CN109173310A - Dimethoxym ethane rectifying column - Google Patents

Dimethoxym ethane rectifying column Download PDF

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Publication number
CN109173310A
CN109173310A CN201810995558.6A CN201810995558A CN109173310A CN 109173310 A CN109173310 A CN 109173310A CN 201810995558 A CN201810995558 A CN 201810995558A CN 109173310 A CN109173310 A CN 109173310A
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CN
China
Prior art keywords
tower
section
packing section
packing
tower body
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.)
Pending
Application number
CN201810995558.6A
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Chinese (zh)
Inventor
顾国兴
程凯
顾聪
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.)
ZHANGJIAGANG KEHUA CHEMICAL EQUIPMENT MANUFACTURING Co Ltd
Original Assignee
ZHANGJIAGANG KEHUA CHEMICAL EQUIPMENT MANUFACTURING Co Ltd
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.)
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Publication date
Application filed by ZHANGJIAGANG KEHUA CHEMICAL EQUIPMENT MANUFACTURING Co Ltd filed Critical ZHANGJIAGANG KEHUA CHEMICAL EQUIPMENT MANUFACTURING Co Ltd
Priority to CN201810995558.6A priority Critical patent/CN109173310A/en
Publication of CN109173310A publication Critical patent/CN109173310A/en
Pending legal-status Critical Current

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Classifications

    • 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
    • B01D3/009Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
    • 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
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C41/00Preparation of ethers; Preparation of compounds having groups, groups or groups
    • C07C41/48Preparation of compounds having groups
    • C07C41/58Separation; Purification; Stabilisation; Use of additives

Abstract

This application discloses a kind of dimethoxym ethane rectifying columns, including tubular tower body, it is set to the skirt of the tower body bottom, the tower top for being set to the tower body top is hung, tower reactor section is followed successively by inside the tower body from lower to upper, tower tray section, packing section and tower top section, the packing section includes at least the first packing section and the second packing section, the upper end of first packing section and the second packing section is provided with liquid distribution trough, the lower part of second packing section is provided with liquid header, it is filled out in first packing section and the second packing section equipped with solid catalysis filler, inlet port and outlet port are opened up on the tower body, the feed inlet includes the gas circulation port that tower reactor section upper side is arranged in, material inlet between tower tray section and the first packing section is set, the refluxing opening of tower top section side is set, the discharge port includes being arranged at tower reactor section bottom The gas vent that the liquid circulation mouth and tower bottoms in portion export and be arranged at the top of tower top section.Product purity can be improved in this application.

Description

Dimethoxym ethane rectifying column
Technical field
This application involves the production equipment technology of dimethoxym ethane, in particular to a kind of dimethoxym ethane rectifying column.
Background technique
Dimethoxym ethane, for the colourless transparent liquid of micro- tool smell.In recent years, domestic to be continued to use always in production dimethoxym ethane technique Sulfuric acid process, to the seriously corroded of equipment.Japan develops to solve the disadvantage of old industry law and cooperate dimethoxym ethane device to urge Change rectification method synthesizing dimethoxym ethane.Catalyst uses hard resin, fundamentally solves the problems, such as equipment corrosion, and greatly improve The yield and quality of product.Shandong University Of Yantai successfully has developed on the basis of Japanese technique with the anti-of solid catalyst It should be with distillation United Technologies, currently, domestic only fewer companies are industrialized.The method uses a tower process, normal pressure behaviour in tower Make, catalyst is filled in tower, and reaction and rectifying carry out in tower.But this process equipment can only produce dimethoxym ethane concentration 85 ~92% dimethoxym ethane product cannot obtain the product of high concentration, limit dimethoxym ethane in this way in the application in some fields. So needing to propose to improve.
Summary of the invention
The purpose of the present invention is to provide a kind of dimethoxym ethane rectifying columns, to overcome deficiency in the prior art.
To achieve the above object, the invention provides the following technical scheme:
The embodiment of the present application discloses a kind of dimethoxym ethane rectifying column, including tubular tower body, is set to the tower body bottom Skirt, the tower top for being set to the tower body top are hung, and are followed successively by tower reactor section inside the tower body from lower to upper, tower tray section, are filled out Expect that section and tower top section, the packing section include at least the first packing section and the second packing section, first packing section and second is filled out The upper end of material section is provided with liquid distribution trough, and the lower part of second packing section is provided with liquid header, and described first fills out It is filled out in material section and the second packing section equipped with solid catalysis filler, opens up inlet port and outlet port, the charging on the tower body Mouthful include be arranged in the gas circulation port of tower reactor section upper side, the raw material being arranged between tower tray section and the first packing section into Mouth, the refluxing opening that tower top section side is arranged in, the discharge port includes the liquid circulation mouth and tower reactor that tower reactor section bottom is arranged in The gas vent that liquid exports and is arranged at the top of tower top section.
Preferably, in above-mentioned dimethoxym ethane rectifying column, the skirt includes skirt cylinder and Basic annular plate, the skirt Cylinder top is welded in the tower body bottom, and the Basic annular plate is fixed on the bottom of the skirt cylinder, the Basic annular plate It is inside recessed with the U-shaped opening slot of several outward openings, the equidistant circumference array of U-shaped opening slot is set to the foundation ring Plate, the skirt cylinder body outer wall are equipped with foundation bolt seat, and the foundation bolt seat includes being fixed on the skirt cylinder body outer wall Circumferential butt is recessed with the first through hole being correspondingly arranged with the U-shaped opening slot, the first through hole two sides point in the cover board It is not provided with the first gusset for connecting the cover board and Basic annular plate, the first through hole top is equipped with backing plate, in the backing plate It is recessed with the second through-hole, the diameter of second through-hole is less than the diameter of the first through hole, and the foundation bolt seat further includes Earth plate, the earth plate are fixed on first gusset.
Preferably, in above-mentioned dimethoxym ethane rectifying column, the skirt cylinder be equipped with respectively with the tower bottoms outlet and The first fairlead of ring-type that liquid phase circulation mouth is correspondingly arranged, the tower bottoms outlet and liquid phase circulation mouth pass through the second extraction respectively Pipe is connected to the tower body bottom, and protrudes from skirt cylinder, and the outer wall of second fairlead is provided with to be drawn with described first The second gusset that inside pipe wall is correspondingly arranged out.
Preferably, in above-mentioned dimethoxym ethane rectifying column, the skirt cylinder is equipped with close to one end outer wall of the tower body Gas vent, the skirt cylinder body bottom are recessed with drainage hole, and the skirt cylinder is additionally provided with inspection hole and tail is hung.
Preferably, in above-mentioned dimethoxym ethane rectifying column, the tower body is filled out in tower reactor section, tower tray section, tower tray section and first Between material section, between the first packing section and the second packing section and tower top section is convexly equipped with manhole to be opened/closed respectively.
Preferably, in above-mentioned dimethoxym ethane rectifying column, tower reactor section side offers the interface of about three distributions, point Not Wei first interface, second interface and third interface, the first interface includes an interface, and is connected to external pressure meter, institute Stating second interface includes two interfaces, and is connected to that external liquidometer and far transmission level meter, the third interface include on the spot Three interfaces are connected to external liquidometer, far transmission level meter and thermometer on the spot.
Preferably, in above-mentioned dimethoxym ethane rectifying column, the tower body is located at first packing section and the second packing section The side of lower section offer the 4th interface respectively, two the 4th interfaces are connected to external thermometer, the tower top section Side is equipped with the 5th interface, and is connected to external pressure meter.
Preferably, in above-mentioned dimethoxym ethane rectifying column, the inner wall of the tower body is equipped with set corresponding with the material inlet The buffer board set, the tower bottoms outlet is interior to be equipped with vortex shield.
Compared with the prior art, the advantages of the present invention are as follows: the utility model dimethoxym ethane rectifying column has tower tray section and filler simultaneously Section greatlys save equipment investment so that reaction process and distillation process are completed in the same apparatus, saves the production time, and Multistage catalytic filler is loaded in same rectifying column enables pure and mild formaldehyde in catalytic rectifying column using catalytic filler While completing condensation reaction, the separation of product is efficiently completed, the reactant of generation is steamed from reaction zone immediately, is destroyed reversible The chemical balance of reaction increases the conversion ratio of reaction, improves the selectivity of reaction.
Detailed description of the invention
In order to illustrate the technical solutions in the embodiments of the present application or in the prior art more clearly, to embodiment or will show below There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this The some embodiments recorded in application, for those of ordinary skill in the art, without creative efforts, It is also possible to obtain other drawings based on these drawings.
Fig. 1 show the structural schematic diagram of dimethoxym ethane rectifying column in the specific embodiment of the invention.
Fig. 2 show the structural schematic diagram of foundation bolt seat in the specific embodiment of the invention.
Fig. 3 show the side view of foundation bolt seat in the specific embodiment of the invention.
Fig. 4 show the scheme of installation of the first fairlead and the second fairlead in the specific embodiment of the invention.
Fig. 5 show the scheme of installation of the second gusset in the specific embodiment of the invention.
Fig. 6 show the structural schematic diagram of buffer board in the specific embodiment of the invention.
Fig. 7 show the scheme of installation of vortex shield in the specific embodiment of the invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out detailed retouch It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention In embodiment, those of ordinary skill in the art's every other implementation obtained without making creative work Example, shall fall within the protection scope of the present invention.
Join shown in Fig. 1 to Fig. 7, the dimethoxym ethane rectifying column in the present embodiment, including tubular tower body 100, is set to tower body 100 The skirt 200 of bottom, the tower top davit 300 for being set to 100 top of tower body are followed successively by tower reactor section inside tower body 100 from lower to upper 400, tower tray section 500, packing section 600 and tower top section 700, packing section 600 include at least the first packing section 610 and the second packing section 620, the upper end of the first packing section 610 and the second packing section 620 is provided with liquid distribution trough 800, under the second packing section 620 Portion is provided with liquid header 900, fills out in the first packing section 610 and the second packing section 620 equipped with solid catalysis filler, tower body Inlet port and outlet port are opened up on 100, feed inlet includes the gas circulation port 110 that 400 upper side of tower reactor section is arranged in, setting Material inlet 120 between tower tray section 500 and the first packing section 610, the refluxing opening 130 that 700 side of tower top section is set, out Material mouth includes that the liquid circulation mouth 140 that 400 bottom of tower reactor section is arranged in and tower bottoms export 150 and be arranged in tower top section 700 The gas vent 160 at top.
In the technical solution, the preferred highly acid large aperture cation resin catalyzing agent of solid catalysis filler or HZSM-5 molecule The solid acid catalysts such as sieve are made, and pure and mild formaldehyde is enabled to complete condensation reaction in catalytic rectifying column, in use process, Methanol is added by material inlet, methanol flows into tower reactor Duan Houcong liquid circulation mouth and enters reboiler, and reboiler is with low-pressure steam For the methanol that heat source heating flows into, methanol enters in tower body after being heated to form gas from gas circulation port, and gas is by bottom in tower body Portion constantly flows up, and formalin liquid then is added from refluxing opening and flows from top to bottom, and methanol gas flows from lower to upper, It is evenly distributed in liquid distribution trough by the formalin under tower top stream and flows downwardly into the second packing section, formalin and rising Gas continue to flow downward into liquid header after the second filler section surface comes into full contact with, liquid header receives liquid It is sent after collection to liquid distribution trough and redistributes liquid, the liquid being re-distributed flows into the first packing section, at this time liquid and rising Gas continue to flow through tower tray Duan Houzhi tower reactor section, in the process, formaldehyde down after the first filler section surface comes into full contact with It reacts with methanol and generates dimethoxym ethane, the dimethoxym ethane of generation steams immediately, destroys the chemical balance of reversible reaction, increases reaction Conversion ratio, improve the selectivity of reaction, meanwhile, acetal is destroyed using water contained in formalin and is total to what alcohol was formed Object is boiled, the concentration of tower top dimethoxym ethane is improved, dimethoxym ethane is flowed out by gas vent, and the gas condensation process flowed out from tower top obtains The dimethoxym ethane and formaldehyde of high concentration, formaldehyde is made formalin and is flowed into tower body by refluxing opening again, when liquid flows across trays section, Dimethoxym ethane and formaldehyde in liquid switch to gas phase rising, and the liquid for eventually entering into tower reactor section contains methanol and the first lower than 500ppm Aldehyde, then by the processing of the equipment such as external reboiler, methanol enters in tower body after being heated to form gas again from gas circulation port, The water contained lower than 500ppm formaldehyde returns to formaldehyde absorbing tower as process water, as absorbing liquid, to realize closing for process water Road circulation.
Further, skirt 200 includes skirt cylinder 210 and Basic annular plate 220, and 210 top of skirt cylinder is welded in tower 100 bottom of body, Basic annular plate 220 are fixed on the bottom of skirt cylinder 210, several outward openings are recessed in Basic annular plate 220 U-shaped opening slot 221, the equidistant circumference array of U-shaped opening slot 221 is set to Basic annular plate 220, and 210 outer wall of skirt cylinder is set There is foundation bolt seat, foundation bolt seat includes the circumferential butt 230 for being fixed on 210 outer wall of skirt cylinder, is recessed in cover board 230 The first through hole 231 being correspondingly arranged with U-shaped opening slot 221,231 two sides of first through hole are respectively arranged with connecting cover plate 230 and base First gusset 240 of plinth ring flat-plate 220,231 top of first through hole are equipped with backing plate 250, are recessed with the second through-hole 251 in backing plate 250, The diameter of second through-hole 251 is less than the diameter of first through hole 231, and foundation bolt seat further includes earth plate 260, and earth plate 260 is solid Due to the first gusset 240.
In the technical solution, the dimethoxym ethane rectifying column is fixed using the foundation bolt of M54, U-shaped opening slot it is straight Diameter is 80mm, and the first diameter passed through is 75mm, facilitates being arranged for foundation bolt, and the diameter of the second through-hole is 59mm, to this Dimethoxym ethane rectifying column lifts and with after foundation bolt positioning, backing plate is welded in cover board, so that the dimethoxym ethane rectifying column is fixed more Add stabilization.
Further, skirt cylinder 210 is equipped with is correspondingly arranged with liquid circulation mouth 140 and tower bottoms outlet 150 respectively Cyclic annular first fairlead 270, liquid circulation mouth 140 and tower bottoms outlet 150 are connected to tower body by the second fairlead 170 respectively 100 bottoms, and skirt cylinder 210 is protruded from, the outer wall of the second fairlead, which is provided with, draws what inside pipe wall was correspondingly arranged with first Second gusset 171.
In the technical solution, the outer wall of the second fairlead is equipped with the second gusset of three pieces of equidistant circumference array settings, the Inside pipe wall interval 2mm setting is drawn with first in two gusset outer ends, and the second fairlead is avoided to deform or be bent over.
Further, skirt cylinder 210 is equipped with gas vent 211,210 bottom of skirt cylinder close to one end outer wall of tower body 100 Portion is recessed with drainage hole 212, and skirt cylinder 210 is additionally provided with inspection hole 280 and tail hangs 290.
In the technical solution, gas vent and drainage hole for balance pressure change caused by due to temperature change and discharge because Temperature change and the liquid generated, for inspection hole for observing skirt inner case, tail hangs the lifting for skirt.
Further, tower body 100 is between tower reactor section 400, tower tray section 500, tower tray section 500 and the first packing section 610, Between one packing section 610 and the second packing section 620 and tower top section 700 is convexly equipped with manhole 180 to be opened/closed respectively.
In the technical scheme, manhole is in normally off, opening when needing to check or safeguard.
Further, 400 side of tower reactor section offers first interface 1, second interface 2 and the third interface of about three distributions 3, first interface includes an interface, and is connected to external pressure meter, and second interface includes two interfaces, and is connected to outside just Ground liquidometer and far transmission level meter, third interface include three interfaces, be connected to external liquidometer on the spot, far transmission level meter and Thermometer.
In the technical scheme, to monitor liquid level and temperature in tower reactor section.
Further, the side that tower body 100 is located at the lower section of the first packing section 610 and the second packing section 620 opens up respectively There is the 4th interface 4, two the 4th interfaces are connected to external thermometer, and 700 side of tower top section is equipped with the 5th interface 5, and connects In external pressure meter.
In the technical scheme, the 4th interface is connected to external thermometer monitoring the first packing section 610 and second and fills out Expect the temperature of section 620, the dimethoxym ethane after guaranteeing reaction can steam in time, destroy the chemical balance of reversible reaction, increase reaction Conversion ratio improves the selectivity of reaction.
Further, the inner wall of tower body 100 is equipped with the buffer board 121 being correspondingly arranged with material inlet 120, tower bottoms outlet Vortex shield 151 is equipped in 150.
In the technical scheme, buffer board is used to buffered methanol to the impact inside tower body, and vortex shield is used to avoid or subtract Issuable vortex when few tower bottoms extraction.
In conclusion the utility model dimethoxym ethane rectifying column has tower tray section and packing section simultaneously, so that reaction process and rectifying Journey is completed in the same apparatus, greatlys save equipment investment, saves the production time, and is loaded multistage in same rectifying column and urged Change filler, using catalytic filler, while enabling pure and mild formaldehyde to complete condensation reaction in catalytic rectifying column, efficiently The separation of product is completed, the reactant of generation steams from reaction zone immediately, destroys the chemical balance of reversible reaction, increase reaction Conversion ratio improves the selectivity of reaction.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that There is also other identical elements in process, method, article or equipment including the element.
The above is only the specific embodiment of the application, it is noted that for the ordinary skill people of the art For member, under the premise of not departing from the application principle, several improvements and modifications can also be made, these improvements and modifications are also answered It is considered as the protection scope of the application.

Claims (8)

1. a kind of dimethoxym ethane rectifying column, which is characterized in that including tubular tower body, the skirt that is set to the tower body bottom, setting Tower top in the tower body top is hung, and is followed successively by tower reactor section, tower tray section, packing section and tower top inside the tower body from lower to upper Section, the packing section include at least the first packing section and the second packing section, the upper end of first packing section and the second packing section It is provided with liquid distribution trough, the lower part of second packing section is provided with liquid header, first packing section and second It is filled out in packing section equipped with solid catalysis filler, inlet port and outlet port is opened up on the tower body, the feed inlet includes setting In the gas circulation port of tower reactor section upper side, the material inlet being arranged between tower tray section and the first packing section, setting in tower Push up section side refluxing opening, the discharge port include be arranged in tower reactor section bottom liquid circulation mouth and tower bottoms outlet and Gas vent at the top of tower top section is set.
2. dimethoxym ethane rectifying column according to claim 1, it is characterised in that: the skirt includes skirt cylinder and foundation ring Plate, the skirt cylinder top are welded in the tower body bottom, and the Basic annular plate is fixed on the bottom of the skirt cylinder, institute The U-shaped opening slot that several outward openings are recessed in Basic annular plate is stated, the equidistant circumference array of U-shaped opening slot is set to institute Basic annular plate is stated, the skirt cylinder body outer wall is equipped with foundation bolt seat, and the foundation bolt seat includes being fixed on the skirt cylinder The circumferential butt of external wall is recessed with the first through hole being correspondingly arranged with the U-shaped opening slot in the cover board, and described first is logical Hole two sides are respectively arranged with the first gusset for connecting the cover board and Basic annular plate, and the first through hole top is equipped with backing plate, institute It states and is recessed with the second through-hole in backing plate, the diameter of second through-hole is less than the diameter of the first through hole, the foundation bolt Seat further includes earth plate, and the earth plate is fixed on first gusset.
3. dimethoxym ethane rectifying column according to claim 2, it is characterised in that: the skirt cylinder be equipped with respectively with the tower The first fairlead of ring-type that kettle liquid outlet and liquid phase circulation mouth are correspondingly arranged, the tower bottoms outlet and liquid phase circulation mouth lead to respectively Cross the second fairlead and be connected to the tower body bottom, and protrude from skirt cylinder, the outer wall of second fairlead be provided with The second gusset that the first extraction inside pipe wall is correspondingly arranged.
4. dimethoxym ethane rectifying column according to claim 2, it is characterised in that: the skirt cylinder is close to the one of the tower body Outer wall is held to be equipped with gas vent, the skirt cylinder body bottom is recessed with drainage hole, and the skirt cylinder is additionally provided with inspection hole and tail is hung.
5. dimethoxym ethane rectifying column according to claim 1, it is characterised in that: the tower body is in tower reactor section, tower tray section, tower tray Between section and the first packing section, between the first packing section and the second packing section and tower top section is convexly equipped with people to be opened/closed respectively Hole.
6. dimethoxym ethane rectifying column according to claim 1, it is characterised in that: tower reactor section side offers about three points The interface of cloth, respectively first interface, second interface and third interface, the first interface include an interface, and are connected to outer Portion's pressure gauge, the second interface include two interfaces, and are connected to external liquidometer and far transmission level meter on the spot, and described the Three interfaces include three interfaces, are connected to external liquidometer, far transmission level meter and thermometer on the spot.
7. dimethoxym ethane rectifying column according to claim 1, it is characterised in that: the tower body be located at first packing section and The side of the lower section of second packing section offers the 4th interface respectively, and two the 4th interfaces are connected to external thermometer, The tower top section side is equipped with the 5th interface, and is connected to external pressure meter.
8. dimethoxym ethane rectifying column according to claim 1, it is characterised in that: the inner wall of the tower body is equipped with and the raw material The buffer board that import is correspondingly arranged, the tower bottoms outlet is interior to be equipped with vortex shield.
CN201810995558.6A 2018-08-29 2018-08-29 Dimethoxym ethane rectifying column Pending CN109173310A (en)

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