CN110229090A - A kind of preparation system of octylpyrrolidone - Google Patents
A kind of preparation system of octylpyrrolidone Download PDFInfo
- Publication number
- CN110229090A CN110229090A CN201910594305.2A CN201910594305A CN110229090A CN 110229090 A CN110229090 A CN 110229090A CN 201910594305 A CN201910594305 A CN 201910594305A CN 110229090 A CN110229090 A CN 110229090A
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- China
- Prior art keywords
- setting
- hole
- reboiler
- turntable
- cleaning ball
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 75
- 238000004140 cleaning Methods 0.000 claims abstract description 64
- 239000000047 product Substances 0.000 claims abstract description 34
- 239000010865 sewage Substances 0.000 claims abstract description 28
- 230000003068 static effect Effects 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 24
- 239000012043 crude product Substances 0.000 claims abstract description 19
- 230000000712 assembly Effects 0.000 claims abstract description 12
- 238000000429 assembly Methods 0.000 claims abstract description 12
- 238000003860 storage Methods 0.000 claims abstract description 11
- 230000001360 synchronised effect Effects 0.000 claims abstract description 5
- 238000000746 purification Methods 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 3
- 239000006227 byproduct Substances 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 description 16
- 238000010586 diagram Methods 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- YEJRWHAVMIAJKC-UHFFFAOYSA-N gamma-butyrolactone Natural products O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 229930188620 butyrolactone Natural products 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- WPPOGHDFAVQKLN-UHFFFAOYSA-N N-Octyl-2-pyrrolidone Chemical compound CCCCCCCCN1CCCC1=O WPPOGHDFAVQKLN-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000004080 punching Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NJPQAIBZIHNJDO-UHFFFAOYSA-N 1-dodecylpyrrolidin-2-one Chemical compound CCCCCCCCCCCCN1CCCC1=O NJPQAIBZIHNJDO-UHFFFAOYSA-N 0.000 description 1
- JVCRHTKQAPRUKG-UHFFFAOYSA-N 1-dodecylpyrrolidine Chemical group CCCCCCCCCCCCN1CCCC1 JVCRHTKQAPRUKG-UHFFFAOYSA-N 0.000 description 1
- 208000019901 Anxiety disease Diseases 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000036506 anxiety Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000002837 defoliant Substances 0.000 description 1
- 210000004262 dental pulp cavity Anatomy 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000009972 noncorrosive effect Effects 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
- B01D3/322—Reboiler specifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D207/18—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member
- C07D207/22—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D207/24—Oxygen or sulfur atoms
- C07D207/26—2-Pyrrolidones
- C07D207/263—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms
- C07D207/267—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to the ring nitrogen atom
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Cleaning In General (AREA)
Abstract
The present invention relates to a kind of preparation systems of octylpyrrolidone, including the first metering pump, the second metering pump, static mixer, high-temperature pipe reactor, crude product temporary storage tank, circulating pump a, light component rectifying column, reboiler a, circulating pump b, product rectifying column, reboiler b, cooler a, product slot；The reboiler a, reboiler b include body assembly, the water inlet component being arranged on the body assembly, the cleaning assemblies being arranged in the body assembly and the discharge component that setting and synchronous rotation are connected to the water inlet component；The discharge component includes sewage unit and drainage cell, and the sewage unit and drainage cell are connected to setting with the water inlet component alternative expression respectively, completes the mask work of water purification and dirty material；The technical issues of present invention solves in reboiler the step, can generate scale, influence product purity quality.
Description
Technical field
The present invention relates to a kind of octylpyrrolidone preparation technical field more particularly to a kind of preparations of octylpyrrolidone
System.
Background technique
N-octylpyrrolidone is a kind of chemical substance, and molecular formula is C12H23NO, is the colourless liquid for having amine taste to yellow
Body compound, No. CAS is 2687-94-7, and molecular weight 197.32 is widely used as insecticide, cotton defoliant, concentrated cleaner,
Chemically react solvent, pharmaceutical synthesis medium, the stripper for coating layer in electronics industry.As surfactant, can with anion or
Nonionic surfactant is used in compounding, and is reduced surface tension, is provided properties of product.
Currently, octylpyrrolidone production technology is mostly the batch production process that pressurizes, the relative productivity of this production method
Smaller, equipment land occupation is big, and is difficult to realize automation control, and capital investment is big, high production cost, and machinery stirs at high temperature
It mixes machine envelope and is prone to wear damage, cause device maintenance cost high.
The patent document of Patent No. CN2006100520938N discloses a kind of production of N-dodecylpyrrolidone
Mixture is sent into after high-speed stirred by method method includes the following steps: lauryl amine, r- butyrolactone are put into batching kettle by (1)
One leading portion 40%-60% length thereof is reacted in the pipeline reactor of static mixer；It (2) will be anti-in duct type
It answers the mixture after reacting in device to be sent into continuous still tower and carries out decompression separation, it is N- dodecyl pyrrolidine that tower bottom, which distillates product,
Ketone.
But in actual use, inventor's discovery can generate scale in reboiler the step, scale with
Also the problem of will affect product purity while clear water mask work is cumbersome.
Summary of the invention
The purpose of the present invention is in view of the deficiencies of the prior art, wash away cleaning assemblies by the way that hydraulic pressure is arranged, guide it
Steadily moved in heat exchanger tube, rapidly and efficiently removing to scale realized in moving process, thus solve reboiler this
In step, scale can be generated, the technical issues of scale and clear water mask work also will affect product purity while cumbersome.
Against the above technical problems, as follows using technical solution: a kind of preparation system of octylpyrrolidone, feature exist
In: including the first metering pump, the second metering pump, static mixer, high-temperature pipe reactor, crude product temporary storage tank, circulating pump a, light
Component rectifying column, reboiler a, circulating pump b, product rectifying column, reboiler b, cooler a, product slot, cooler b, described first
Metering pump, the second metering pump are connected to setting, the static mixer and high-temperature pipe reactor with static mixer by threeway
It is connected and is arranged by pipeline, static mixer is connected with the feed inlet of crude product temporary storage tank, and light component rectifying column and crude product are temporary
It is connected between tank by circulating pump a, light component rectifying column connect setting with the feed inlet of cooler b, and circulating pump a passes through product essence
It evaporates tower and connect setting with circulating pump b, cooler a connect setting, reboiler a discharge port and light component rectifying column with product rectifying column
Discharge port connection and its feed inlet connect setting with the discharge port of circulating pump a, the discharge port of reboiler b and, product rectifying column
Discharge port connection and its feed inlet with the discharge port of circulating pump b connect setting；
The reboiler a, reboiler b include body assembly, the water inlet component being arranged on the body assembly, setting
Cleaning assemblies in the body assembly and the discharge component that setting and synchronous rotation are connected to the water inlet component；
The discharge component includes sewage unit and drainage cell, the sewage unit and drainage cell respectively with it is described into
The connection setting of water assembly alternative expression, completes the mask work of water purification and dirty material.
Preferably, the body assembly includes:
Rack；And
Body, the body include shell, flange, discharge port, feed inlet, tube sheet and heat exchanger tube.
Preferably, the water inlet component includes:
Water supplying unit, the water supplying unit include the water pump water tank all-in-one machine being mounted on the rack and with the water pump
The water pipe a of water tank all-in-one machine connection setting；And
Control unit, described control unit include the turntable that the flange side is arranged in and is bonded setting with the flange
With the turntable side is set and is bonded the fixing seat of setting with the turntable, the turntable is rotatably arranged on the rack
On, the fixing seat is fixedly mounted in the rack；
The flange, turntable and fixing seat are coaxially disposed and turntable is centrally located.
Preferably, offer through-hole a in the flange and fixing seat and be symmetrical arranged relatively with the turntable, it is described
The through-hole a of fixing seat is connected to setting with the water pipe a；
Be also provided on the flange and fixing seat through-hole b and it is opposite be symmetrical arranged with the turntable, the through-hole a and
Through-hole b is diametrically linearly arranged, and the through-hole b of the fixing seat is connected to setting with the discharge component；
The turntable offers through-hole c and through-hole d, and the through-hole c and through-hole d are interrupted with the through-hole a and through-hole b respectively
Formula connection setting；
The through-hole a, through-hole b, through-hole c are identical with through-hole d caliber size, are A1.
Preferably, the cleaning assemblies includes:
Cleaning ball, the cleaning ball is cylindrical body and is flexible material structure setting, and the cleaning ball both ends are hollow set
Set and intermediate position be solid setting, the cleaning ball under the impulse force of water successively flow path through-hole c, through-hole a, heat exchanger tube, through-hole b and
Through-hole d；
Salient point, the salient point is evenly distributed on cleaning ball side and through setting, in the cleaning ball short transverse
The alternate setting of the salient point dislocation of neighbouring two, and described in adjacent along cleaning ball high perpendicular direction two
The distance between salient point is L1, and the width of salient point is L2, L1=L2, and the salient point is located at cleaning ball interior section bottom and opens
Equipped with chamfering；And
Shore unit, it is described to shore unit and be symmetricly set on the cleaning ball along the middle line in the cleaning ball length
Upper bottom surface comprising the mobile tapered pole for being arranged in inside the cleaning ball and match setting with the salient point bottom surface, symmetrically
The connecting plate and one end that tapered pole bottom surface is arranged connect setting with the connecting plate and the other end is connect with the cleaning ball bottom
The spring of setting.
Preferably, the discharge component further includes driving unit, the driving unit includes:
Motor, the motor are mounted on the rack；
Drive shaft, described drive shaft one end is connect with the output end of the motor and the other end and the turntable are fixed and connected
It connecing, wears groove of the drive shaft in the fixing axle, the bore of the wears groove is D1, and the bore of the drive shaft is D2,
D1 > D2；
Gear a, the gear a is coaxial with the drive shaft and is fixedly connected；
Gear b, the gear b are engaged with the gear a；
Rotation axis, the rotation axis fixed setting rotate setting on the fixing seat and with the gear b.
Preferably, the sewage unit and drainage cell are water pipe b, it is arranged in the rotation axis and symmetrically sets
It sets in the two sides of the rotation axis, the drainage cell is embedded in the sewage unit towards motor one end towards motor one end,
The outer annular diameter of water pipe b is A2, annular diameters A3, A2 > A1 > A3.
Preferably, the high-temperature tubular reactor is 230-300 DEG C of reaction temperature.
Preferably, the external dimensions of the high-temperature tubular reactor is DN800*4000.
As preferably, the static mixer uses jacket type structure again.
Beneficial effects of the present invention:
(1) cleaning assemblies is washed away by the way that hydraulic pressure is arranged in the present invention, guides it steadily to move in heat exchanger tube, moving process
Middle rapidly and efficiently removing of the realization to scale, and the work such as need not be shut down, be dismantled to reboiler, greatly reduce manpower object
The investment of power, improves production efficiency；Additionally by sewage unit and drainage cell alternative expression and water group in setting discharge component
Being automatically separated for the connection of part, realization scale and clear water, improves the automation of whole device, reduces labour productive forces；
(2) tapered pole and salient point angle are utilized when hydraulic pressure acts on tapered pole by setting cleaning assemblies in the present invention
Cooperation, makes it under hydraulic pressure, and salient point struts outward, comes into full contact with the inner wall of heat exchanger tube, even and if then guaranteeing be used for a long time
Afterwards, the come into full contact with tensile force that simultaneously using the two is bonded of the cleaning ball with heat exchanger tube, raising cleaning ball exchange still be can guarantee
Scale on heat pipe inner wall sufficiently cleans, while being conducive to preferably convey scale, improves working efficiency；
(3) sewage unit and drainage cell are cooperated by setting driving unit in the present invention, realizes driving unit on the one hand
Turntable rotation is driven, realizes that cleaning ball is reset to initialization position；In addition the rotation of sewage unit and drainage cell is driven, it is real
The alternating switching that existing blowdown, draining two work；By two work by a power drive, front and back working relation is close, is not easy
Error is advantageously implemented being completely separated for scale and clear water；Extra power is saved simultaneously, reduces production cost；
(4) continuous feed and output can be realized, the kettle used more in the prior art by pipeline reactor in the present invention
Formula reactor, plant capacity are obviously improved, and have equipment to be changed into static equipment, and service life of equipment is long, production effect
Rate is high, while using double tower continuous rectification, improves unit production capacity, and product quality is more stable.
In conclusion the equipment has the advantages that device lifetime is long, production cost is low, it is particularly suitable for octylpyrrolidone
Preparation technical field.
Detailed description of the invention
It, below will be to required use in embodiment description for the clearer technical solution for illustrating the embodiment of the present invention
Attached drawing be briefly described, it should be apparent that, drawings discussed below is only some embodiments of the present invention, for ability
For the those of ordinary skill in domain, without creative efforts, it is attached to can also be obtained according to these attached drawings other
Figure.
Fig. 1 is the flow diagram of the preparation system of octylpyrrolidone.
Fig. 2 is the structural schematic diagram of reboiler a.
Fig. 3 is the structural schematic diagram of control unit.
Fig. 4 is the structural schematic diagram of cleaning assemblies.
Fig. 5 is the structural schematic diagram of salient point distribution.
Fig. 6 is the alternation schematic diagram of sewage unit and drainage cell.
Fig. 7 is the schematic cross-sectional view of driving unit.
Fig. 8 is partial enlargement diagram of the Fig. 7 at A.
Fig. 9 is partial enlargement diagram of the Fig. 7 at B.
Figure 10 is partial enlargement diagram of the Fig. 7 at C.
Specific embodiment
Technical solution in the embodiment of the present invention is clearly and completely illustrated with reference to the accompanying drawing.
Embodiment one
As shown in Figure 1 and Figure 2, a kind of preparation system of octylpyrrolidone, including the first metering pump 101, the second metering pump
102, static mixer 103, high-temperature pipe reactor 104, crude product temporary storage tank 105, circulating pump a106, light component rectifying column 107,
Reboiler a108, circulating pump b109, product rectifying column 110, reboiler b111, cooler a112, product slot 113, cooler
B114, first metering pump 101, the second metering pump 102 are connected to setting, the static state with static mixer 103 by threeway
Mixer 103 and high-temperature pipe reactor 104 connect setting by pipeline, static mixer 103 and crude product temporary storage tank 105 into
Material mouth is connected, and is connected between light component rectifying column 107 and crude product temporary storage tank 105 by circulating pump a106, light component rectifying column
107 connect setting with the feed inlet of cooler b114, and circulating pump a106 is connect with circulating pump b109 by product rectifying column 110 and set
It sets, cooler a112 connect setting, the discharging of reboiler a108 discharge port and light component rectifying column 107 with product rectifying column 110
Mouthful connection and its feed inlet connect setting with the discharge port of circulating pump a106, the discharge port of reboiler b111 and, product rectifying column
110 discharge port connection and its feed inlet with the discharge port of circulating pump b109 connect setting；
The water inlet that the reboiler a108, reboiler b111 include body assembly 1, is arranged on the body assembly 1
Component 2, the cleaning assemblies 3 being arranged in the body assembly 1 and be connected to the water inlet component 2 setting and synchronous rotation
Discharge component 4；
The discharge component 4 includes sewage unit 47 and drainage cell 48, and the sewage unit 47 and drainage cell 48 divide
Setting is not connected to 2 alternative expression of water inlet component, completes the mask work of water purification and dirty material.
More traditional preparation system, the invention are washed away clearly in reboiler a108, reboiler b111 by the way that hydraulic pressure is arranged
Clean component 3, guides it steadily to move in heat exchanger tube, the rapidly and efficiently removing to scale is realized in moving process, and need not be right
Reboiler such as is shut down, is dismantled at the work, is greatly reduced the investment of manpower and material resources, is improved production efficiency；Additionally by setting
Set discharge component 4 in sewage unit 47 and drainage cell 48 alternative expression and water assembly 2 connection, realization scale and clear water it is automatic
Separation improves the automation of whole device, reduces labour productive forces.
In the present embodiment, preparation flow successively passes through the first metering pump 101, the second metering pump 102, static mixer
103, high-temperature tubular reactor 104, crude product temporary storage tank 105, circulating pump a106, light component rectifying column 107, reboiler a108, follow
Ring pumps b109, product rectifying column 110, reboiler b111, cooler a112, product slot 113, the feed inlet connection of the first metering pump
Butyrolactone head tank, the feed inlet of the second metering pump connect n-octyl amine head tank, and two metering pump discharges are by threeway by quiet
After state mixer is sufficiently mixed, high-temperature tubular reactor is removed, flows into static mixer by the material of high-temperature tubular reactor
Collet removes preheating material mixture, then arrives crude product temporary tank, removes light component rectifying column by pump, removes in light component rectifying column
After light component water, it is continuously pumped into product rectifying column, continuous output product；Whole flow process capital investment and equipment land occupation are smaller, behaviour
Make simple, realize continuous production, and can DCS automation control, energy saving and cost of labor, reduce production cost；Reaction
Time is short, and stable yield can reach 93% or more；Pressurization closed reaction, safety coefficient are high.Non-corrosive or thorn in production process
Swash property substance to generate, because without corroding production equipment and generation environment pollution.
Specifically, the discharge port of the discharge port of the first metering pump and the second metering pump is connected to a root canal by threeway
Road, another pipe end of the tee tube connect check valve, the check valve by pipeline connect the static mixer into
Material mouth, the discharge port of the static mixer connect the feed inlet of the high-temperature tubular reactor, the high temperature pipe by pipeline
The discharge port of formula reactor connects the collet feed inlet of the static mixer by pipeline, and the collet of the static mixer goes out
Material mouth connects crude product temporary tank, and the discharge port of the crude product temporary tank is continuously pumped into light component rectifying column, light component warp by pump
Condensation removal system is crossed, semi-finished product are continuously pumped into product rectifying column, and product condenses continuous output by separation.Ball is equipped in system
Valve, sampling valve, blow valve and tube side thermometer are equipped with counterbalance valve and tube side pressure gauge etc..
In addition, the crude product is continuously separated by double tower, and continuous output, convenient for operating, and it is energy saving, improve tower
Utilization rate；Meanwhile by pipeline reactor, continuous feed and output can be realized, the still reaction used more in the prior art
Device, plant capacity are obviously improved, and have equipment to be changed into static equipment, and service life of equipment is long, high production efficiency, together
Shi Caiyong double tower continuous rectification improves unit production capacity, and product quality is more stable.
Further, as shown in Fig. 2, the body assembly 1 includes:
Rack 11；And
Body 12, the body 12 include shell 15, flange 16, discharge port 17, feed inlet 18, tube sheet 19 and heat exchanger tube
20。
In the present embodiment, body 12 can realize the heating of material, vaporescence, and wherein material is from 15 bottom of shell
Feed inlet 18, while gaseous phase materials return in rectifying column from discharge port 17
Further, as shown in Figure 2 and Figure 3, the water inlet component 2 includes:
Water supplying unit 21, the water supplying unit 21 include the water pump water tank all-in-one machine 22 that is mounted in the rack 11 and with
The water pipe a23 of the connection of water pump water tank all-in-one machine 22 setting；And
Control unit 24, described control unit 24 include that setting is set in 16 side of flange and being bonded with the flange 16
The turntable 25 set and 25 side of turntable is set and is bonded the fixing seat 26 of setting, 25 turns of the turntable with the turntable 25
Dynamic to be arranged in the rack 11, the fixing seat 26 is fixedly mounted in the rack 11；
The flange 16, turntable 25 and fixing seat 26 are coaxially disposed and turntable 25 is centrally located.
In the present embodiment, by the way that turntable 25 is arranged, the work that the embedded cleaning ball 31 of turntable 25 automatically resets is realized；Together
When, during turntable 25 rotates, the effect of sealing is played to body 12.
Further, as shown in figure 3, offered in the flange 16 and fixing seat 26 through-hole a27 and it is opposite with described turn
Disk 25 is symmetrical arranged, and the through-hole a27 of the fixing seat 26 is connected to setting with the water pipe a23；
Through-hole b28 and opposite arranged symmetrically with the turntable 25, institute are also provided on the flange 16 and fixing seat 26
It states through-hole a27 and through-hole b28 is diametrically linearly arranged, the through-hole b28 of the fixing seat 26 is connected to the discharge component 4
Setting；
The turntable 25 offers through-hole c29 and through-hole d30, the through-hole c29 and through-hole d30 respectively with the through-hole
A27 is connected to setting with through-hole b28 discontinuous；
The through-hole a27, through-hole b28, through-hole c29 are identical with through-hole d30 caliber size, are A1.
In the present embodiment, cleaning ball successively flow path through-hole a27, through-hole c29, through-hole a27, heat exchange under the washing away of hydraulic pressure
Pipe 20, through-hole b28, through-hole d30, through-hole b28 are connected using its mouthful of mouth, realize the normal streaming of water.
Further, as shown in Figure 4, Figure 5, the cleaning assemblies 3 includes:
Cleaning ball 31, the cleaning ball 31 is cylindrical body and is flexible material structure setting, and 31 both ends of cleaning ball are
Hollow setting and centre position are solid setting；
Salient point 32, the salient point 32 is evenly distributed on 31 side of cleaning ball and through setting, high along the cleaning ball 31
Neighbouring two salient points 32 misplace alternate setting, and the phase along the 31 high perpendicular direction of cleaning ball on degree direction
The distance between two adjacent described salient points 32 are L1, and the width of salient point 32 is L2, L1=L2, and the salient point 32 is located at described clear
Section bottom inside clean ball 31 offers chamfering；And
Shore unit 33, it is described shore unit 33 be symmetricly set on along the middle line in 31 length of cleaning ball it is described clear
The upper bottom surface of clean ball 31 comprising mobile that 31 inside of cleaning ball is set and matches setting with 32 bottom surface of salient point
Tapered pole 34, be symmetrical arranged 34 bottom surface of tapered pole connecting plate 35 and one end connect with the connecting plate 35 be arranged and the other end and
The spring 36 of 31 bottom of the cleaning ball connection setting.
In the present embodiment, by the way that cleaning assemblies 3 is arranged, when hydraulic pressure acts on tapered pole 34, using tapered pole 34 with
The cooperation of 32 angle of salient point, makes it under hydraulic pressure, and salient point struts outward, comes into full contact with the inner wall of heat exchanger tube 20, and then guarantee is
Just after long-term use, still can guarantee cleaning ball 31 and heat exchanger tube 20 come into full contact with simultaneously using both the anxiety that is bonded
Power improves the scale that cleaning ball 31 is exchanged on 20 inner wall of heat pipe and sufficiently cleans, improves working efficiency；
It is worth noting that 34 automatically reseting in the case where not washed away by hydraulic pressure of tapered pole is realized by the way that spring 36 is arranged,
Since cleaning ball 31 is flexible material structure setting, and then when cleaning ball 31 moves in heat exchanger tube 20, work will not be interfered
Make；
It additionally needs, it is emphasized that the setting of salient point is to accomplish to realize cleaning ball 31 and heat exchanger tube 20 using least material
The adequacy of inner wall contacts, and improves fully flushing for exchange 20 inner wall scale of heat pipe.
Further, as shown in Figure 6, Figure 7, the discharge component 4 further includes driving unit 40, and the driving unit 40 wraps
It includes:
Motor 41, the motor 41 are mounted in the rack 11；
Drive shaft 42, described 42 one end of drive shaft is connect with the output end of the motor 41 and the other end and the turntable 25
It is fixedly connected, wears groove 43 of the drive shaft 42 in the fixing axle, the bore of the wears groove 43 is D1, the drive shaft
42 bore is D2, D1 > D2；
Gear a44, the gear a44 is coaxial with the drive shaft 42 and is fixedly connected；
Gear b45, the gear b45 are engaged with the gear a44；And
Rotation axis 46, the rotation axis 46, which is fixed in the fixing seat 26 and rotates with the gear b45, to be arranged.
In the present embodiment, sewage unit 47 and drainage cell 48 are cooperated by setting driving unit 40, realizes that driving is single
On the one hand driving turntable 25 rotates member 40, realizes that cleaning ball is reset to initialization position；In addition sewage unit 47 and row are driven
The alternating switching of blowdown, two work of draining is realized in the rotation of water unit 48；By two work by a power drive, realize
The dirt of 31 front of cleaning ball first passes through the output of sewage unit 47, the movement that the subsequent clear water of cleaning ball 31 is resetted in cleaning ball 31
In, the switching of synchronous drive sewage unit 47 and drainage cell 48, clear water is flowed out from drainage cell 48, and front and back working relation is tight
It is close, it is not easy to make mistakes, it is advantageously implemented being completely separated for scale and clear water；Extra power is saved simultaneously, reduces production cost.
Specifically, while the proportion of gear tooth, while so that motor 41 drives turntable to turn 180 °, gear b45 turns
180°。
Further, 104 reaction temperature of high-temperature tubular reactor is 230-300 DEG C.
Further, the external dimensions of the high-temperature tubular reactor 104 is DN800*4000.
It is noted that the collet of high-temperature tubular reactor walks conduction oil.
Further, the static mixer 103 uses jacket type structure.
In the present embodiment, jacketed formula is used by setting static mixer 103, using the heat of reaction mass to original
Material is preheated.
Embodiment two
As shown in Figure 9, Figure 10, wherein with component identical or corresponding in embodiment one using corresponding with embodiment one attached
Icon note hereafter only describes the distinctive points with embodiment one for simplicity.The difference of the embodiment two and embodiment one
It is:
Further, as shown in Figure 9, Figure 10, the sewage unit 47 and drainage cell 48 are water pipe b, are arranged in institute
State in rotation axis 46 and be symmetricly set on the two sides of the rotation axis 46, the drainage cell 48 is towards in described 41 one end of motor
Embedded in the sewage unit 47 towards described 41 one end of motor, the outer annular diameter of water pipe b is A2, annular diameters A3, A2 >
A1 > A3.
In the present embodiment, pass through setting sewage unit 47 and the embedded setting of the output par, c of drainage cell 48, purpose
It is, avoids sewage unit 47 and drainage cell 48 in the course of rotation, the phenomenon that the winding that knot occurs, interfering work just
Often operation, it is worth noting that, it is conventional technical means in the art that drainage cell 48, which embeds sewage unit 47, only need to be by blowdown list
47 punching of member allows drainage cell 48 to pierce into, and 47 bore of sewage unit is big, and punching junction can be connected by sealing means such as glue.
It is worth noting that the purpose of A2 > A1 > A3 is, clear water or scale is on the one hand enabled to fully flow into water
In pipe b；On the other hand, position-limiting action is played to cleaning ball using the wall thickness of water pipe b.
The course of work:
Raw material butyrolactone is by metering pump a in terms of the speed of 300kg/h is pumped into three-way pipeline and raw material n-octyl amine passes through
After amount pump b is pumped into mixing with 450kg/h, to the static mixer of jacketed, by high temperature pipe after being sufficiently mixed and preheating
Formula reactor reaction, high-temperature reactor are reacted by heat-conducting oil heating to temperature at 280 degree, and material passes through high-temperature tubular reactor
Output crude product afterwards, arrives preheater collet preheating material mixture, at the same crude product it is cooled under come crude product temporary storage tank, sampling analysis
Content 94.3%.Crude product temporary storage tank material is continuously pumped into light component rectifying column by pump, and lights column is heated by reboiler a,
Light component water continuously is separated, heavy constituent i.e. half product removes product rectifying column, and product rectifying column is heated through reboiler b and Gao Zhen
Sky continuously separates product, product content 99.2%, a small amount of high boiling removal system in product rectifying column.
The specific works material of reboiler a enters inside shell 15 from feed inlet 18, and material is contacted with heat exchanger tube 20 and gone forward side by side
Row heat transmitting, while water pump water tank all-in-one machine 22 starts, hot water flows into heat exchanger tube 20 by water pipe a23, while by cleaning ball 31
It pushes, cleaning ball 31 struts, while will be on 20 inner wall of heat exchanger tube in the presence of hydraulic pressure during heat exchanger tube 20 is mobile
Scale washes away, and scale is located at 31 front of cleaning ball, and clear water is located at 31 rear of cleaning ball, and scale is discharged from sewage unit 47, opens
Dynamic motor, motor 41 rotate 180 °, and cleaning ball 3 is reset to initial position, while gear b45 rotates 180 °, drainage cell 48 with
Through-hole b28 connection setting, clear water discharge；During clear water flows in heat exchanger tube 20, the water of high temperature adds the material of low temperature
The material of heat, vaporization, gas phase enters subsequent processing by discharge port 17:
The specific works of reboiler b are identical as the work of reboiler a, and not in this to go forth.
In the description of the present invention, it is to be understood that, the orientation or positional relationship of the instructions such as term " front and back ", " left and right "
To be based on the orientation or positional relationship shown in the drawings, be merely for convenience of description of the present invention and simplification of the description, rather than indicate or
It implies that signified equipment or component must have a particular orientation, is constructed and operated in a specific orientation, therefore should not be understood as
Limitation to invention.
Certainly in the technical scheme, those skilled in the art is it should be understood that term " one " is interpreted as " at least
One " or " one or more ", i.e., in one embodiment, the quantity of an element can be one, and in other implementation
In example, the quantity of the element can be it is multiple, term " one " should not be understood as the limitation to quantity.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any changes or substitutions that can be easily thought of under technical clarification of the invention by anyone skilled in the art, should all contain
Lid is within protection scope of the present invention.Therefore, the scope of protection of the invention shall be subject to the scope of protection specified in the patent claim.
Claims (10)
1. a kind of preparation system of octylpyrrolidone, it is characterised in that: including the first metering pump (101), the second metering pump
(102), static mixer (103), high-temperature pipe reactor (104), crude product temporary storage tank (105), circulating pump a (106), light component
Rectifying column (107), reboiler a (108), circulating pump b (109), product rectifying column (110), reboiler b (111), cooler a
(112), product slot (113), cooler b (114), first metering pump (101), the second metering pump (102) by threeway with
Static mixer (103) connection setting, the static mixer (103) are connect with high-temperature pipe reactor (104) by pipeline
Setting, static mixer (103) are connected with the feed inlet of crude product temporary storage tank (105), and light component rectifying column (107) and crude product are temporary
It deposits and is connected between tank (105) by circulating pump a (106), light component rectifying column (107) is connect with the feed inlet of cooler b (114)
Setting, circulating pump a (106) connect setting, cooler a (112) and product with circulating pump b (109) by product rectifying column (110)
Rectifying column (110) connection setting, reboiler a (108) discharge port is connect with the discharge port of light component rectifying column (107) and it feeds
Mouth connect setting with the discharge port of circulating pump a (106), the discharge port of reboiler b (111) and, the discharging of product rectifying column (110)
Mouthful connection and its feed inlet with the discharge port of circulating pump b (109) connect setting；
The reboiler a (108), reboiler b (111) include body assembly (1), are arranged on the body assembly (1)
Water inlet component (2), cleaning assemblies (3) in the body assembly (1) is set and be connected to the water inlet component (2) be arranged and
The discharge component (4) of synchronous rotation；
The discharge component (4) includes sewage unit (47) and drainage cell (48), the sewage unit (47) and drainage cell
(48) setting is connected to the water inlet component (2) alternative expression respectively, completes the mask work of water purification and dirty material.
2. a kind of preparation system of octylpyrrolidone according to claim 1, which is characterized in that the body assembly
(1) include:
Rack (11)；And
Body (12), the body (12) include shell (15), flange (16), discharge port (17), feed inlet (18), tube sheet (19)
With heat exchanger tube (20).
3. a kind of preparation system of octylpyrrolidone according to claim 2, which is characterized in that the water inlet component
(2) include:
Water supplying unit (21), the water supplying unit (21) include the water pump water tank all-in-one machine (22) being mounted on the rack (11)
The water pipe a (23) of setting is connected to with the water pump water tank all-in-one machine (22)；And
Control unit (24), described control unit (24) include that setting is pasted in the flange (16) side and with the flange (16)
It closes the turntable (25) of setting and is arranged in the turntable (25) side and is bonded the fixing seat (26) being arranged with the turntable (25),
The turntable (25) is rotatably arranged on the rack (11), and the fixing seat (26) is fixedly mounted on the rack (11)；
The flange (16), turntable (25) and fixing seat (26) are coaxially disposed and turntable (25) is centrally located.
4. a kind of preparation system of octylpyrrolidone according to claim 3, which is characterized in that the flange (16) and
Through-hole a (27) is offered in fixing seat (26) and is symmetrical arranged relatively with the turntable (25), and the fixing seat (26) is led to
Hole a (27) is connected to setting with the water pipe a (23)；
It is also provided with through-hole b (28) on the flange (16) and fixing seat (26) and is symmetrically set with the turntable (25) relatively
Set, the through-hole a (27) and through-hole b (28) diametrically linear setting, the through-hole b (28) of the fixing seat (26) with it is described
Component (4) connection setting is discharged；
The turntable (25) offers through-hole c (29) and through-hole d (30), the through-hole c (29) and through-hole d (30) respectively with it is described
Through-hole a (27) is connected to setting with through-hole b (28) discontinuous；
The through-hole a (27), through-hole b (28), through-hole c (29) are identical with through-hole d (30) caliber size, are A1.
5. a kind of preparation system of octylpyrrolidone according to claim 1, which is characterized in that the cleaning assemblies
(3) include:
Cleaning ball (31), the cleaning ball (31) are cylindrical body and are flexible material structure setting, cleaning ball (31) both ends
For hollow setting and intermediate position is solid setting；
Salient point (32), the salient point (32) is evenly distributed on cleaning ball (31) side and through setting, along the cleaning ball
(31) two neighbouring in the short transverse salient points (32) misplace alternate setting, and hang down along the cleaning ball (31) height
The distance between adjacent two described salient points (32) are L1 to histogram upwards, and the width of salient point (32) is L2, L1=L2, described convex
Point (32) is located at the internal section bottom of the cleaning ball (31) and offers chamfering；And
Shore unit (33), it is described shore unit (33) be symmetricly set on along the middle line in the cleaning ball (31) length it is described
The upper bottom surface of cleaning ball (31) comprising mobile setting it is internal in the cleaning ball (31) and with the salient point (32) bottom surface
The connecting plate (35) of tapered pole (34), tapered pole (34) bottom surface arranged symmetrically with setting and one end and the connecting plate (35) are even
It connects setting and the other end connect the spring (36) being arranged with the cleaning ball (31) bottom.
6. a kind of preparation system of octylpyrrolidone according to claim 3, which is characterized in that the discharge component
It (4) further include driving unit (40), the driving unit (40) includes:
Motor (41), the motor (41) are mounted on the rack (11)；
Drive shaft (42), described drive shaft (42) one end is connect with the output end of the motor (41) and the other end and the turntable
(25) it being fixedly connected, wears groove (43) of the drive shaft (42) in the fixing axle, the bore of the wears groove (43) is D1,
The bore of the drive shaft (42) is D2, D1 > D2；
Gear a (44), the gear a (44) is coaxial with the drive shaft (42) and is fixedly connected；
Gear b (45), the gear b (45) are engaged with the gear a (44)；And
Rotation axis (46), the rotation axis (46) are fixed on the fixing seat (26) and rotate with the gear b (45)
Setting.
7. a kind of preparation system of octylpyrrolidone according to claim 6, which is characterized in that the sewage unit
(47) and drainage cell (48) is water pipe b, is arranged on the rotation axis (46) and is symmetricly set on the rotation axis
(46) two sides, the drainage cell (48) are embedded in the sewage unit (47) described in towards the motor (41) one end
Motor (41) one end, the outer annular diameter of water pipe b are A2, annular diameters A3, A2 > A1 > A3.
8. a kind of preparation system of octylpyrrolidone according to claim 1, which is characterized in that the high-temperature tubular is anti-
Answering device (104) reaction temperature is 230-300 DEG C.
9. a kind of preparation system of octylpyrrolidone according to claim 1, which is characterized in that the high-temperature tubular is anti-
The external dimensions for answering device (104) is DN800*4000.
10. a kind of preparation system of octylpyrrolidone according to claim 1, which is characterized in that the static mixing
Device (103) uses jacket type structure.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910594305.2A CN110229090B (en) | 2019-07-02 | 2019-07-02 | Preparation system of octyl pyrrolidone |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910594305.2A CN110229090B (en) | 2019-07-02 | 2019-07-02 | Preparation system of octyl pyrrolidone |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112023861A (en) * | 2020-09-14 | 2020-12-04 | 安徽英特力工业工程技术有限公司 | Energy-saving NMP reactor |
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| CN1865243A (en) * | 2006-06-23 | 2006-11-22 | 杭州建华科技有限公司 | Production method of N-dodecyl pyrrolidone |
| CN204246861U (en) * | 2014-10-30 | 2015-04-08 | 天津河清化学工业有限公司 | Isooctyl thioglycolate continuous rectification system |
| CN106311685A (en) * | 2016-08-30 | 2017-01-11 | 安徽安特食品股份有限公司 | Non-halt efficient scale removing equipment of horizontal reboiler |
| WO2017177763A1 (en) * | 2016-04-11 | 2017-10-19 | 山东万圣博科技股份有限公司 | System and method for separating n-methyl-2-pyrrolidone/chloroform |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1865243A (en) * | 2006-06-23 | 2006-11-22 | 杭州建华科技有限公司 | Production method of N-dodecyl pyrrolidone |
| CN204246861U (en) * | 2014-10-30 | 2015-04-08 | 天津河清化学工业有限公司 | Isooctyl thioglycolate continuous rectification system |
| WO2017177763A1 (en) * | 2016-04-11 | 2017-10-19 | 山东万圣博科技股份有限公司 | System and method for separating n-methyl-2-pyrrolidone/chloroform |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112023861A (en) * | 2020-09-14 | 2020-12-04 | 安徽英特力工业工程技术有限公司 | Energy-saving NMP reactor |
| CN112023861B (en) * | 2020-09-14 | 2024-05-14 | 安徽英特力工业工程技术有限公司 | Energy-saving NMP reactor |
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| CN110229090B (en) | 2024-01-23 |
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