CN110229090B - Preparation system of octyl pyrrolidone - Google Patents
Preparation system of octyl pyrrolidone Download PDFInfo
- Publication number
- CN110229090B CN110229090B CN201910594305.2A CN201910594305A CN110229090B CN 110229090 B CN110229090 B CN 110229090B CN 201910594305 A CN201910594305 A CN 201910594305A CN 110229090 B CN110229090 B CN 110229090B
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- assembly
- cleaning ball
- Prior art date
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- WPPOGHDFAVQKLN-UHFFFAOYSA-N N-Octyl-2-pyrrolidone Chemical compound CCCCCCCCN1CCCC1=O WPPOGHDFAVQKLN-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 103
- 238000004140 cleaning Methods 0.000 claims abstract description 80
- 239000000047 product Substances 0.000 claims abstract description 33
- 230000003068 static effect Effects 0.000 claims abstract description 28
- 238000003860 storage Methods 0.000 claims abstract description 17
- 239000012043 crude product Substances 0.000 claims abstract description 12
- 238000000926 separation method Methods 0.000 claims abstract description 12
- 239000010865 sewage Substances 0.000 claims abstract description 12
- 239000008213 purified water Substances 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 230000000149 penetrating effect Effects 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 3
- 238000010276 construction Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 description 17
- 238000007599 discharging Methods 0.000 description 16
- 238000000034 method Methods 0.000 description 11
- 239000002994 raw material Substances 0.000 description 10
- 238000011010 flushing procedure Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 7
- 238000010586 diagram Methods 0.000 description 5
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 4
- 238000007789 sealing Methods 0.000 description 3
- NJPQAIBZIHNJDO-UHFFFAOYSA-N 1-dodecylpyrrolidin-2-one Chemical compound CCCCCCCCCCCCN1CCCC1=O NJPQAIBZIHNJDO-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229930188620 butyrolactone Natural products 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001944 continuous distillation Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002837 defoliant Substances 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
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 239000002085 irritant Substances 0.000 description 1
- 231100000021 irritant Toxicity 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
- 238000010907 mechanical stirring Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000005070 sampling Methods 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
- 239000008207 working material Substances 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
Abstract
The invention relates to a preparation system of octyl pyrrolidone, which comprises a first metering pump, a second metering pump, a static mixer, a high-temperature pipeline reactor, a crude product temporary storage tank, a circulating pump a, a light component rectifying tower, a reboiler a, a circulating pump b, a product rectifying tower, a reboiler b, a cooler a and a product tank; the reboiler a and the reboiler b comprise a main body assembly, a water inlet assembly arranged on the main body assembly, a cleaning assembly arranged in the main body assembly and a discharge assembly communicated with the water inlet assembly and synchronously rotating with the water inlet assembly; the drainage assembly comprises a drainage unit and a drainage unit, and the drainage unit and the water inlet assembly are respectively and alternately communicated to finish the separation work of the purified water and the sewage; the invention solves the technical problems that scale is generated in the reboiler step and the purity and quality of the product are affected.
Description
Technical Field
The invention relates to the technical field of octyl pyrrolidone preparation, in particular to a system for preparing octyl pyrrolidone.
Background
N-octyl pyrrolidone is a chemical substance, has a molecular formula of C12H23NO, is a colorless to yellow liquid compound with an amine smell, has a CAS number of 2687-94-7 and a molecular weight of 197.32, and is widely used as an insecticide, a cotton defoliant, a concentrated cleaning agent, a chemical reaction solvent, a pharmaceutical synthesis medium and a coating stripping agent in the electronic industry. Can be used as a surfactant, can be compounded with anionic or nonionic surfactants to reduce the surface tension and provide the product performance.
At present, most of octyl pyrrolidone production processes are pressurized intermittent production processes, the production method has the advantages of relatively small productivity, large equipment occupation, difficulty in realizing automatic control, large capital investment and high production cost, and mechanical stirring mechanical sealing is easy to wear and damage at high temperature, so that the maintenance cost of the device is high.
Patent document CN2006100520938N discloses a process for the production of N-dodecyl pyrrolidone, which comprises the steps of: (1) Adding the dodecyl amine and the r-butyrolactone into a batching kettle, stirring at a high speed, and then sending the mixture into a pipeline reactor with a front section of which the length is 40% -60% of that of a static mixer for reaction; (2) And (3) sending the mixture after the reaction in the pipeline reactor into a continuous distillation tower for decompression separation, wherein the bottom product is N-dodecyl pyrrolidone.
However, in the actual use process, the inventor finds that scale is generated in the reboiler step, and the separation of the scale and the clean water is complicated and the purity of the product is affected.
Disclosure of Invention
The invention aims at overcoming the defects of the prior art, and the water pressure flushing cleaning assembly is arranged to guide the water pressure flushing cleaning assembly to stably move in the heat exchange tube, so that the scale is quickly and efficiently removed in the moving process, and the technical problems that the scale is generated in the step of a reboiler, the separation work of the scale and clear water is complicated, and the purity of a product is influenced are solved.
Aiming at the technical problems, the technical scheme is as follows: a system for preparing octyl pyrrolidone, characterized by: the device comprises a first metering pump, a second metering pump, a static mixer, a high-temperature pipeline reactor, a crude product temporary storage tank, a circulating pump a, a light component rectifying tower, a reboiler a, a circulating pump b, a product rectifying tower, a reboiler b, a cooler a, a product tank and a cooler b, wherein the first metering pump and the second metering pump are communicated with the static mixer through a tee joint, the static mixer is connected with the high-temperature pipeline reactor through a pipeline, the static mixer is connected with a feed inlet of the crude product temporary storage tank, the light component rectifying tower is connected with the crude product temporary storage tank through the circulating pump a, the light component rectifying tower is connected with a feed inlet of the cooler b, the circulating pump a is connected with the circulating pump b through the product rectifying tower, a discharge port of the reboiler a is connected with a discharge port of the light component rectifying tower, the discharge port of the reboiler b is connected with a discharge port of the circulating pump a, and the feed inlet of the reboiler b is connected with a discharge port of the circulating pump b;
the reboiler a and the reboiler b comprise a main body assembly, a water inlet assembly arranged on the main body assembly, a cleaning assembly arranged in the main body assembly and a discharge assembly communicated with the water inlet assembly and synchronously rotating with the water inlet assembly;
the drainage assembly comprises a drainage unit and a drainage unit, the drainage unit and the drainage unit are respectively communicated with the water inlet assembly alternately, and the separation work of the purified water and the sewage is completed.
Preferably, the body assembly includes:
a frame; and
the device body comprises a shell, a flange, a discharge hole, a feed inlet, a tube plate and a heat exchange tube.
Preferably, the water inlet assembly includes:
the water supply unit comprises a water pump and water tank integrated machine arranged on the frame and a water pipe a communicated with the water pump and water tank integrated machine; and
the control unit comprises a rotary table arranged on one side of the flange and attached to the flange, and a fixed seat arranged on one side of the rotary table and attached to the rotary table, wherein the rotary table is rotatably arranged on the frame, and the fixed seat is fixedly arranged on the frame;
the flange, the turntable and the fixing seat are coaxially arranged, and the turntable is arranged in the middle.
Preferably, the flange and the fixing seat are provided with through holes a which are symmetrically arranged relative to the turntable, and the through holes a of the fixing seat are communicated with the water pipe a;
the flange and the fixing seat are respectively provided with a through hole b which is symmetrically arranged relative to the turntable, the through holes a and b are linearly arranged along the diameter direction, and the through holes b of the fixing seat are communicated with the discharge assembly;
the turntable is provided with a through hole c and a through hole d, and the through hole c and the through hole d are respectively communicated with the through hole a and the through hole b in an intermittent manner;
and the apertures of the through holes a, b, c and d are the same as each other, and the apertures are all A1.
Preferably, the cleaning assembly comprises:
the cleaning ball is cylindrical and is of a flexible material structure, two ends of the cleaning ball are hollow, the middle part of the cleaning ball is solid, and the cleaning ball sequentially flows through a through hole c, a through hole a, a heat exchange tube, a through hole b and a through hole d under the impulse of water;
the bumps are uniformly distributed on the side surface of the cleaning ball and penetrate through the side surface of the cleaning ball, two adjacent bumps are arranged alternately in a staggered mode along the height direction of the cleaning ball, the distance between the two adjacent bumps along the vertical direction of the height of the cleaning ball is L1, the width of each bump is L2, L1=L2, and a chamfer is formed in the bottom of the part of each bump, which is positioned inside the cleaning ball; and
the supporting unit is symmetrically arranged on the upper bottom surface and the lower bottom surface of the cleaning ball along the central line on the length of the cleaning ball, and comprises a conical column, a connecting plate and a spring, wherein the conical column is movably arranged inside the cleaning ball and matched with the bottom surface of the convex point, the connecting plate is symmetrically arranged on the bottom surface of the conical column, one end of the connecting plate is connected with the connecting plate, and the other end of the spring is connected with the bottom of the cleaning ball.
Preferably, the discharge assembly further includes a driving unit including:
the motor is arranged on the frame;
the driving shaft penetrates through a through groove on the fixed shaft, the caliber of the through groove is D1, the caliber of the driving shaft is D2, and D1 is more than D2;
the gear a is coaxial with the driving shaft and fixedly connected with the driving shaft;
the gear b is meshed with the gear a;
and the rotating shaft is fixedly arranged on the fixed seat and is rotatably arranged with the gear b.
Preferably, the drainage unit and the drainage unit are water pipes b which are arranged on the rotating shaft and symmetrically arranged on two sides of the rotating shaft, the drainage unit is embedded into one end of the drainage unit, which faces the motor, of the drainage unit, the diameter of the outer ring of the water pipe b is A2, the diameter of the inner ring of the water pipe b is A3, and A2 is more than A1 and more than A3.
Preferably, the high-temperature tubular reactor has a reaction temperature of 230-300 ℃.
Preferably, the external dimensions of the high temperature tubular reactor are DN800 x 4000.
As a further preference, the static mixer is of a jacketed construction.
The invention has the beneficial effects that:
(1) According to the invention, the water pressure flushing cleaning assembly is arranged to guide the water pressure flushing cleaning assembly to stably move in the heat exchange tube, so that the scale is quickly and efficiently removed in the moving process, and the reboiler is not required to be stopped, disassembled and the like, so that the investment of manpower and material resources is greatly reduced, and the production efficiency is improved; in addition, by arranging the sewage discharging unit and the water discharging unit in the discharging assembly to be alternately connected with the water assembly, the automatic separation of scale and clean water is realized, the automation of the whole device is improved, and the labor productivity is reduced;
(2) According to the invention, the cleaning assembly is arranged, when water pressure acts on the conical column, the conical column is matched with the salient points through the inclined openings, so that the salient points are outwards spread under the water pressure and fully contact with the inner wall of the heat exchange tube, and further, even after the cleaning assembly is used for a long time, the cleaning assembly can still ensure the full contact between the cleaning ball and the heat exchange tube, and simultaneously, the tension force of the cleaning ball for bonding the cleaning ball and the heat exchange tube is utilized, so that the cleaning ball can fully clean the scale on the inner wall of the heat exchange tube, and meanwhile, the cleaning assembly is beneficial to better conveying the scale and improving the working efficiency;
(3) According to the invention, the driving unit is arranged to be matched with the sewage discharging unit and the water discharging unit, so that the driving unit drives the turntable to rotate on one hand, and the cleaning ball is reset to the initial working position; in addition, the sewage draining unit and the water draining unit are driven to rotate, so that alternate switching of sewage draining and water draining works is realized; the two works are driven by one power, the front and back works are closely connected, errors are not easy to occur, and the thorough separation of scale and clean water is facilitated; meanwhile, extra power is saved, and the production cost is reduced;
(4) According to the invention, continuous feeding and output can be realized through the pipeline reactor, compared with the kettle reactor adopted in the prior art, the production capacity of the device is obviously improved, movable equipment is changed into static equipment, the service life of the equipment is long, the production efficiency is high, meanwhile, double-tower continuous rectification is adopted, the unit productivity is improved, and the product quality is more stable.
In conclusion, the equipment has the advantages of long service life and low production cost, and is particularly suitable for the technical field of octyl pyrrolidone preparation.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, it being obvious that the drawings described below are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic flow diagram of a system for preparing octyl pyrrolidone.
Fig. 2 is a schematic structural diagram of reboiler a.
Fig. 3 is a schematic structural diagram of the control unit.
Fig. 4 is a schematic structural view of the cleaning assembly.
Fig. 5 is a schematic diagram of a bump distribution structure.
Fig. 6 is a schematic diagram of the alternate operation of the blowdown unit and the drain unit.
Fig. 7 is a schematic cross-sectional view of the drive unit.
Fig. 8 is an enlarged partial schematic view of fig. 7 at a.
Fig. 9 is an enlarged partial schematic view of fig. 7 at B.
Fig. 10 is an enlarged partial schematic view of fig. 7 at C.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the accompanying drawings.
Example 1
As shown in fig. 1 and fig. 2, a preparation system of octyl pyrrolidone comprises a first metering pump 101, a second metering pump 102, a static mixer 103, a high-temperature pipeline reactor 104, a crude product temporary storage tank 105, a circulating pump a106, a light component rectifying tower 107, a reboiler a108, a circulating pump b109, a product rectifying tower 110, a reboiler b111, a cooler a112, a product tank 113 and a cooler b114, wherein the first metering pump 101 and the second metering pump 102 are communicated with the static mixer 103 through a tee joint, the static mixer 103 is connected with the high-temperature pipeline reactor 104 through a pipeline, the static mixer 103 is connected with a feed port of the crude product temporary storage tank 105, the light component rectifying tower 107 is connected with the crude product temporary storage tank 105 through a circulating pump a106, the circulating pump a106 is connected with the circulating pump b109, the cooler a112 is connected with the product rectifying tower 110, a discharge port of the a108 is connected with a discharge port of the light component rectifying tower 107 and the circulating pump b111 is connected with a discharge port of the circulating pump b 106, and the discharge port of the light component rectifying tower 107 is connected with the discharge port of the circulating pump b 110;
the reboiler a108 and the reboiler b111 comprise a main body component 1, a water inlet component 2 arranged on the main body component 1, a cleaning component 3 arranged in the main body component 1 and a discharge component 4 communicated with the water inlet component 2 and synchronously rotating with the water inlet component;
the discharging assembly 4 comprises a pollution discharge unit 47 and a drainage unit 48, and the pollution discharge unit 47 and the drainage unit 48 are respectively communicated with the water inlet assembly 2 alternately to finish the separation work of the purified water and the sewage.
Compared with the traditional preparation system, the invention creatively has the advantages that the reboiler a108 and the reboiler b111 are provided with the water pressure flushing cleaning assembly 3 to guide the water pressure flushing cleaning assembly to stably move in the heat exchange tube, the scale is quickly and efficiently removed in the moving process, the reboiler is not required to be stopped, disassembled and the like, the investment of manpower and material resources is greatly reduced, and the production efficiency is improved; in addition, by arranging the sewage discharging unit 47 and the water discharging unit 48 in the discharging assembly 4 to be alternately connected with the water assembly 2, the automatic separation of scale and clean water is realized, the automation of the whole device is improved, and the labor productivity is reduced.
In the embodiment, the preparation process sequentially passes through a first metering pump 101, a second metering pump 102, a static mixer 103, a high-temperature tubular reactor 104, a crude product temporary storage tank 105, a circulating pump a106, a light component rectifying tower 107, a reboiler a108, a circulating pump b109, a product rectifying tower 110, a reboiler b111, a cooler a112 and a product tank 113, wherein a feed inlet of the first metering pump is connected with a butyrolactone raw material tank, a feed inlet of the second metering pump is connected with an n-octylamine raw material tank, outlets of the two metering pumps are fully mixed through the static mixer through a tee joint, the mixture is sent to the high-temperature tubular reactor, a material passing through the high-temperature tubular reactor flows into a jacket of the static mixer to preheat the raw material mixture, then the mixture is sent to the crude product temporary storage tank, the light component rectifying tower is pumped into the product rectifying tower, and after light component water is removed from the light component rectifying tower, and products are continuously produced; the investment and equipment occupation of the whole process are small, the operation is simple, the continuous production is realized, the DCS can be controlled automatically, the energy consumption and the labor cost are saved, and the production cost is reduced; the reaction time is short, the yield is stable, and the yield can reach more than 93 percent; the pressure airtight reaction is carried out, and the safety coefficient is high. The production process has no corrosion or irritant substances, so that the production equipment is not corroded and the environmental pollution is not generated.
In detail, the discharge gate of first measuring pump and the discharge gate of second measuring pump are connected to a pipeline through the tee bend, the check valve is connected through the pipe connection the feed inlet of static mixer to another pipe end, the discharge gate of static mixer passes through the pipe connection the feed inlet of high temperature tubular reactor, the discharge gate of high temperature tubular reactor passes through the pipe connection the clamp cover feed inlet of static mixer, the clamp cover discharge gate of static mixer is connected crude temporary storage tank, the light component rectifying column is gone into through the pump continuous pump to the discharge gate of crude temporary storage tank, and the light component shifts out the system through the condensation, and semi-manufactured goods pump into product rectifying column in succession, and the product is through separation condensation continuous output. The system is provided with a ball valve, a sampling valve, an emptying valve, a tube side thermometer, a back pressure valve, a tube side pressure gauge and the like.
In addition, the crude product is continuously separated and produced through double towers, so that the operation is convenient, the energy is saved, and the utilization rate of the towers is improved; meanwhile, continuous feeding and output can be realized through the pipeline reactor, compared with a kettle-type reactor adopted in the prior art, the production capacity of the device is obviously improved, movable equipment is changed into static equipment, the service life of the equipment is long, the production efficiency is high, double-tower continuous rectification is adopted, the unit productivity is improved, and the product quality is more stable.
Further, as shown in fig. 2, the main body assembly 1 includes:
a frame 11; and
the device body 12, the device body 12 comprises a shell 15, a flange 16, a discharge hole 17, a feed inlet 18, a tube plate 19 and heat exchange tubes 20.
In this embodiment, the device body 12 can heat and vaporize the material from the inlet 18 at the bottom of the housing 15, and the gas phase material is returned from the outlet 17 to the rectifying tower
Further, as shown in fig. 2 and 3, the water inlet assembly 2 includes:
a water supply unit 21, wherein the water supply unit 21 comprises a water pump and water tank integrated machine 22 arranged on the frame 11 and a water pipe a23 communicated with the water pump and water tank integrated machine 22; and
the control unit 24 comprises a rotary table 25 arranged on one side of the flange 16 and attached to the flange 16, and a fixed seat 26 arranged on one side of the rotary table 25 and attached to the rotary table 25, wherein the rotary table 25 is rotatably arranged on the frame 11, and the fixed seat 26 is fixedly arranged on the frame 11;
the flange 16, the turntable 25 and the fixed seat 26 are coaxially arranged, and the turntable 25 is arranged in the middle.
In the embodiment, the turntable 25 is arranged to realize the automatic resetting of the cleaning balls 31 embedded in the turntable 25; meanwhile, the turntable 25 has a sealing effect on the device body 12 in the process of rotating.
Further, as shown in fig. 3, the flange 16 and the fixing seat 26 are provided with a through hole a27 and are symmetrically arranged relative to the turntable 25, and the through hole a27 of the fixing seat 26 is communicated with the water pipe a23;
the flange 16 and the fixed seat 26 are respectively provided with a through hole b28 which is symmetrically arranged relative to the turntable 25, the through holes a27 and b28 are linearly arranged along the diameter direction, and the through hole b28 of the fixed seat 26 is communicated with the discharge assembly 4;
the turntable 25 is provided with a through hole c29 and a through hole d30, and the through hole c29 and the through hole d30 are respectively communicated with the through hole a27 and the through hole b28 in an intermittent manner;
the diameters of the through hole a27, the through hole b28, the through hole c29 and the through hole d30 are the same, and the diameters are all A1.
In this embodiment, the cleaning ball flows through the through hole a27, the through hole c29, the through hole a27, the heat exchange tube 20, the through hole b28, the through hole d30 and the through hole b28 in sequence under the flushing of the water pressure, and the normal flow of water is realized by connecting the ports of the cleaning ball.
Further, as shown in fig. 4 and 5, the cleaning assembly 3 includes:
the cleaning balls 31 are cylindrical and are of flexible material structures, two ends of each cleaning ball 31 are hollow, and the middle part of each cleaning ball 31 is solid;
the bumps 32 are uniformly distributed on the side surface of the cleaning ball 31 and penetrate through the cleaning ball, two bumps 32 which are adjacent up and down along the height direction of the cleaning ball 31 are arranged at intervals in a staggered manner, the distance between two adjacent bumps 32 along the height direction of the cleaning ball 31 is L1, the width of each bump 32 is L2, L1=L2, and a chamfer is formed at the bottom of a part of each bump 32 which is positioned inside the cleaning ball 31; and
the supporting unit 33, the supporting unit 33 is symmetrically arranged on the upper bottom surface and the lower bottom surface of the cleaning ball 31 along the central line on the length of the cleaning ball 31, and comprises a conical column 34, a connecting plate 35 and a spring 36, wherein the conical column 34 is movably arranged inside the cleaning ball 31 and is matched with the bottom surface of the convex point 32, the connecting plate 35 is symmetrically arranged on the bottom surface of the conical column 34, one end of the spring 36 is connected with the connecting plate 35, and the other end of the spring is connected with the bottom of the cleaning ball 31.
In this embodiment, by arranging the cleaning assembly 3, when water pressure acts on the tapered column 34, the tapered column 34 is utilized to be matched with the protruding points 32 in a bevel manner, so that the protruding points are outwards spread under the water pressure and fully contact with the inner wall of the heat exchange tube 20, and further, even after long-term use, the cleaning ball 31 can be fully contacted with the heat exchange tube 20, and meanwhile, the tension force of the cleaning ball 31 attached to the heat exchange tube 20 is utilized, so that the scale on the inner wall of the heat exchange tube 20 is fully cleaned by the cleaning ball 31, and the working efficiency is improved;
it should be noted that, by arranging the spring 36, the automatic reset of the conical column 34 under the condition of no flushing by water pressure is realized, and as the cleaning ball 31 is of a flexible material structure, the cleaning ball 31 does not interfere when moving in the heat exchange tube 20;
it should be emphasized that the provision of the bumps is to achieve sufficient contact between the cleaning balls 31 and the inner wall of the heat exchange tube 20 with a minimum of material, so as to enhance the overall flushing of the scale on the inner wall of the heat exchange tube 20.
Further, as shown in fig. 6 and 7, the discharging unit 4 further includes a driving unit 40, and the driving unit 40 includes:
a motor 41, said motor 41 being mounted on said frame 11;
the driving shaft 42, one end of the driving shaft 42 is connected with the output end of the motor 41, and the other end of the driving shaft 42 is fixedly connected with the turntable 25, the driving shaft 42 penetrates through a penetrating groove 43 on the fixing shaft, the caliber of the penetrating groove 43 is D1, and the caliber of the driving shaft 42 is D2, wherein D1 is more than D2;
a gear a44, wherein the gear a44 is coaxial with and fixedly connected with the driving shaft 42;
a gear b45, wherein the gear b45 is meshed with the gear a 44; and
the rotating shaft 46, the rotating shaft 46 is fixedly arranged on the fixing seat 26 and is rotatably arranged with the gear b 45.
In the embodiment, by arranging the driving unit 40 to cooperate with the sewage discharging unit 47 and the water discharging unit 48, the driving unit 40 drives the turntable 25 to rotate on one hand, and the cleaning balls are reset to the initial working position; in addition, the rotation of the sewage discharging unit 47 and the water discharging unit 48 is driven to realize the alternate switching of the sewage discharging and water discharging; the two works are driven by one power, so that dirt in front of the cleaning ball 31 is output through the pollution discharge unit 47, and clear water behind the cleaning ball 31 synchronously drives the switching of the pollution discharge unit 47 and the water discharge unit 48 in the resetting action of the cleaning ball 31, so that clear water flows out of the water discharge unit 48, the front and rear works are closely connected, errors are not easy to occur, and the thorough separation of the water scale and the clear water is facilitated; meanwhile, extra power is saved, and the production cost is reduced.
In detail, the ratio of the teeth of the gears is such that the motor 41 drives the turntable to rotate 180 ° and the gear b45 rotates 180 °.
Further, the reaction temperature of the high-temperature tubular reactor 104 is 230-300 ℃.
Further, the external dimensions of the high temperature tubular reactor 104 are DN800 x 4000.
It is worth mentioning that the jacket of the high temperature tube reactor is heated by heat transfer oil.
Further, the static mixer 103 adopts a jacket type structure.
In this example, the raw materials were preheated by the heat of the reaction mass by providing a static mixer 103 using a jacketed type.
Example two
As shown in fig. 9 and 10, the same or corresponding parts as those in the first embodiment are denoted by the same reference numerals as those in the first embodiment, and only the differences from the first embodiment will be described below for the sake of brevity. The second embodiment is different from the first embodiment in that:
further, as shown in fig. 9 and 10, the drain unit 47 and the drain unit 48 are water pipes b, which are disposed on the rotating shaft 46 and symmetrically disposed on two sides of the rotating shaft 46, one end of the drain unit 48 facing the motor 41 is embedded in one end of the drain unit 47 facing the motor 41, an outer ring diameter of the water pipe b is A2, and an inner ring diameter thereof is A3, A2 > A1 > A3.
In this embodiment, by arranging the output portions of the drain unit 47 and the drain unit 48 in an embedded manner, the purpose of the present embodiment is to avoid the phenomenon that the drain unit 47 and the drain unit 48 are knotted and wound in the rotation process, and interfere with the normal operation of the work, which is worth to be explained, the embedded drain unit 47 of the drain unit 48 is a conventional technical means in the art, only the drain unit 47 needs to be perforated to allow the drain unit 48 to penetrate, the caliber of the drain unit 47 is large, and the perforated connection portion can be connected in a sealing manner such as glue.
It should be noted that the purpose of A2 > A1 > A3 is, on the one hand, to allow clean water or scale to flow completely into the water pipe b; on the other hand, the wall thickness of the water pipe b is used for limiting the cleaning ball.
The working process comprises the following steps:
the raw material butyrolactone is pumped into a three-way pipeline at the speed of 300kg/h through a metering pump a and the raw material n-octylamine is pumped into a static mixer with a jacket at the speed of 450kg/h through a metering pump b for mixing, the mixture is fully mixed and preheated and then reacted through a high-temperature tubular reactor, the high-temperature reactor is heated to the temperature of 280 ℃ through heat conducting oil for reaction, the raw material is produced after passing through the high-temperature tubular reactor, the raw material mixture is preheated through a preheater jacket, and meanwhile, the raw material is cooled down to a raw material temporary storage tank, and the sample analysis content is 94.3%. The crude product temporary storage tank material is continuously pumped into a light component rectifying tower through a pump, the light component tower is heated through a reboiler a, light component water is continuously separated, a heavy component, namely a semi-product, is removed from the product rectifying tower, the product rectifying tower is heated through a reboiler b and is in high vacuum, products are continuously separated in the product rectifying tower, the product content is 99.2%, and a small amount of high-boiling product is removed from the system.
The specific working materials of the reboiler a enter the shell 15 from the feed inlet 18, the materials are in contact with the heat exchange tube 20 and perform heat transfer, meanwhile, the water pump and water tank integrated machine 22 is started, hot water flows into the heat exchange tube 20 through the water tube a23 and pushes the cleaning ball 31, the cleaning ball 31 is spread under the action of water pressure in the moving process of the heat exchange tube 20, meanwhile, scale on the inner wall of the heat exchange tube 20 is flushed, the scale is positioned in front of the cleaning ball 31, clean water is positioned behind the cleaning ball 31, the scale is discharged from the pollution discharge unit 47, the motor 41 is started, the motor 41 rotates 180 degrees, the cleaning ball 3 is reset to an initial position, the gear b45 rotates 180 degrees, the water discharge unit 48 is communicated with the through hole b28, and clean water is discharged; in the process of the clear water flowing in the heat exchange tube 20, the high-temperature water heats and vaporizes the low-temperature materials, and the gas-phase materials enter the subsequent treatment through the discharge hole 17:
the specific operation of reboiler b is the same as that of reboiler a and will not be described here.
In the description of the present invention, it should be understood that the directions or positional relationships indicated by the terms "front and rear", "left and right", etc. are based on the directions or positional relationships shown in the drawings, are merely for convenience of description and simplification of the description, and do not indicate or imply that the apparatus or component in question must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as limiting the invention.
Of course, in this disclosure, those skilled in the art will understand that the term "a" or "an" is to be interpreted as "at least one" or "one or more," i.e., in one embodiment, the number of elements may be one, and in another embodiment, the number of elements may be multiple, and the term "a" is not to be construed as limiting the number.
The foregoing is merely a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions easily conceivable by those skilled in the art under the technical teaching of the present invention should be included in the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.
Claims (6)
1. A system for preparing octyl pyrrolidone, characterized by: including first measuring pump (101), second measuring pump (102), static mixer (103), high temperature pipeline reactor (104), crude 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 groove (113), cooler b (114), first measuring pump (101), second measuring pump (102) are through tee bend and static mixer (103) intercommunication setting, static mixer (103) are connected with the feed inlet that high temperature pipeline reactor (104) passed through the pipeline and set up, static mixer (103) are connected with crude temporary storage tank (105), be connected through circulating pump a (106) between light component rectifying column (107) and crude temporary storage tank (105), feed inlet that light component rectifying column (107) and cooler b (114) are connected and are set up, circulating pump a (106) are connected through product rectifying column (110) and circulating pump b (109) are connected and are set up, cooler a (108) are connected with reboiler a (110) and are connected with light component rectifying column (110) and product rectifying column (112) are connected with the feed inlet (110) and discharge port (106) are connected with crude product temporary storage tank (105) and discharge port (106) The discharge port of the product rectifying tower (110) is connected with the discharge port of the circulating pump b (109);
the reboiler a (108) and the reboiler b (111) comprise a main body component (1), a water inlet component (2) arranged on the main body component (1), a cleaning component (3) arranged in the main body component (1) and a discharge component (4) communicated with the water inlet component (2) and synchronously rotating with the water inlet component;
the drainage assembly (4) comprises a drainage unit (47) and a drainage unit (48), and the drainage unit (47) and the drainage unit (48) are respectively and alternately communicated with the water inlet assembly (2) to finish the separation work of purified water and sewage;
the body assembly (1) comprises:
a frame (11); and
the device comprises a device body (12), wherein the device body (12) comprises a shell (15), a flange (16), a discharge hole (17), a feed inlet (18), a tube plate (19) and heat exchange tubes (20);
the water inlet assembly (2) comprises:
the water supply unit (21), the water supply unit (21) comprises a water pump and water tank integrated machine (22) arranged on the frame (11) and a water pipe a (23) communicated with the water pump and water tank integrated machine (22); and
the control unit (24), the control unit (24) comprises a rotary table (25) arranged on one side of the flange (16) and attached to the flange (16) and a fixed seat (26) arranged on one side of the rotary table (25) and attached to the rotary table (25), the rotary table (25) is rotatably arranged on the frame (11), and the fixed seat (26) is fixedly arranged on the frame (11);
the flange (16), the rotary table (25) and the fixed seat (26) are coaxially arranged, and the rotary table (25) is arranged in the middle;
the flange (16) and the fixing seat (26) are respectively provided with a through hole a (27) and are symmetrically arranged relative to the turntable (25), and the through holes a (27) of the fixing seat (26) are communicated with the water pipe a (23);
the flange (16) and the fixed seat (26) are respectively provided with a through hole b (28) which is symmetrically arranged relative to the turntable (25), the through holes a (27) and b (28) are linearly arranged along the diameter direction, and the through holes b (28) of the fixed seat (26) are communicated with the discharge assembly (4);
the turntable (25) is provided with a through hole c (29) and a through hole d (30), and the through hole c (29) and the through hole d (30) are respectively communicated with the through hole a (27) and the through hole b (28) in an intermittent mode;
the diameters of the through hole a (27), the through hole b (28), the through hole c (29) and the through hole d (30) are the same, and are all A1;
the cleaning assembly (3) comprises:
the cleaning ball (31) is in a cylindrical shape and is in a flexible material structure, two ends of the cleaning ball (31) are in a hollow structure, and the middle part of the cleaning ball is in a solid structure;
the bumps (32) are uniformly distributed on the side surface of the cleaning ball (31) and penetrate through the cleaning ball, two adjacent bumps (32) are arranged at intervals in a staggered mode along the height direction of the cleaning ball (31), the distance between two adjacent bumps (32) along the height vertical direction of the cleaning ball (31) is L1, the width of each bump (32) is L2, L1=L2, and a chamfer is formed in the bottom of a part of each bump (32) positioned in the cleaning ball (31); and
the supporting unit (33), supporting unit (33) are along the central line symmetry on cleaning ball (31) length sets up the upper and lower bottom surface of cleaning ball (31), and it is including removing setting up cleaning ball (31) inside and with conical column (34) of bump (32) bottom surface matching setting, connecting plate (35) of symmetry setting conical column (34) bottom surface and one end with connecting plate (35) are connected and are set up and the other end with cleaning ball (31) bottom is connected spring (36) that set up.
2. The system for preparing octyl pyrrolidone according to claim 1, characterized in that said evacuation assembly (4) further comprises a driving unit (40), said driving unit (40) comprising:
a motor (41), the motor (41) being mounted on the frame (11);
the driving shaft (42), one end of the driving shaft (42) is connected with the output end of the motor (41) and the other end of the driving shaft is fixedly connected with the rotary table (25), the driving shaft (42) penetrates through a penetrating groove (43) on the fixed shaft, the caliber of the penetrating groove (43) is D1, and the caliber of the driving shaft (42) is D2, wherein D1 is more than D2;
a gear a (44), said gear a (44) being coaxial and fixedly connected to said drive shaft (42);
a gear b (45), wherein the gear b (45) is meshed with the gear a (44); and
the rotating shaft (46) is fixedly arranged on the fixing seat (26) and is rotatably arranged with the gear b (45).
3. The system for preparing octyl pyrrolidone according to claim 2, wherein the drain unit (47) and the drain unit (48) are water pipes b, which are disposed on the rotating shaft (46) and symmetrically disposed on both sides of the rotating shaft (46), one end of the drain unit (48) facing the motor (41) is embedded in one end of the drain unit (47) facing the motor (41), an outer ring diameter of the water pipes b is A2, and an inner ring diameter thereof is A3, A2 > A1 > A3.
4. The system for preparing octyl pyrrolidone according to claim 1, wherein the reaction temperature of the high temperature pipeline reactor (104) is 230-300 ℃.
5. The system for preparing octyl pyrrolidone according to claim 1, characterized in that the external dimensions of the high temperature pipeline reactor (104) are DN800 x 4000.
6. The system for preparing octyl pyrrolidone according to claim 1, characterized in that the static mixer (103) is of jacketed construction.
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| CN201910594305.2A CN110229090B (en) | 2019-07-02 | 2019-07-02 | Preparation system of octyl pyrrolidone |
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| CN201910594305.2A CN110229090B (en) | 2019-07-02 | 2019-07-02 | Preparation system of octyl pyrrolidone |
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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 |
| 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 |
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