CN109836309A - Utilize the solid-state methanol sodium alkali process units of vacuum pump recycling methanol - Google Patents
Utilize the solid-state methanol sodium alkali process units of vacuum pump recycling methanol Download PDFInfo
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- CN109836309A CN109836309A CN201910243033.1A CN201910243033A CN109836309A CN 109836309 A CN109836309 A CN 109836309A CN 201910243033 A CN201910243033 A CN 201910243033A CN 109836309 A CN109836309 A CN 109836309A
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- methanol
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- negative pressure
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- vacuum pump
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims abstract description 288
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000003513 alkali Substances 0.000 title claims abstract description 22
- YWOITFUKFOYODT-UHFFFAOYSA-N methanol;sodium Chemical compound [Na].OC YWOITFUKFOYODT-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000004064 recycling Methods 0.000 title claims abstract description 22
- 238000001816 cooling Methods 0.000 claims abstract description 109
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000010079 rubber tapping Methods 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000011084 recovery Methods 0.000 claims abstract description 12
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 10
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims description 36
- 238000007789 sealing Methods 0.000 claims description 26
- 239000007792 gaseous phase Substances 0.000 claims description 23
- 239000007791 liquid phase Substances 0.000 claims description 23
- 230000001476 alcoholic effect Effects 0.000 claims description 12
- 239000012071 phase Substances 0.000 claims description 12
- 230000008878 coupling Effects 0.000 claims description 11
- 238000010168 coupling process Methods 0.000 claims description 11
- 238000005859 coupling reaction Methods 0.000 claims description 11
- 238000009527 percussion Methods 0.000 claims description 11
- 239000002826 coolant Substances 0.000 claims description 10
- 238000007599 discharging Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 230000004087 circulation Effects 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000013589 supplement Substances 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 3
- 239000008246 gaseous mixture Substances 0.000 claims description 3
- 239000011229 interlayer Substances 0.000 claims description 3
- 230000037237 body shape Effects 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 13
- 238000005452 bending Methods 0.000 abstract description 4
- 238000011068 loading method Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 description 11
- 238000005265 energy consumption Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- LYQARTBYZUZKPJ-UHFFFAOYSA-N [Na].CO.CO Chemical compound [Na].CO.CO LYQARTBYZUZKPJ-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A kind of solid-state methanol sodium alkali process units using vacuum pump recycling methanol, including sodium methoxide synthesis unit, rake type drier, methanol negative-pressure recovery device, in the present invention, the power that bar is tapped to the second stopper is vertical with fixed link, the shaft connecting with fixed link is only by the moment loading for tapping bar, it not will cause shaft bending, it taps bar and strikes the second stopper, then vibration is provided to fixed link, shaft, the material sticks in shaft can be removed, the water conservancy diversion sieve plate being staggered from top to bottom in cooling tower body, can the effective use liquid methanol that has agglomerated capture methanol gas, and then promote methanol gas cohesion, the methanol gas volatilized in rake type drier is effectively recycled, reduce the low problem of Methanol Recovery rate caused by the outlet for the methanol gas for having little time cohesion, the cooling unit of multistage can be according to different produced quantities The adjustment for carrying out the cooler number that overhead vapours flows through avoids the cooling insufficient or undercooling of single cooler.
Description
Technical field
The present invention relates to sodium methoxide synthesis device technical field, in particular to a kind of solid-state using vacuum pump recycling methanol
Methanol sodium alkali process units.
Background technique
Industrially mostly use alkaline process produce sodium methoxide, be dehydrated required methanol steam from synthetic tower tower bottom be added, methanol and
The mixed vapour of water is expelled to rectifying column progress rectifying separation by synthesizing column overhead, and obtained anhydrous methanol enters synthetic tower circulation
It uses, during this, the stability contorting of synthetic tower and rectifying column operating condition is being critical to for sodium methoxide controlling of production process
Point, the cooling of conventional the top of the distillation column steam use single cooler, and modification scope is very limited, it is difficult to meet synthetic tower
With the requirement of rectifying column operating condition accuracy controlling, the sodium methoxide of liquid it is subsequent will also pass through rake type drier drying process,
The biggish material of stickiness is easily adhered in shaft, and conventional stamp directly strikes shaft, will cause shaft bending and can not
It works normally, after the methanol generated in sodium methoxide drying process is extracted out by vacuum pump, into the storage tank for having cooling sandwith layer, because coming
Not as good as cooling, can also some methanol gas can be emptied by vacuum pump and methanol be caused to waste.
Summary of the invention
In view of this, in view of the above deficiencies, it is necessary to propose that a kind of high utilization vacuum pump of Methanol Recovery rate recycles methanol
Solid-state methanol sodium alkali process units.
A kind of solid-state methanol sodium alkali process units using vacuum pump recycling methanol, including sodium methoxide synthesis unit, rake
Formula drying machine, methanol negative-pressure recovery device, the sodium methoxide synthesis unit include the first preheater, synthetic tower, rectifying column, multistage
Cooling unit, the second preheater, the synthetic tower left upper portion have a feed(raw material)inlet, and alcoholic lye enters the first preheater
Shell side is added synthetic tower by feed(raw material)inlet after the heating of the first preheater, has a gaseous phase outlet at the top of the synthetic tower,
Middle and lower part has a gas phase entrance, the gaseous phase outlet of synthetic tower and the gas phase entrance pipeline of rectifying column on the left of the rectifying column
Connection, so that the gaseous mixture of first alcohol and water is sent into rectifying column in synthetic tower, there is a gas phase to go out for described the top of the distillation column
Mouthful, the gaseous phase outlet of rectifying column connect with the tube-side inlet of the first preheater, the gaseous phase outlet of rectifying column and the first preheater it
Between pipeline on the first pneumatic operated valve is installed, the cooling on the right side of the tube side inlet/outlet of the first preheater and multistage cooling unit always enters
Mouth connection, the gaseous phase outlet of rectifying column are connect with the cooling main entrance in the left side of multistage cooling unit, in multistage cooling unit
Second pneumatic operated valve, second pneumatic operated valve are installed on the pipeline between the cooling main entrance in left side and the gaseous phase outlet of rectifying column
Between the first pneumatic operated valve and multistage cooling unit, the multistage cooling unit has a methanol inlet, to be multistage cold
But unit supplements anhydrous methanol, and the multistage cooling unit has a total coolant outlet, the multistage cooling unit it is total cold
But outlet is connect with the second preheater by pipeline, is cooled down in multistage and is equipped with the on the pipeline between unit and the second preheater
Three pneumatic operated valves, rectifying column right upper portion are equipped with the first liquid phase entrance, and total coolant outlet of the cooling unit of multistage passes through pipeline and essence
The first liquid phase entrance connection of tower is evaporated, the 4th pneumatic operated valve, institute are installed on the pipeline between multistage cooling unit and rectifying column
The 4th pneumatic operated valve is stated between third pneumatic operated valve and rectifying column, the synthetic tower left lower has a methanol eddy mouth,
The outlet of second preheater is connected by the methanol eddy mouth of pipeline and synthetic tower, and the multistage cooling unit includes first cooling
Device, the second cooler, third cooler, holding tank, left side of the first cooler left hand inlet port as multistage cooling unit
Cooling main entrance, the right side of the first cooler right hand inlet port and the second cooler left hand inlet port as multistage cooling unit
Cooling main entrance, the outlet of the first cooler, the second cooler, third cooler connect with the entrance of holding tank side,
Outlet at the top of holding tank is connect with the entrance on the right side of the second cooler, the entrance on the left of third cooler by pipeline, is kept in
Methanol inlet of the entrance of box top as multistage cooling unit, the outlet of holding tank bottom is as the total cold of multistage cooling unit
Outlet, it is described synthesis tower bottom liquid-phase outlet and rake type drier liquid phase entrance by pipeline connect, by sodium methoxide with
Methanol solution is conveyed into rake type drier, and the rake type drier includes cylinder, shaft, taps component, the left and right of the shaft
Both ends are rotatablely connected with the both ends end face of cylinder respectively, and the percussions component includes fixed link, percussion bar, the first stopper, the
Two stoppers, fixed link are vertically arranged with respect to shaft, and one end of fixed link is connecting pin, and connecting pin and the shaft of fixed link are fixed
Connection, the other end of fixed link are free end, and the one end for tapping bar is connecting pin, tap the connecting pin of bar and the freedom of fixed link
End rotation connection, the other end for tapping bar is free end, is provided with the first stopper, the second stopper in fixed link, first
Block is arranged close to the free end of fixed link, and the second block is arranged close to the connecting pin of fixed link, taps between bar and fixed link
Angle be 180 °, the first stopper prevents to tap bar to be rotated counterclockwise, and tapping the angle between bar and fixed link is 0 °, second
Stopper prevents percussion bar from rotating clockwise, and the methanol negative-pressure recovery device includes cooling tower, the first vacuum pump, the cooling
The gaseous phase outlet of the cylinder of the gas phase entrance and rake type drier of the bottom of tower connects, so that the first volatilized in rake type drier
Alcohol gas enters cooling tower, and the entrance of the first vacuum pump and the top of cooling tower evacuate mouth connection, cold to enter for methanol gas
But tower provides draft, and the cooling tower includes that staggered linde sieve tray, tower body are folder from top to bottom in tower body and tower body
Layer structure, circulation has cooling medium in the interlayer of tower body, and the linde sieve tray is horizontally set in tower body, one end of linde sieve tray
It is connect with tower body inner wall, the other end and the tower body inner wall of linde sieve tray are not connected to, and linde sieve tray is opposite with tower body unconnected one
End is bent upwards.
Preferably, the solid-state methanol sodium alkali process units using vacuum pump recycling methanol further includes that negative pressure discharging fills
Set, the bottom of the cylinder of rake type drier setting once discharge port, the section of a discharge port be it is trapezoidal, it is described
Negative pressure device for discharging includes negative pressure cylinder, guide sleeve, guide rod, valve body, handwheel, is flexible coupling, vent valve, the second vacuum pump, sealing
It covers, hold down assembly, the closed end end face of the upper end opening of the negative pressure cylinder, lower end closed, negative pressure cylinder is provided with secondary discharge port,
Bottom wall on the outside of the cylinder of rake type drier is close in the upper end end face of negative pressure cylinder, and the cylinder lumen of the rake type drier passes through primary
Discharge port is connected to negative pressure tube inner chamber, and the lower end of guide sleeve is fixedly connected with bottom wall on the inside of negative pressure cylinder, is equipped in guide sleeve center
Vertical pilot hole, guide rod passes through pilot hole, and is threadedly coupled with pilot hole, and the upper end of guide rod is equipped with valve body, guiding
The lower end of bar is equipped with handwheel, the center line of pilot hole, the center line of guide rod, valve body center line with discharge port
Center line is overlapped, and the shape of valve body and the type chamber of a discharge port match, and to drive guide rod rotation by rotation handwheel, is led
Set is oppositely oriented to bar to be moved upwardly or downwardly, and a discharge port is closed or opened with lid, is equipped between valve body and guide sleeve soft
Connection, this is flexible coupling is made of gas impermeable material, is equipped with blow vent on negative pressure cylinder ring wall top, deflation is equipped on blow vent
Valve is equipped with negative pressure mouth on negative pressure cylinder ring wall top, and negative pressure mouth connect with the entrance of the second vacuum pump, holds down assembly no less than two
A, described hold down assembly is evenly distributed with along negative pressure cylinder ring wall, and the sealing cover is covered on secondary discharge port, and will be close by holding down assembly
It covers relatively fixed with negative pressure cylinder.
Preferably, described to hold down assembly including fixed ring, movable earrings, puller bolt, fixed ring and the fixed company of negative pressure cylinder
It connects, movable earrings is at L-shaped, and movable earrings includes vertical section, horizontal segment, and vertical section and fixed ring are rotatablely connected, set on horizontal segment
Have a threaded hole being threadedly coupled with puller bolt, puller bolt dextrorotation or left-handed, by sealing cover and negative pressure cylinder it is relatively fixed or
It unclamps.
Preferably, the rectifying column lower right side is equipped with second liquid phase entrance, and the second liquid phase entrance of the rectifying column is logical
The pipeline crossed between pipeline and the first liquid phase entrance of rectifying column, the 4th pneumatic operated valve is connected to.
Preferably, the solid-state methanol sodium alkali process units using vacuum pump recycling methanol further includes controller, temperature
Sensor is spent, the temperature sensor is used to detect the real time temperature of alcoholic lye in the first preheater, and real time temperature is conveyed
To controller, temperature threshold is preset in the controller, real time temperature is more than or equal to temperature threshold, and controller controls the first gas
Dynamic valve is closed, and the second pneumatic operated valve is opened, and real time temperature is less than temperature threshold, and controller controls the first pneumatic operated valve and opens, the second gas
Dynamic valve is closed.
Preferably, the solid-state methanol sodium alkali process units using vacuum pump recycling methanol further includes humidity sensor
Device, the temperature sensor are used to detect the real-time water content of methanol solution in holding tank, are preset with water content in the controller
Threshold value, real-time water content are more than or equal to water content threshold value, and controller controls third pneumatic operated valve and closes, and the 4th pneumatic operated valve is opened, real
When water content be less than water content threshold value, controller control third pneumatic operated valve open, the 4th pneumatic operated valve close.
In the present invention, the power for tapping bar to the second stopper is vertical with fixed link, the shaft being connect with fixed link by
The moment loading for tapping bar, not will cause shaft bending, taps bar and strikes the second stopper, then provide vibration to fixed link,
Shaft can remove the material sticks in shaft.
In the present invention, the water conservancy diversion sieve plate being staggered from top to bottom in cooling tower body can efficiently use the liquid agglomerated
State methanol captures methanol gas, and then promotes methanol gas cohesion, has effectively recycled the first volatilized in rake type drier
Alcohol gas reduces the low problem of Methanol Recovery rate caused by the outlet for the methanol gas for having little time cohesion.
The cooling unit of the multistage being arranged in the present invention has three coolers, and overhead vapours passes through one in three coolers
It is a or it is several gradually cool down after to holding tank, one or several circulations being then back in three coolers by pipeline again are cold
But, it can guarantee cooling technique requirement, compared with single cooler, the cooling unit of multistage can carry out tower according to different produced quantities
The adjustment for the cooler number that top steam flows through, also the number of the cooler of adjustable reflux, it is cold to avoid single cooler
The drawbacks of insufficient or undercooling, it ensure that the reasonable consumption of energy consumption, meet synthetic tower and rectifying column operating condition is accurate
The requirement of regulation.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the solid-state methanol sodium alkali process units that methanol is recycled using vacuum pump.
Fig. 2 is the schematic diagram for showing rake type drier and negative pressure device for discharging internal structure.
Fig. 3 is the main view for tapping component.
Fig. 4 is the right view for tapping component.
Fig. 5 is the enlarged view to hold down assembly.
Fig. 6 is the partial view for showing cooling tower internal structure.
In figure: sodium methoxide synthesis unit 10, the first preheater 11, the first pneumatic operated valve 111, synthetic tower 12, rectifying column 13, more
The cooling unit 14 of grade, the second pneumatic operated valve 141, third pneumatic operated valve 142, the 4th pneumatic operated valve 143, the first cooler 144, second are cooling
Device 145, third cooler 146, holding tank 147, the second preheater 15, rake type drier 20,21, discharge ports 211 of cylinder,
Shaft 22 taps component 23, fixed link 231, taps bar 232, the first stopper 233, the second stopper 234, negative pressure discharging dress
Set that 30, negative pressure cylinder 31, secondary discharge port 311, guide sleeve 32, guide rod 33, valve body 34, handwheel 35, be flexible coupling 36, vent valve
37, sealing cover 38, the 39, fixed ring 391 that holds down assembly, movable earrings 392, puller bolt 393, methanol negative-pressure recovery device 40,
Cooling tower 41, tower body 411, linde sieve tray 412, the first vacuum pump 42.
Specific embodiment
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be apparent that, drawings in the following description are some embodiments of the invention, common for this field
For technical staff, without creative efforts, it is also possible to obtain other drawings based on these drawings.
Referring to Fig. 1 to Fig. 6, the embodiment of the invention provides a kind of solid-state methanol sodium alkalis using vacuum pump recycling methanol
Process units, including sodium methoxide synthesis unit 10, rake type drier 20, methanol negative-pressure recovery device 40, sodium methoxide synthesis unit
10 include the first preheater 11, synthetic tower 12, rectifying column 13, multistage cooling unit 14, the second preheater 15,12 left side of synthetic tower
Top has a feed(raw material)inlet, and alcoholic lye enters the shell side of the first preheater 11, passes through original after the heating of the first preheater 11
Expect that synthetic tower 12 is added in entrance, there is a gaseous phase outlet, 13 left side middle and lower part of rectifying column has a gas at the top of synthetic tower 12
Phase entrance, the gaseous phase outlet of synthetic tower 12 are connect with the gas phase entrance of rectifying column 13 with pipeline so that in synthetic tower 12 methanol and
The gaseous mixture of water is sent into rectifying column 13, and 13 tower top of rectifying column has a gaseous phase outlet, the gaseous phase outlet of rectifying column 13 with
The tube-side inlet of first preheater 11 connects, and the is installed on the pipeline between the gaseous phase outlet of rectifying column 13 and the first preheater 11
One pneumatic operated valve 111, the tube side inlet/outlet of the first preheater 11 are connect with the cooling main entrance on the right side of multistage cooling unit 14, essence
The gaseous phase outlet for evaporating tower 13 is connect with the cooling main entrance in the left side of multistage cooling unit 14, in the left side of multistage cooling unit 14
Cooling main entrance and rectifying column 13 gaseous phase outlet between pipeline on the second pneumatic operated valve 141, the second pneumatic operated valve 141 are installed
Between the first pneumatic operated valve 111 and multistage cooling unit 14, the cooling unit 14 of multistage has a methanol inlet, for multistage
Cooling unit 14 supplements anhydrous methanol, and the cooling unit 14 of multistage has a total coolant outlet, the cooling unit 14 of multistage it is total cold
But outlet is connect with the second preheater 15 by pipeline, is pacified on the pipeline between multistage cooling unit 14 and the second preheater 15
Equipped with third pneumatic operated valve 142,13 right upper portion of rectifying column is equipped with the first liquid phase entrance, total coolant outlet of the cooling unit 14 of multistage
It is connect by pipeline with the first liquid phase entrance of rectifying column 13, is pacified on the pipeline between multistage cooling unit 14 and rectifying column 13
Equipped with the 4th pneumatic operated valve 143, the 4th pneumatic operated valve 143 is between third pneumatic operated valve 142 and rectifying column 13, under 12 left side of synthetic tower
Portion has a methanol eddy mouth, and the outlet of the second preheater 15 is connect by pipeline with the methanol eddy mouth of synthetic tower 12, more
The cooling unit 14 of grade includes the first cooler 144, the second cooler 145, third cooler 146, holding tank 147, and first is cooling
Cooling main entrance of 144 left hand inlet port of device as the left side of multistage cooling unit 14,144 right hand inlet port of the first cooler and second
Cooling main entrance of 145 left hand inlet port of cooler as the right side of multistage cooling unit 14, the first cooler 144, second are cooling
The outlet of device 145, third cooler 146 is connect with the entrance of 147 side of holding tank, the outlet at the top of holding tank 147 and the
The entrance on two coolers, 145 right side, the entrance in 146 left side of third cooler are connected by pipeline, the entrance at 147 top of holding tank
As the methanol inlet of multistage cooling unit 14, total cold outlet of the outlet of 147 bottom of holding tank as multistage cooling unit 14,
The liquid-phase outlet of 12 bottom of synthetic tower is connect with the liquid phase entrance of rake type drier 20 by pipeline, and sodium methoxide and methanol is molten
Liquid is conveyed into rake type drier 20, and rake type drier 20 includes cylinder 21, shaft 22, taps component 23, the left and right two of shaft 22
End is rotatablely connected with the both ends end face of cylinder 21 respectively, is tapped component 23 and is included fixed link 231, taps bar 232, the first stopper
233, the second stopper 234, fixed link 231 are vertically arranged with respect to shaft 22, and one end of fixed link 231 is connecting pin, fixed link
231 connecting pin is fixedly connected with shaft 22, and the other end of fixed link 231 is free end, and the one end for tapping bar 232 is connection
The free end at end, the connecting pin and fixed link 231 that tap bar 232 is rotatablely connected, and the other end for tapping bar 232 is free end,
The first stopper 233, the second stopper 234 are provided in fixed link 231, the first block is set close to the free end of fixed link 231
It sets, the second block is arranged close to the connecting pin of fixed link 231, and the angle tapped between bar 232 and fixed link 231 is 180 °, the
One stopper 233 prevents to tap the rotation counterclockwise of bar 232, and tapping the angle between bar 232 and fixed link 231 is 0 °, the second resistance
Block 234 prevents percussion bar 232 from rotating clockwise, and methanol negative-pressure recovery device 40 includes cooling tower 41, the first vacuum pump 42, cold
But the gaseous phase outlet of the cylinder 21 of the gas phase entrance and rake type drier 20 of the bottom of tower 41 is connect, so that in rake type drier 20
The methanol gas volatilized enters cooling tower 41, and the entrance of the first vacuum pump 42 evacuates mouth with the top of cooling tower 41 and connect, with
Enter cooling tower 41 for methanol gas and draft is provided, cooling tower 41 includes staggered row from top to bottom in tower body 411 and tower body 411
The linde sieve tray 412 of column, tower body 411 are sandwich, and circulation has cooling medium, 412 water of linde sieve tray in the interlayer of tower body 411
Flat to be arranged in tower body 411, one end of linde sieve tray 412 is connect with 411 inner wall of tower body, the other end and tower of linde sieve tray 412
411 inner wall of body is not connected to, and linde sieve tray 412 is opposite to be bent upwards with the unconnected one end of tower body 411.
Alcoholic lye is added from 12 tower top of synthetic tower, is dehydrated required anhydrous methanol steam and is added from tower bottom, passes through alcoholic lye
With anhydrous methanol steam in synthetic tower 12 continuous flow upstream contact reacted, in synthetic tower 12 in liquid phase water molar fraction from
Tower top is gradually decreased to tower bottom, and the molar fraction of the water in gas phase is gradually decreased from tower bottom to tower top, reaches phase in tower top
Balance, the mixed vapour of first alcohol and water is discharged by tower top, and the water for being 2% 3% containing mass fraction in the mixed vapour, remaining is
Methanol is passed directly into rectifying column 13 and carries out rectifying separation, and obtained anhydrous methanol enters the recycling of synthetic tower 12, synthetic tower 12
The sodium methoxide of generation is discharged from tower bottom, as can be seen that 13 overhead vapours of rectifying column needs a large amount of condensed waters from the production technology
It is cooling, and in 13 reboiler of rectifying column, 12 reboiler of synthetic tower need to be added a large amount of steam and vaporize tower bottoms and first
Preheater 11, the second preheater 15 are also required to steam heating, therefore in entire technical process, required energy consumption is very big.
Alcoholic lye needs to be preheated to 70~100 DEG C, after anhydrous methanol needs to be preheated to 115~150 DEG C of production methanol steams
Into synthetic tower 12.
In the present embodiment, 13 overhead vapours a part of rectifying column enters the shell side of the first preheater 11, to heat alcoholic lye,
Alcoholic lye has been preheated while cooling 13 overhead vapours of rectifying column, has reduced energy consumption.
The methanol gas volatilized from rake type drier 20 is under the draft effect of the first vacuum pump 42, from 41 tower of cooling tower
Bottom enters, and tortuous upward along linde sieve tray 412, methanol gas is constantly condensed into liquid during rising, sieves in guiding
Plate 412 forms the liquid methanol of certain liquid height, and liquid methanol a part is under the sieve pore solid stream of linde sieve tray 412, and one
Along linde sieve tray 412, complications are flowed down from top to bottom for part, so that the liquid of the liquid methanol on supplement lower layer's linde sieve tray 412
Face, it is constantly cooling by 411 side wall of tower body during methanol gas rises in tower body 411, simultaneously because with by raindrop shape liquid
Body methanol comes into full contact with, and is constantly captured and forms liquid methanol.
" angle tapped between bar 232 and fixed link 231 is 0 ° " mentioned here refers to, the connecting pin of fixed link 231
It is overlapped with the free end for tapping bar 232.
Percussion bar 232 mentioned here is counterclockwise or rotates clockwise, and is the sight with the direction in paper in Fig. 3 for reader
Examine direction.
Originally, when the angle between percussion bar 232 and fixed link 231 is 0 °, at this point, the start angle of fixed link 231 is fixed
Position is 0 °, and as fixed link 231 continues to rotate clockwise, the angle tapped between bar 232 and fixed link 231 constantly increases, directly
180 ° are rotated to fixed link 231, the angle tapped between bar 232 and fixed link 231 is 180 °, due to the first stopper 233
Effect, fixed link 231 continue to rotate clockwise, and the angle tapped between bar 232 and fixed link 231 is always maintained at 180 °, until
Fixed link 231 rotates 360 ° of percussion bars 232 due to the effect of gravity, rotates relative to fixed bar 231, then hits the second stopper
Stop after 234.
In the present invention, the power for tapping bar 232 to the second stopper 234 is vertical with fixed link 231, connect with fixed link 231
Shaft 22 only by tap bar 232 moment loading, not will cause shaft 22 bending, tap bar 232 strike the second stopper
234, vibration is then provided to fixed link 231, shaft 22, can remove the material sticks in shaft 22.
In the present invention, the linde sieve tray 412 being staggered from top to bottom in 41 tower body 411 of cooling tower can be efficiently used
The liquid methanol of cohesion captures methanol gas, and then promotes methanol gas cohesion, has effectively recycled in rake type drier 20
The methanol gas volatilized reduces the low problem of Methanol Recovery rate caused by the outlet for the methanol gas for having little time cohesion.
There are three cooler, overhead vapours passes through in three coolers the cooling tool of unit 14 of the multistage being arranged in the present invention
It is one or several gradually cool down after to holding tank 147, be then back to again by pipeline one or several in three coolers
Circulating cooling can guarantee cooling technique requirement, and compared with single cooler, the cooling unit 14 of multistage can be according to different extraction
Amount carries out the adjustment for the cooler number that overhead vapours flows through, and also the number of the cooler of adjustable reflux, avoids single
The drawbacks of cooling deficiency of cooler or undercooling, it ensure that the reasonable consumption of energy consumption, meet synthetic tower 12 and rectifying column 13
The requirement of operating condition accuracy controlling.
Of course, it is possible to which more stages cooler is added as needed, the cooling capacity of each cooler can be different, for example,
By adjusting 144 to one cooling velocity appropriate of the first cooler, a small amount of steam in 13 overhead vapours of rectifying column is just solidifying
Gather and is separated by the first cooler 144 with methanol steam.
In the present embodiment, by reasonably adjusting multistage cooling unit 14, after 13 overhead vapours of rectifying column can be made cooling not
The second preheater 15 must be passed through again to preheat, just meet the technique requirement for entering synthetic tower 12, reduce adding for the second preheater 15
Thermal energy consumption.
Referring to Fig. 1 to Fig. 6, further, the solid-state methanol sodium alkali process units using vacuum pump recycling methanol further includes
Negative pressure device for discharging 30, bottom setting once discharge port 211 of the cylinder 21 of rake type drier 20, discharge port 211
Section be it is trapezoidal, negative pressure device for discharging 30 include negative pressure cylinder 31, guide sleeve 32, guide rod 33, valve body 34, handwheel 35, be flexible coupling
36, vent valve 37, the second vacuum pump, sealing cover 38, hold down assembly 39, the upper end opening of negative pressure cylinder 31, lower end closed, negative pressure cylinder
31 closed end end face is provided with secondary discharge port 311, and the cylinder 21 of rake type drier 20 is close in the upper end end face of negative pressure cylinder 31
21 inner cavity of cylinder of outside bottom wall, rake type drier 20 is connected to by a discharge port 211 with 31 inner cavity of negative pressure cylinder, guide sleeve 32
Lower end be fixedly connected with 31 inside bottom wall of negative pressure cylinder, be equipped with vertical pilot hole in the center of guide sleeve 32, guide rod 33 passes through
Pilot hole, and be threadedly coupled with pilot hole, the upper end of guide rod 33 is equipped with valve body 34, and the lower end of guide rod 33 is equipped with handwheel
35, the center line of pilot hole, the center line of guide rod 33, valve body 34 center line weight of the center line with a discharge port 211
It closing, the shape of valve body 34 and the type chamber of a discharge port 211 match, to drive guide rod 33 to rotate by rotation handwheel 35,
Guide rod 33 is oppositely oriented set 32 and is moved upwardly or downwardly, and a discharge port 211, valve body 34 and guide sleeve 32 are closed or opened with lid
Between be equipped with and be flexible coupling 36, this is flexible coupling 36 is made of gas impermeable material, be equipped with blow vent on 31 ring wall top of negative pressure cylinder,
Vent valve 37 is installed on blow vent, is equipped with negative pressure mouth, the entrance of negative pressure mouth and the second vacuum pump on 31 ring wall top of negative pressure cylinder
Connection holds down assembly 39 no less than two, holds down assembly 39 uniformly distributed along 31 ring wall of negative pressure cylinder, sealing cover 38 is covered on secondary discharging
On mouthfuls 311, and it is 39 sealing cover 38 and negative pressure cylinder 31 is relatively fixed by holding down assembly.
Existing 20 outlet valve of rake type drier realizes the tight fit of valve core and valve seat using worm and gear, and reaches close
Effect is sealed, the outlet valve of this structure seals discontinuity, to influence sealing effect, some material sticks are in spool
On tapered surface, sealing effect is also influenced.
In the present embodiment, after the material in rake type drier 20 is unsnatched, due to the effect of vacuum pump, in rake type drier 20
Air-flow between valve body 34 and a discharge port 211 gap flow out, with the distance between valve body 34 and a discharge port 211
Reduce, rake type drier 20 flow into negative pressure cylinder 31 air-flow velocity increase, adherency with 34 sealing surface of valve body on material by by
The big power of gradual change, adherency are moved with the material on 34 sealing surface of valve body, thus achieve the effect that clear up 34 sealing surface of valve body,
Improve the sealing effect of valve body 34.
In the present embodiment, when the sealing surface poor sealing of valve body 34, negative pressure cylinder 31 is used as secondary seal.
In the present embodiment, there are gaps between guide rod 33 and guide sleeve 32, so that 31 sealing effect of negative pressure cylinder is bad, often
The method of rule, is set with filler between guide rod 33 and guide sleeve 32, and the method for this sealing not only causes the structure of equipment multiple
Hydridization, and be association of activity and inertia and locate high failure rate, increase maintenance of equipment cost.
In the present embodiment, moved along a straight line up and down in guide sleeve 32 by guide rod 33, since guide rod 33 is in valve body 34
Center, the problem of so as to avoid 34 sealing surface discontinuity of valve body;It is flexible coupling using made of gas impermeable material
36 solve the sealing of negative pressure cylinders 31, and be flexible coupling 36 can unfold and fold with valve body 34, not only solve the problems, such as sealing, but also reduce
The failure rate of equipment is discharged using the method negative pressure of connection vacuum pump, and the material at 34 sealing surface of valve body is able to self-cleaning, improves
The leakproofness of valve body 34.
Referring to Fig. 1 to Fig. 6, further, holding down assembly 39 includes fixed ring 391, movable earrings 392, puller bolt 393,
Fixed ring 391 is fixedly connected with negative pressure cylinder 31, and movable earrings 392 is at L-shaped, and movable earrings 392 includes vertical section, horizontal segment, is erected
Straight section and fixed ring 391 are rotatablely connected, and horizontal segment is equipped with the threaded hole being threadedly coupled with puller bolt 393, puller bolt 393
Dextrorotation is left-handed, by sealing cover 38 and negative pressure cylinder 31 it is relatively fixed or unclamp.
Referring to Fig. 1, further, 13 lower right side of rectifying column is equipped with second liquid phase entrance, and the second liquid phase of rectifying column 13 enters
Mouth is connected to by the pipeline between pipeline and the first liquid phase entrance of rectifying column 13, the 4th pneumatic operated valve 143.
By second liquid phase inlet return after 13 overhead vapours of rectifying column is cooling, the excessively program-controlled of smart gold-plating can be advanced optimized
System guarantees anhydrous methanol moisture up to standard.
Referring to Fig. 1, further, the solid-state methanol sodium alkali process units using vacuum pump recycling methanol further includes control
Device, temperature sensor, temperature sensor are used to detect the real time temperature of alcoholic lye in the first preheater 11, and real time temperature is defeated
It send to controller, temperature threshold is preset in controller, real time temperature is more than or equal to temperature threshold, and controller control first is pneumatic
Valve 111 is closed, and the second pneumatic operated valve 141 is opened, and real time temperature is less than temperature threshold, and controller controls the first pneumatic operated valve 111 and opens,
Second pneumatic operated valve 141 is closed.
In the present embodiment, by automatic control means, it is able to maintain the first preheater 11 and technique is met to the preheating of alcoholic lye
It is required that, moreover it is possible to the waste heat for rationally utilizing 13 overhead vapours of rectifying column ensure that the reasonable consumption of energy consumption, also avoid manual operation
Trouble.
Referring to Fig. 1, further, the solid-state methanol sodium alkali process units using vacuum pump recycling methanol further includes that humidity passes
Sensor, temperature sensor are used to detect the real-time water content of methanol solution in holding tank 147, are preset with water content threshold in controller
Value, real-time water content are more than or equal to water content threshold value, and controller controls third pneumatic operated valve 142 and closes, and the 4th pneumatic operated valve 143 is beaten
It opens, real-time water content is less than water content threshold value, and controller controls third pneumatic operated valve 142 and opens, and the 4th pneumatic operated valve 143 is closed.
Rectifying column 13 is in a unstable state at booting initial stage, passes through back after 13 overhead vapours of rectifying column is cooling
It flows, gradually adjustment 13 to one stable state of rectifying column, in the present embodiment, is adjusted by automatic control means, avoided artificial
The trouble of operation.
Module or unit in the device of that embodiment of the invention can be combined, divided and deleted according to actual needs.
The above disclosure is only the preferred embodiments of the present invention, cannot limit the right model of the present invention with this certainly
It encloses, those skilled in the art can understand all or part of the processes for realizing the above embodiment, and wants according to right of the present invention
Made equivalent variations is sought, is still belonged to the scope covered by the invention.
Claims (6)
1. a kind of solid-state methanol sodium alkali process units using vacuum pump recycling methanol, it is characterised in that: closed including sodium methoxide
At unit, rake type drier, methanol negative-pressure recovery device, the sodium methoxide synthesis unit includes the first preheater, synthetic tower, essence
Evaporate tower, multistage cooling unit, the second preheater, the synthetic tower left upper portion has a feed(raw material)inlet, and alcoholic lye enters the
The shell side of one preheater is added synthetic tower by feed(raw material)inlet after the heating of the first preheater, has one at the top of the synthetic tower
A gaseous phase outlet, rectifying column left side middle and lower part have a gas phase entrance, the gaseous phase outlet of synthetic tower and the gas of rectifying column
Phase entrance is connected with pipeline, so that the gaseous mixture of first alcohol and water is sent into rectifying column, the top of the distillation column tool in synthetic tower
Have a gaseous phase outlet, the gaseous phase outlet of rectifying column is connect with the tube-side inlet of the first preheater, the gaseous phase outlet of rectifying column with
First pneumatic operated valve, the right side of the tube side inlet/outlet of the first preheater and multistage cooling unit are installed on the pipeline between the first preheater
The cooling main entrance of side connects, and the gaseous phase outlet of rectifying column is connect with the cooling main entrance in the left side of multistage cooling unit, more
The second pneumatic operated valve, institute are installed on pipeline between the cooling main entrance in left side and the gaseous phase outlet of rectifying column of the cooling unit of grade
It states the second pneumatic operated valve to be located between the first pneumatic operated valve and multistage cooling unit, there is the multistage cooling unit methanol to enter
Mouthful, to supplement anhydrous methanol for the cooling unit of multistage, the multistage cooling unit has a total coolant outlet, and the multistage is cold
But total coolant outlet of unit is connect with the second preheater by pipeline, the pipe between multistage cooling unit and the second preheater
Third pneumatic operated valve is installed, rectifying column right upper portion is equipped with the first liquid phase entrance, total coolant outlet of the cooling unit of multistage on line
It is connected by the first liquid phase entrance of pipeline and rectifying column, the is equipped on the pipeline between multistage cooling unit and rectifying column
Four pneumatic operated valves, for the 4th pneumatic operated valve between third pneumatic operated valve and rectifying column, the synthetic tower left lower has one
The outlet of methanol eddy mouth, the second preheater is connected by the methanol eddy mouth of pipeline and synthetic tower, the multistage cooling unit
Including the first cooler, the second cooler, third cooler, holding tank, the first cooler left hand inlet port is as multistage cold
But the cooling main entrance in the left side of unit, the first cooler right hand inlet port and the second cooler left hand inlet port are as multistage cold
But the cooling main entrance on the right side of unit, the first cooler, the second cooler, third cooler outlet with holding tank side
Entrance connection, the outlet at the top of holding tank passes through pipe with the entrance on the right side of the second cooler, the entrance on the left of third cooler
Line connects, and methanol inlet of the entrance at the top of holding tank as multistage cooling unit, the outlet of holding tank bottom is as multistage cold
But total cold outlet of unit, the liquid-phase outlet of the synthesis tower bottom and the liquid phase entrance of rake type drier are connected by pipeline,
Sodium methoxide and methanol solution are conveyed into rake type drier, the rake type drier includes cylinder, shaft, taps component, institute
It states the left and right ends of shaft to be rotatablely connected with the both ends end face of cylinder respectively, the percussions component includes fixed link, percussion bar, the
One stopper, the second stopper, fixed link are vertically arranged with respect to shaft, and one end of fixed link is connecting pin, the connection of fixed link
End is fixedly connected with shaft, and the other end of fixed link is free end, and the one end for tapping bar is connecting pin, tap bar connecting pin and
The free end of fixed link is rotatablely connected, and the other end for tapping bar is free end, and the first stopper, second are provided in fixed link
Stopper, the first block close to fixed link free end be arranged, the second block close to fixed link connecting pin be arranged, tap bar with
Angle between fixed link is 180 °, and the first stopper prevents percussion bar from rotating counterclockwise, taps the folder between bar and fixed link
Angle is 0 °, and the second stopper prevents percussion bar from rotating clockwise, and the methanol negative-pressure recovery device includes cooling tower, the first vacuum
Pump, the gaseous phase outlet connection of the cylinder of the gas phase entrance and rake type drier of the bottom of the cooling tower, so that rake type drier
The methanol gas inside volatilized enters cooling tower, and the entrance of the first vacuum pump and the top of cooling tower evacuate mouth connection, for first
Alcohol gas enters cooling tower and provides draft, and the cooling tower includes that staggered guiding is sieved from top to bottom in tower body and tower body
Plate, tower body are sandwich, and circulation has cooling medium in the interlayer of tower body, and the linde sieve tray is horizontally set in tower body, leads
It is connect to one end of sieve plate with tower body inner wall, the other end and the tower body inner wall of linde sieve tray are not connected to, and linde sieve tray is opposite and tower
The unconnected one end of body is bent upwards.
2. utilizing the solid-state methanol sodium alkali process units of vacuum pump recycling methanol as described in claim 1, it is characterised in that:
The solid-state methanol sodium alkali process units using vacuum pump recycling methanol further includes negative pressure device for discharging, and the rake is dry
Once discharge port, the section of a discharge port are trapezoidal, the negative pressure device for discharging packet for the bottom setting of the cylinder of machine
Negative pressure cylinder is included, guide sleeve, guide rod, valve body, handwheel, is flexible coupling, vent valve, the second vacuum pump, sealing cover, holds down assembly, institute
The upper end opening of negative pressure cylinder, lower end closed are stated, the closed end end face of negative pressure cylinder is provided with secondary discharge port, the upper end end of negative pressure cylinder
Bottom wall on the outside of the cylinder of rake type drier is close in face, and the cylinder lumen of the rake type drier passes through a discharge port and negative pressure cylinder
The lower end of inner cavity connection, guide sleeve is fixedly connected with bottom wall on the inside of negative pressure cylinder, is equipped with vertical pilot hole in guide sleeve center, is led
Pilot hole is passed through to bar, and is threadedly coupled with pilot hole, the upper end of guide rod is equipped with valve body, and the lower end of guide rod is equipped with hand
Wheel, the center line of pilot hole, the center line of guide rod, valve body center line be overlapped with the center line of a discharge port, valve body
Shape and the type chamber of a discharge port match, to drive guide rod rotation by rotation handwheel, guide rod is oppositely oriented set
Be moved upwardly or downwardly, with lid close or open a discharge port, be equipped with and be flexible coupling between valve body and guide sleeve, this be flexible coupling for
Gas impermeable material is made, and is equipped with blow vent on negative pressure cylinder ring wall top, vent valve is equipped on blow vent, in negative pressure cylinder ring wall
Top is equipped with negative pressure mouth, and negative pressure mouth connect with the entrance of the second vacuum pump, holds down assembly no less than two, the edge that holds down assembly
Negative pressure cylinder ring wall is uniformly distributed, and the sealing cover is covered on secondary discharge port, and by holding down assembly that sealing cover is opposite with negative pressure cylinder
It is fixed.
3. utilizing the solid-state methanol sodium alkali process units of vacuum pump recycling methanol as claimed in claim 2, it is characterised in that:
Described to hold down assembly including fixed ring, movable earrings, puller bolt, fixed ring is fixedly connected with negative pressure cylinder, and movable earrings is at L
Shape, movable earrings include vertical section, horizontal segment, and vertical section and fixed ring are rotatablely connected, and horizontal segment is equipped with and puller bolt spiral shell
Line connection threaded hole, puller bolt dextrorotation or left-handed, by sealing cover and negative pressure cylinder it is relatively fixed or unclamp.
4. utilizing the solid-state methanol sodium alkali process units of vacuum pump recycling methanol as described in claim 1, it is characterised in that:
The rectifying column lower right side is equipped with second liquid phase entrance, and the second liquid phase entrance of the rectifying column passes through pipeline and rectifying column
Pipeline connection between first liquid phase entrance, the 4th pneumatic operated valve.
5. utilizing the solid-state methanol sodium alkali process units of vacuum pump recycling methanol as described in claim 1, it is characterised in that:
The solid-state methanol sodium alkali process units using vacuum pump recycling methanol further includes controller, temperature sensor, the temperature
Degree sensor is used to detect the real time temperature of alcoholic lye in the first preheater, and real time temperature is delivered to controller, the control
Temperature threshold is preset in device processed, real time temperature is more than or equal to temperature threshold, and controller controls the first pneumatic operated valve and closes, the second gas
Dynamic valve is opened, and real time temperature is less than temperature threshold, and controller controls the first pneumatic operated valve and opens, and the second pneumatic operated valve is closed.
6. utilizing the solid-state methanol sodium alkali process units of vacuum pump recycling methanol as claimed in claim 5, it is characterised in that:
The solid-state methanol sodium alkali process units using vacuum pump recycling methanol further includes humidity sensor, the temperature sensor
For detecting the real-time water content of methanol solution in holding tank, water content threshold value is preset in the controller, real-time water content is big
In being equal to water content threshold value, controller controls third pneumatic operated valve and closes, and the 4th pneumatic operated valve is opened, and real-time water content is less than water content
Threshold value, controller control third pneumatic operated valve and open, and the 4th pneumatic operated valve is closed.
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GB625453A (en) * | 1947-08-20 | 1949-06-28 | Robert Arthur Rosser | Improvements in or relating to the production of sodium methoxide |
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USH1697H (en) * | 1996-03-20 | 1997-11-04 | E. I. Du Pont De Nemours And Company | Continuous process for sodium methylate |
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CN105884578A (en) * | 2016-04-21 | 2016-08-24 | 赖明空 | Method for high temperature and high pressure production of sodium methoxide and device thereof |
CN208406975U (en) * | 2018-05-23 | 2019-01-22 | 阿拉善盟兰峰化工有限责任公司 | A kind of sodium methoxide production system |
CN209741030U (en) * | 2019-03-28 | 2019-12-06 | 宁夏恒汇鲁丰科技有限公司 | Solid sodium methoxide alkaline production device for recovering methanol by vacuum pump |
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GB625453A (en) * | 1947-08-20 | 1949-06-28 | Robert Arthur Rosser | Improvements in or relating to the production of sodium methoxide |
GB698282A (en) * | 1951-03-20 | 1953-10-14 | Frank Talbot | Improvements in or relating to the production of sodium methoxide |
USH1697H (en) * | 1996-03-20 | 1997-11-04 | E. I. Du Pont De Nemours And Company | Continuous process for sodium methylate |
CN104713335A (en) * | 2014-05-14 | 2015-06-17 | 安徽黑钰颜料新材料有限公司 | Anti-blocking type vacuum harrow dryer |
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