower bottom one joint, all the other respectively save the bigger filler of inner packing ratio surface area, every meter number of theoretical plate of filler 6~21.The filler filling mode is: filler stacks from inner-tower filling material support ring (plate), is stacked to the packing press ring place of every joint.Total height reaches designing requirement with the number of theoretical plate of whole fillers in the tower and is as the criterion.4. material distributor assembly: form by stainless steel cylinder, material feed pipe and material shower nozzle.The stainless steel cylinder wall thickness is consistent with body of the tower with internal diameter.The material feed pipe is entered in the tower by the circular hole on the stainless steel cylinder, and pipe end is established the material shower nozzle.High 80~the 100mm of stainless steel cylinder.Material distributor assembly is installed in respectively and saves between the body of the tower.5. all seal between tower lid and body of the tower, body of the tower and the material distributor assembly, connect with high-pressure bolt by Screw-thread sealing plug with SW with outside ring.6. rectifying column maximum working pressure 35MPa, tower internal diameter 200~500mm, tower height 10~32m can realize not manufacturing and designing of co-content rectifying column.7. each material inlet and outlet caliber are DN32~DN50.
Below rectifying column and use preference and in conjunction with the accompanying drawings the utility model be described in detail, but and do not mean that restriction scope of the present utility model.
Tower body adopts the stainless-steel seamless pipe manufacturing, and material is 0Cr18Ni9, and tower wall thickness 20~45mm, maximum working pressure are 35MPa; The built-in filler of tower is a stainless steel, and material is 0Cr18Ni9.Used filler is regular corrugation filler, and is cylindrical, and the bottom surface diameter is consistent with the packed tower internal diameter, 200~500mm, and high 80~100mm closely piles up in tower in turn to the cat head place.The filler voidage is 085~0.95, and specific surface is 910~3200 squares of m/ cube of m.
Example 1:300L rectifying column, rectifying column maximum working pressure 32MPa, tower wall thickness 30mm, tower internal diameter 210mm, tower height 12m.Body of the tower divides three sections.Whole rectifying column be by tower top cover, three sections bodies of the tower, material distributor assembly, CO 2Feed distributor, the stainless steel wire corrugated wire gauze packing, SW with outside ring, high-pressure bolt is formed.Establish temperature sensor on the tower top cover, measure the overhead fraction temperature, material outlet pipe caliber is DN32, material outlet Guan Shangshe safety valve, and pressure sensor more than guarantees safety and measures the rectifying tower top outlet pressure.Body of the tower is formed by three sections, on, in two the joint height be 3.6m, the high 4.2m of following joint, material is the 0Cr18Ni9 stainless steel tube.Establish by the high pressure Screw-thread sealing plug between joint and middle joint, middle joint and the following joint on the body of the tower and connect with Luo Ta.The sealing of use SW with outside ring.The filler gripper shoe of tower bottom is located at 600mm place at the bottom of tower, and the feed carbon dioxide pipe is located under the tower and saves from tower bottom 500mm place, and caliber is DN32.On the art, middle part filler packed height is 3.55m, the bottom is 4.15m.Filler is the stainless steel cloth corrugated, makes regular cylindrically, and diameter is 210mm, each high 50mm.The tower filler voidage of joint from the filler gripper shoe to its height 1/2 filling down is 0.83, and specific area is 910m 2/ m 3, the voidage that remainder is filled filler is 0.92, specific area is 1650m 2/ m 3Tower top cover is established temperature sensor, material outlet pipe, establishes the safety valve that pressure rating is 32MPa in the outlet.The high 100mm of material distributor assembly stainless steel cylinder.Tower bottom is established temperature sensor, material outlet pipe.
Example 2.1000L rectifying column rectifying column operating pressure is 30MPa, tower wall thickness 40mm, tower internal diameter 300mm, tower height 16m.Body of the tower divides four joints, the high 4m of every joint.It is 3.2m that tower descends joint to fill packed height most, and the filler voidage is 0.84, and specific area is 960m 2/ m 3, all the other respectively save the filler packed height is 3.85m, and the filler voidage is 0.93, and specific area is 2100m 2/ m 3Each filler diameter is 300mm, high 50mm.Each material inlet and outlet caliber are DN40.Establish material distributor assembly between the Ta Gejie, the high 100mm of stainless steel cylinder.Tower descends the filler gripper shoe of joint to be located at 650mm place at the bottom of tower most, and the carbon dioxide inlet pipe is located at 600mm place at the bottom of tower.Between each joint and the material distributor assembly, all connect the SW with outside ring sealing between tower lid and the body of the tower with the high pressure securing member.All the other conditions are with example 1.
Example 3.3000L rectifying column rectifying column operating pressure 30MPa, tower wall thickness 64mm, tower height 16m, tower internal diameter 500mm, body of the tower divides four joints, and each material inlet and outlet caliber are DN50, and all the other conditions are with example 2.

Claims (7)

1, a kind of rectifying column of supercritical carbon dioxide fluid continuous countercurrent extraction, comprise tower body, Ta Gai, material import and export, steam jacket and valve, it is characterized in that tower body divides 3~8 joints, tower is gone up a joint top most has the tower lid to connect, cat head has material outlet, and tower next section is established carbon dioxide inlet and material outlet, establishes material inlet in the middle of two joint towers, filler is housed, every joint tower peripheral hardware steam jacket and steam inlet, condensation-water drain in the tower body.
2, rectifying column according to claim 1 is characterized in that tower height 10~32m, and every joint tower body height is basic identical, 3~5m, tower diameter 200~500mm.
3, rectifying column according to claim 2 is characterized in that tower height 10~15m, and tower body divides 3 joints, the basic identical 3~5m of every joint tower body height, tower diameter 200~500mm.
4, rectifying column according to claim 2 is characterized in that tower height 15~20m, and tower body divides 4 joints, the basic identical 3~5m of every joint tower body height, tower internal diameter 200~500mm.
5, rectifying column according to claim 1 and 2 is characterized in that establishing material inlet between per two joint bodies of the tower, and import department establishes distributor.
6, rectifying column according to claim 1 and 2 is characterized in that filler is the cylindrical structured packing identical with the tower internal diameter, and a plurality of cylindrical structured packings stack.
7, rectifying column according to claim 1 and 2, it is characterized in that apart from rectifying column at the bottom of next joint tower 500~800mm place establish gripper shoe, other establish support ring at the bottom of respectively saving tower, support top filler, filler adopts regular stainless steel helices, specific area 900~3000m 2/ m 3, voidage is 0.80~0.93, to the top, the space of one section dress material distributor is stayed to filler by the intermediate material import departments of two joint towers from the gripper shoe of every joint tower bottom or ring filling.
CN 02228379 2002-02-07 2002-02-07 Fractionating rectifying tower for supercritical carbon dioxide fluid continuous countercurrent extraction Expired - Fee Related CN2561484Y (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102250691A (en) * 2011-06-09 2011-11-23 安徽中草香料有限公司 Process for preparing ginger essential oil
CN102321384A (en) * 2011-06-21 2012-01-18 西北大学 Liquid-phase supercritical method for removing and separating spiciness from capsicum red pigment and device special for liquid-phase critical method
CN104548655A (en) * 2013-10-28 2015-04-29 贵州航天乌江机电设备有限责任公司 Manufacturing method of hanging basket in extraction kettle and hanging basket
CN111100107A (en) * 2018-10-26 2020-05-05 中国石油化工股份有限公司 Method for removing pigment and impurities in crude lactide
CN113471515A (en) * 2021-06-30 2021-10-01 广州市浩立生物科技有限公司 Method for recycling lithium battery electrolyte by combining supercritical extraction rectification and molecular distillation
CN114275872A (en) * 2022-01-14 2022-04-05 杭州深瑞水务有限公司 Oxidation tower for subcritical water oxidation process
CN114870429A (en) * 2022-04-25 2022-08-09 贵州航天乌江机电设备有限责任公司 Wall thickness variable continuous extractor barrel and continuous extractor

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102250691A (en) * 2011-06-09 2011-11-23 安徽中草香料有限公司 Process for preparing ginger essential oil
CN102321384A (en) * 2011-06-21 2012-01-18 西北大学 Liquid-phase supercritical method for removing and separating spiciness from capsicum red pigment and device special for liquid-phase critical method
CN102321384B (en) * 2011-06-21 2013-11-20 西北大学 Liquid-phase supercritical method for removing and separating spiciness from capsicum red pigment and device special for liquid-phase critical method
CN104548655A (en) * 2013-10-28 2015-04-29 贵州航天乌江机电设备有限责任公司 Manufacturing method of hanging basket in extraction kettle and hanging basket
CN104548655B (en) * 2013-10-28 2016-08-17 贵州航天乌江机电设备有限责任公司 The manufacture method of hanging basket and hanging basket in a kind of extraction kettle
CN111100107A (en) * 2018-10-26 2020-05-05 中国石油化工股份有限公司 Method for removing pigment and impurities in crude lactide
CN111100107B (en) * 2018-10-26 2021-03-05 中国石油化工股份有限公司 Method for removing pigment and impurities in crude lactide
CN113471515A (en) * 2021-06-30 2021-10-01 广州市浩立生物科技有限公司 Method for recycling lithium battery electrolyte by combining supercritical extraction rectification and molecular distillation
CN114275872A (en) * 2022-01-14 2022-04-05 杭州深瑞水务有限公司 Oxidation tower for subcritical water oxidation process
CN114870429A (en) * 2022-04-25 2022-08-09 贵州航天乌江机电设备有限责任公司 Wall thickness variable continuous extractor barrel and continuous extractor
CN114870429B (en) * 2022-04-25 2023-08-04 贵州航天乌江机电设备有限责任公司 Wall thickness variable continuous extraction device cylinder and continuous extraction device

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C19 Lapse of patent right due to non-payment of the annual fee
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