CN115212839A - Purification device and purification method for prenol production - Google Patents
Purification device and purification method for prenol production Download PDFInfo
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- CN115212839A CN115212839A CN202210947068.5A CN202210947068A CN115212839A CN 115212839 A CN115212839 A CN 115212839A CN 202210947068 A CN202210947068 A CN 202210947068A CN 115212839 A CN115212839 A CN 115212839A
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- 238000000746 purification Methods 0.000 title claims abstract description 108
- ASUAYTHWZCLXAN-UHFFFAOYSA-N prenol Chemical compound CC(C)=CCO ASUAYTHWZCLXAN-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 12
- 238000007789 sealing Methods 0.000 claims abstract description 78
- 238000006243 chemical reaction Methods 0.000 claims abstract description 56
- 230000007246 mechanism Effects 0.000 claims abstract description 52
- 239000003054 catalyst Substances 0.000 claims description 34
- QVDTXNVYSHVCGW-ONEGZZNKSA-N isopentenol Chemical compound CC(C)\C=C\O QVDTXNVYSHVCGW-ONEGZZNKSA-N 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 4
- 229920006324 polyoxymethylene Polymers 0.000 claims description 4
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 3
- 235000019800 disodium phosphate Nutrition 0.000 claims description 3
- 239000001488 sodium phosphate Substances 0.000 claims description 3
- 230000000903 blocking effect Effects 0.000 claims 1
- 238000004891 communication Methods 0.000 claims 1
- 238000007670 refining Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 description 9
- 238000009434 installation Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 4
- 238000006073 displacement reaction Methods 0.000 description 4
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 3
- 235000017491 Bambusa tulda Nutrition 0.000 description 3
- 241001330002 Bambuseae Species 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 3
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 3
- 239000011425 bamboo Substances 0.000 description 3
- 239000012295 chemical reaction liquid Substances 0.000 description 3
- -1 isoamylene alcohol Chemical compound 0.000 description 3
- 239000011435 rock Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- WTEVQBCEXWBHNA-JXMROGBWSA-N geranial Chemical class CC(C)=CCC\C(C)=C\C=O WTEVQBCEXWBHNA-JXMROGBWSA-N 0.000 description 1
- 210000004907 gland Anatomy 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002728 pyrethroid Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/28—Moving reactors, e.g. rotary drums
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0073—Sealings
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/28—Moving reactors, e.g. rotary drums
- B01J19/285—Shaking or vibrating reactors; reactions under the influence of low-frequency vibrations or pulsations
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/44—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring increasing the number of carbon atoms by addition reactions, i.e. reactions involving at least one carbon-to-carbon double or triple bond
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a purification device and a purification method for prenol production, and the purification device and the purification method comprise a base, wherein a support column is arranged on the base, a fixed mounting ring is installed at the top of the support column, a purification reaction kettle is installed in the fixed mounting ring, a top cover is arranged at the top of the purification reaction kettle, a sealing strip is arranged on the top cover, a trapezoidal groove is formed in the purification reaction kettle, the top cover is matched with the trapezoidal groove through the sealing strip, a locking mechanism is arranged between the top cover and the reaction kettle, a longitudinal swinging assembly and a circumferential rotating assembly are arranged between the purification reaction kettle and the fixed mounting ring, the top cover and the locking mechanism are sealed, the pressure relief and air replacement discharge operation in the purification process is realized through matching of the pressure relief mechanism and an exhaust mechanism, the purification reaction kettle is stirred through combining the longitudinal swinging assembly and the circumferential rotating assembly, and the reaction efficiency is improved.
Description
Technical Field
The invention relates to the technical field of chemical purification equipment, in particular to a purification device and a purification method for producing isopentenol.
Background
The isopentenol is an important organic fine chemical intermediate, and has wide application in the fields of pesticides, synthetic perfumes and the like. The prenol is colorless liquid, and has a density of 0.85g/cm3 (20 deg.C) and a boiling point of 140.2 deg.C. The isopentenol is mainly used as a basic raw material for producing high-efficiency low-toxicity pesticide pyrethroid and citral series essences and fragrances. The capacity of the global isoamylene alcohol reaches about 10-20 kt/a at present, the BASF company in Germany is located in the Ludwigshafen which is the largest producer of the isoamylene alcohol in the world at present, and China mainly consumes the isoamylene alcohol by about 3kt/a in an import or self-production mode at present. The prenol can be obtained by reacting isobutene with formaldehyde. Adding 95% polyformaldehyde into a stainless steel autoclave, taking disodium hydrogen phosphate as a catalyst, adding tert-butyl alcohol, replacing air in the reactor with nitrogen, then adding isobutene, heating to 200 ℃ under stirring to react for 4 hours, then cooling, discharging and distilling to obtain the 3-methyl-2-butenol, wherein the yield can reach 85%.
Prenol when the preparation, need purify it, reaches the prenol of high-purity, prenol is in the purification in-process, needs several kinds of materials to carry out the mixing reaction and is carrying out distillation purification, and is current at the mixture to the material not enough even, and mixing efficiency is slow, and follow-up separation to the catalyst is comparatively difficult.
Disclosure of Invention
The invention aims to provide a purification device and a purification method for producing isopentenol, which are used for solving the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
the utility model provides a purification device is used in prenol production, the on-line screen storage device comprises a base, be provided with the support column on the base, the fixed mounting ring is installed at the top of support column, install purification reation kettle in the fixed mounting ring, purification reation kettle's top is provided with the top cap, be provided with the sealing strip on the top cap, be provided with the dovetail groove on the purification reation kettle, the top cap passes through mutually supporting between sealing strip and the dovetail groove, be provided with locking mechanism between top cap and the reation kettle, still be provided with pressure relief mechanism and exhaust mechanism on the top cap, be provided with vertical swing subassembly and circumference rotation subassembly between purification reation kettle and the fixed mounting ring.
As a further scheme of the invention: locking mechanism is including setting up the locking handle at top cap central point, locking handle links to each other with the locking lever, the bottom plate is installed to the bottom of locking lever, the locking lever is provided with the locking plate at the upside of bottom plate, the bottom outer lane of locking lever is provided with the locking screw thread, the locking plate passes through the locking screw thread and installs with the locking lever between the screw thread, the edge of locking plate is provided with the cooperation flange, purification reation kettle's inner circle is provided with the locking cooperation piece, be provided with the cooperation groove on the locking cooperation piece, the cooperation flange is mutually supported with the cooperation groove, the bottom in cooperation groove is provided with the locking groove.
As a still further scheme of the invention: the locking mechanism further comprises a sealing assembly, the sealing assembly comprises a first sealing groove formed in the bottom plate, a first sealing ring is fixedly arranged on the locking plate at a position corresponding to the first sealing groove, a second sealing groove is formed in the outer ring position of the locking rod at the upper side of the locking plate, a second sealing ring matched with the second sealing groove is arranged at the bottom of the top cover, and the second sealing ring and the bottom of the top cover are fixedly installed.
As a still further scheme of the invention: the pressure relief mechanism includes the pressure release urceolus, be provided with the air duct on the top cap, the upper end extension of air duct sets up, threaded connection between the outside of air duct upper end and the pressure release urceolus, the outer lane of pressure release urceolus is provided with the hexagonal outer lane, the central axis position in the pressure release urceolus is provided with the pressure release inner tube, evenly be provided with venthole one on the lateral wall of pressure release inner tube, pressure release inner tube and air duct intercommunication, the top of pressure release urceolus is provided with the roof, be provided with the threaded rod on the roof, the end connection of threaded rod has the exhaust handle, the bottom of threaded rod is connected with the cooperation circle, the cooperation circles the side and has cup jointed the shutoff board, be provided with the sealing ring on the inner wall of pressure release urceolus, the threaded rod outer lane between roof and the shutoff board is provided with the top spring, be provided with venthole two on the pressure release urceolus lateral wall of sealing ring upside.
As a still further scheme of the invention: the air outlet is arranged in a downward inclined mode, and a third sealing ring is arranged between the pressure relief outer cylinder and the top plate.
As a still further scheme of the invention: the exhaust mechanism comprises a replacement pipe arranged on the top plate, an internal thread is arranged inside the replacement pipe, an external thread is arranged on the outer ring of the replacement pipe, and a sealing sleeve is installed at the top of the replacement pipe in a matched mode.
As a still further scheme of the invention: purification reation kettle's inside is provided with catalyst storage assembly, catalyst storage assembly is including setting up at the inside catalyst section of thick bamboo of purification reation kettle, the outer lane and the bottom of a catalyst section of thick bamboo evenly are provided with the sieve mesh, the diameter of sieve mesh is less than catalyst particle diameter, the top of a catalyst section of thick bamboo is provided with the go-between, rings have been cup jointed on the go-between, rings pass through fixed connection between jib and the locking plate.
As a still further scheme of the invention: the longitudinal swing assembly comprises an installation column arranged on the side edge of the purification reaction kettle, a swing ball is arranged at the tail end of the installation column, the swing ball is connected with the swing frame, a swing groove is formed in the swing ball, and the swing groove is arranged above and below the swing ball; swing springs are arranged on two sides of the annular gear ring, and the swing frame is fixedly connected with the inner ring of the annular gear ring.
As a still further scheme of the invention: the circumference rotating assembly is including setting up the fixed plate on the fixed mounting ring, be provided with drive gear on the fixed plate, the side of fixed mounting ring is provided with the windowing, drive gear is through windowing and the inboard annular ring gear intermeshing of fixed mounting ring, the inboard lower part of fixed mounting ring is provided with the ball bearing, the bottom of annular ring gear is provided with the bearing groove, the bearing groove is mutually supported with the ball bearing.
A purification method of the purification device for producing the isopentenol comprises the following steps:
s1, injecting 95% polyformaldehyde into a purification reaction kettle, filling disodium phosphate into a catalyst cylinder at the bottom of a locking plate, and locking a top plate and the purification reaction kettle through a locking mechanism;
s2, opening an exhaust mechanism through an exhaust handle, filling nitrogen into the purification reaction kettle by combining a replacement pipe, and replacing air in the purification reaction kettle from the exhaust mechanism;
s3, injecting isobutene into the purification reaction kettle, electrifying the heating strip, heating the purification reaction kettle to 200 ℃, continuing for 4 hours, cooling, discharging and distilling to obtain the prenol.
Compared with the prior art, the invention has the beneficial effects that:
(1) The purification reaction kettle is closed by combining the top cover and the locking mechanism, pressure relief and air replacement discharge operation in the purification process is realized by matching the pressure relief mechanism and the exhaust mechanism, and the purification reaction kettle is driven to longitudinally swing and circumferentially rotate by combining the longitudinal swing assembly and the circumferential rotating assembly, so that the purification reaction kettle is stirred, and the reaction efficiency is improved.
(2) The locking plate is placed in the matching groove of the locking matching block along the matching flange, and the locking plate is rotated, so that the matching flange falls into the locking groove of the locking matching block, the locking handle is rotated at the moment, the locking plate moves towards the top plate, and sealing locking between the top plate and the locking plate is achieved. In order to guarantee the sealing effect, a first sealing groove is formed in the bottom plate, a first sealing ring is arranged on the lower side of the locking plate, a second sealing groove is formed in the upper side of the locking plate, a second sealing ring is arranged on the lower side of the top plate, and when the locking plate and the top plate are close to each other and locked, the sealing reliability among the locking plate, the top plate and the locking column is improved.
(3) Set up the air duct on the top cap, the hexagonal outer lane that combines the setting of pressure release urceolus outer lane makes threaded connection and screw between pressure release urceolus and the air duct, when needs pressure release, rotatory exhaust handle, make the cooperation circle of threaded rod bottom remove downwards, the shutoff board separates under the effect of top tension spring and between the sealing ring, thereby realize that venthole one arrives the pressure release exhaust operation of venthole two, when needs are sealed, rotatory exhaust handle makes the cooperation circle rise, it shifts up to drive the shutoff board, make and mutually support between shutoff board and the sealing ring, thereby accomplish sealed operation. The replacement pipe sets up downwards for in the replacement pipe inserts reaction liquid, to the intraductal nitrogen gas that lets in of replacement, open pressure relief mechanism simultaneously, through the air of upwards exhausting method in with purification reation kettle outwards discharge, avoid the air to influence the reaction process. In order to rapidly separate the catalyst and the product after the reaction is completed, the catalyst particles are received by the catalyst cartridge and separated from the product as the top cover is opened after the reaction is completed.
(4) Purification reation kettle can rock along the swing groove, sets up swing spring in the swing groove, can keep at the horizontality after purification reation kettle stop motion, the ejection of compact operation of being convenient for. The annular gear ring is driven to rotate by combining the driving gear and the annular gear ring, so that the purification reaction kettle rotates around the axis, and the stirring reaction effect is realized.
Drawings
FIG. 1 is a schematic structural diagram of a purification device for producing prenol.
FIG. 2 is a schematic diagram of the internal structure of a purification reaction kettle in a purification device for producing prenol.
FIG. 3 is a schematic view of the installation structure of a catalyst cartridge in a purification apparatus for prenol production.
FIG. 4 is a schematic view of the installation structure of a locking mating block in a purification apparatus for prenol production.
FIG. 5 is a schematic distribution diagram of a locking mechanism, a pressure relief mechanism and an exhaust mechanism in a purification device for producing prenol.
Fig. 6 is an enlarged schematic view of a portion a in fig. 5.
Fig. 7 is an enlarged schematic view of B in fig. 5.
Fig. 8 is an enlarged schematic view of the structure at C in fig. 5.
Fig. 9 is a schematic structural diagram of a longitudinal swinging assembly in a purification device for producing isopentenol.
FIG. 10 is a schematic view showing the construction of a circumferential direction rotating unit in a purification apparatus for producing prenol.
In the figure: 1, a base, 2 support columns, 3 a purification reaction kettle, 4 a top cover, 5 a locking mechanism, 6 a pressure relief mechanism, 7 an exhaust mechanism, 8 mounting columns, 80 swing balls, 9 swing frames, 90 swing grooves, 91 swing springs, 10 fixed mounting rings, 100 ball bearings, 11 annular gear rings, 110 bearing grooves, 12 heating strips, 13 catalyst cylinders, 14 fixed plates, 140 driving gears and 15 discharge pipes; 30 locking matching blocks, 31 locking grooves, 32 matching grooves, 40 locking plates, 41 matching flanges, 50 locking handles, 51 locking rods, 52 bottom plates, 53 locking threads, 54 sealing grooves I, 55 sealing rings I, 56 sealing grooves II, 57 sealing rings II and 58 limiting plates; 60 exhaust handles, 61 threaded rods, 62 air ducts, 63 sealing rings III, 64 pressure relief outer cylinders, 65 hexagonal outer rings, 66 pressure relief inner cylinders, 660 air outlet holes I, 67 sealing rings, 68 matching rings, 69 plugging plates, 610 jacking springs, 611 air outlet holes II and 612 top plates; 70 replacement tubes, 71 internal threads, 72 external threads, 73 sealing sleeves; 130 connecting rings, 131 lifting rings, 132 suspension rods.
Detailed Description
In the description of the present invention, it is to be understood that the terms "longitudinal," "lateral," "upper," "lower," "top," "bottom," "inner," "outer," and the like are used in the orientations and positional relationships indicated in the drawings only for the convenience of description and simplicity of description, and do not indicate or imply that the device or element so indicated must have a particular orientation, be constructed in a particular orientation, and be constructed in a particular manner of operation, and thus are not to be construed as limiting the invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
The technical solution of the present patent will be described in further detail with reference to the following embodiments.
Example 1:
as shown in fig. 1, fig. 3, fig. 4, fig. 5, fig. 6, including base 1, be provided with support column 2 on the base 1, fixed mounting ring 10 is installed at the top of support column 2, install purification reation kettle 3 in the fixed mounting ring 10, purification reation kettle 3's top is provided with top cap 4, be provided with the sealing strip on the top cap 4, be provided with the dovetail groove on the purification reation kettle 3, top cap 4 mutually supports through between sealing strip and the dovetail groove, be provided with locking mechanism 5 between top cap 4 and the reation kettle, still be provided with pressure relief mechanism 6 and exhaust mechanism 7 on the top cap 4, be provided with vertical swing subassembly and circumference rotation subassembly between purification reation kettle 3 and the fixed mounting ring 10.
Specifically, purification reation kettle 3 combines top cap 4 and locking mechanism 5, and is airtight, and the cooperation pressure release mechanism 6 and exhaust mechanism 7 realize the pressure release and the air replacement discharge operation of purification in-process, combine vertical swing subassembly and circumference rotating assembly to carry out vertical swing and circumference rotation drive to purification reation kettle 3 to the realization stirs purification reation kettle 3, promotes reaction efficiency.
As shown in fig. 6, the locking mechanism 5 includes a locking handle 50 disposed at a central portion of the top cover 4, the locking handle 50 is connected to a locking rod 51, a bottom plate 52 is mounted at a bottom end of the locking rod 51, the locking rod 51 is provided with a locking plate 40 on an upper side of the bottom plate 52, a locking thread 53 is disposed on an outer ring of a bottom portion of the locking rod 51, the locking plate 40 is threadedly mounted to the locking rod 51 through the locking thread 53, a fitting flange 41 is disposed on an edge of the locking plate 40, a locking fitting block 30 is disposed on an inner ring of the purification reactor 3, a fitting groove 32 is disposed on the locking fitting block 30, the fitting flange 41 is fitted to the fitting groove 32, and a locking groove 31 is disposed at a bottom portion of the fitting groove 32.
Specifically, the locking plate 40 is placed in the fitting groove 32 of the locking fitting block 30 along the fitting flange 41, and the locking plate 40 is rotated so that the fitting flange 41 falls into the locking groove 31 of the locking fitting block 30, and at this time, the locking handle 50 is rotated so that the locking plate 40 moves toward the top plate 612, thereby achieving the sealed locking between the top plate 612 and the locking plate 40.
As shown in fig. 6, the locking mechanism 5 further includes a sealing assembly, the sealing assembly includes a first sealing groove 54 disposed on the bottom plate 52, the locking plate 40 is fixedly provided with a first sealing ring 55 at a position corresponding to the first sealing groove 54, a second sealing groove 56 is disposed at an outer ring position of the locking rod 51 on the upper side of the locking plate 40, a second sealing ring 57 which is mutually matched with the second sealing groove 56 is disposed at the bottom of the top cover 4, and the second sealing ring 57 is fixedly mounted with the bottom of the top cover 4.
Specifically, in order to ensure the sealing effect, a first sealing groove 54 is formed in the bottom plate 52, a first sealing ring 55 is formed on the lower side of the locking plate 40, a second sealing groove 56 is formed on the upper side of the locking plate 40, and a second sealing ring 57 is formed on the lower side of the top plate 612, so that when the locking plate 40 and the top plate 612 are close to each other and locked, the sealing reliability among the locking plate 40, the top plate 612 and the locking column is provided.
Example 2:
this embodiment combines fig. 7, fig. 8 to give on embodiment 1's basis, pressure relief mechanism 6 includes pressure relief urceolus 64, be provided with air duct 62 on top cap 4, the upper end extension of air duct 62 sets up, threaded connection between the outside of air duct 62 upper end and the pressure relief urceolus 64, the outer lane of pressure relief urceolus 64 is provided with hexagonal outer lane 65, the center axis position in the pressure relief urceolus 64 is provided with pressure relief inner tube 66, evenly be provided with venthole 660 on the lateral wall of pressure relief inner tube 66, pressure relief inner tube 66 and air duct 62 intercommunication, the top of pressure relief urceolus 64 is provided with roof 612, be provided with threaded rod 61 on the roof 612, the end connection of threaded rod 61 has exhaust handle 60, the bottom of threaded rod 61 is connected with cooperation circle 68, cooperation circle 68 upside has cup jointed shutoff board 69, be provided with sealing ring 67 on the inner wall of pressure relief urceolus 64, threaded rod 61 outer lane between roof 612 and shutoff board 69 is provided with a top tension spring 610, be provided with venthole two 611 on the lateral wall of the pressure relief urceolus 64 of sealing ring 67 upside.
Specifically, set up air duct 62 on top cap 4, hexagonal outer lane 65 that combines the setting of pressure release urceolus 64 outer lane makes threaded connection and screw between pressure release urceolus 64 and the air duct 62, when needs pressure release, rotatory exhaust handle 60, make the cooperation circle 68 of threaded rod 61 bottom remove downwards, shutoff board 69 under the effect of top tension spring 610 and the separation between sealing ring 67, thereby realize that venthole one 660 rises to the pressure release exhaust operation of venthole two 611, when needs are sealed, rotatory exhaust handle 60 makes cooperation circle 68 rise, drive shutoff board 69 and shift up, make mutually support between shutoff board 69 and the sealing ring 67, thereby accomplish sealed operation.
The air outlet hole II 611 is arranged in a downward inclining mode, and a sealing ring III 63 is arranged between the pressure relief outer cylinder 64 and the top plate 612.
As shown in fig. 8, the exhaust mechanism 7 includes a displacement tube 70 disposed on a top plate 612, an internal thread 71 is disposed inside the displacement tube 70, an external thread 72 is disposed on an outer ring of the displacement tube 70, and a gland 73 is fittingly mounted on a top of the displacement tube 70.
Specifically, replacement pipe 70 sets up downwards for replacement pipe 70 inserts in the reaction liquid, lets in nitrogen gas in replacement pipe 70, opens pressure relief mechanism 6 simultaneously, outwards discharges the air in purification reation kettle 3 through the method of upwards exhausting air, avoids the air to influence the reaction process.
As shown in fig. 2, a catalyst containing assembly is arranged inside the purification reactor 3, the catalyst containing assembly includes a catalyst cylinder 13 arranged inside the purification reactor 3, the outer ring and the bottom of the catalyst cylinder 13 are uniformly provided with sieve holes, the diameter of each sieve hole is smaller than the diameter of a catalyst particle, the top of the catalyst cylinder 13 is provided with a connecting ring 130, the connecting ring 130 is sleeved with a hanging ring 131, and the hanging ring 131 is fixedly connected with the locking plate 40 through a hanging rod 132.
Specifically, in order to rapidly separate the catalyst and the product after the reaction is completed, the catalyst particles are received by the catalyst cartridge 13 and separated from the product as the top cover 4 is opened after the reaction is completed.
Example 3:
in this embodiment, based on embodiments 1 and 2, with reference to fig. 9 and 10, the longitudinal swing assembly includes an installation column 8 disposed at a side of the purification reactor 3, a swing ball 80 is disposed at a terminal of the installation column 8, the swing ball 80 is connected to the swing frame 9, a swing groove 90 is disposed inside the swing ball 80, and the swing groove 90 is located above and below the swing ball 80; and swing springs 91 are arranged on two sides of the swing frame, and the swing frame 9 is fixedly connected with the inner ring of the annular gear ring 11.
Specifically, purification reation kettle 3 can rock along swing tank 90, sets up swing spring 91 in swing tank 90, can keep at the horizontality after 3 stop motion of purification reation kettle, the ejection of compact operation of being convenient for.
The circumference direction rotating assembly is including setting up the fixed plate 14 on fixed mounting ring 10, be provided with drive gear 140 on the fixed plate 14, the side of fixed mounting ring 10 is provided with the windowing, drive gear 140 is through windowing and the inboard annular ring gear 11 intermeshing of fixed mounting ring 10, the inboard lower part of fixed mounting ring 10 is provided with ball bearing 100, the bottom of annular ring gear 11 is provided with bearing groove 110, bearing groove 110 and ball bearing 100 mutually support.
Specifically, drive gear 140 and annular ring gear 11 are combined, drive annular ring gear 11 and rotate to realize that purification reation kettle 3 rotates around the axis, realize stirring reaction's effect.
A purification method of the purification device for producing the isopentenol comprises the following steps:
s1, injecting 95% polyformaldehyde into a purification reaction kettle 3, filling disodium phosphate into a catalyst cylinder 13 at the bottom of a locking plate 40, and locking a top plate 612 and the purification reaction kettle 3 through a locking mechanism 5;
s2, opening the exhaust mechanism 7 through the exhaust handle 60, filling nitrogen into the purification reaction kettle 3 by combining with the replacement pipe 70, and replacing the air in the purification reaction kettle 3 from the exhaust mechanism 7;
s3, injecting isobutene into the purification reaction kettle 3, electrifying the heating strip 12, heating the purification reaction kettle 3 to 200 ℃, continuing for 4 hours, cooling, discharging and distilling to obtain the prenol.
The working principle of the embodiment of the invention is as follows:
as shown in fig. 1-10, purification reaction kettle 3 combines top cap 4 and locking mechanism 5 to be sealed, cooperates with pressure relief mechanism 6 and exhaust mechanism 7 to realize the pressure relief and air replacement discharge operation in the purification process, and combines with longitudinal swing assembly and circumferential rotation assembly to carry out longitudinal swing and circumferential rotation drive on purification reaction kettle 3, thereby realizing stirring purification reaction kettle 3 and improving reaction efficiency. The locking plate 40 is placed in the fitting groove 32 of the locking fitting block 30 along the fitting flange 41, and the locking plate 40 is rotated so that the fitting flange 41 falls into the locking groove 31 of the locking fitting block 30, at which time the locking handle 50 is rotated so that the locking plate 40 moves toward the top plate 612, thereby achieving the sealed locking between the top plate 612 and the locking plate 40. In order to ensure the sealing effect, a first sealing groove 54 is formed in the bottom plate 52, a first sealing ring 55 is formed on the lower side of the locking plate 40, a second sealing groove 56 is formed on the upper side of the locking plate 40, and a second sealing ring 57 is formed on the lower side of the top plate 612, so that the sealing reliability among the locking plate 40, the top plate 612 and the locking column is provided when the locking plate 40 and the top plate 612 are close to each other and locked. Set up air duct 62 on top cap 4, hexagonal outer lane 65 that combines the setting of pressure release urceolus 64 outer lane makes threaded connection and screw between pressure release urceolus 64 and the air duct 62, when the pressure release is required, rotatory exhaust handle 60, make the cooperation circle 68 of threaded rod 61 bottom remove downwards, shutoff board 69 separates under the effect of top tension spring 610 and between sealing ring 67, thereby realize that venthole one 660 is to the pressure release exhaust operation of venthole two 611, when needs are sealed, rotatory exhaust handle 60 makes cooperation circle 68 rise, drive shutoff board 69 and shift up, make and mutually support between shutoff board 69 and the sealing ring 67, thereby accomplish sealed operation. The replacement pipe 70 is arranged downwards, so that the replacement pipe 70 is inserted into the reaction liquid, nitrogen is introduced into the replacement pipe 70, the pressure relief mechanism 6 is opened at the same time, and air in the purification reaction kettle 3 is discharged outwards by an upward air discharge method, so that the influence of the air on the reaction process is avoided. In order to rapidly separate the catalyst and the product after the reaction is completed, catalyst particles are received by the catalyst cartridge 13 and separated from the product as the top cover 4 is opened after the reaction is completed. Purification reation kettle 3 can rock along swing tank 90, sets up swinging spring 91 in swing tank 90, can keep at the horizontality after purification reation kettle 3 stop motion, the ejection of compact operation of being convenient for. Combine drive gear 140 and ring gear 11, drive ring gear 11 and rotate to realize purification reation kettle 3 and rotate round the axis, realize stirring reaction's effect.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present specification describes embodiments, not every embodiment includes only a single embodiment, and such description is for clarity purposes only, and it is to be understood that all embodiments may be combined as appropriate by one of ordinary skill in the art to form other embodiments as will be apparent to those of skill in the art from the description herein.
Claims (10)
1. The utility model provides a purification device is used in prenol production, includes base (1), be provided with support column (2) on base (1), fixed mounting ring (10) are installed at the top of support column (2), install purification reation kettle (3) in fixed mounting ring (10), a serial communication port, the top of purification reation kettle (3) is provided with top cap (4), be provided with the sealing strip on top cap (4), be provided with the dovetail groove on purification reation kettle (3), top cap (4) are through mutually supporting between sealing strip and the dovetail groove, be provided with locking mechanism (5) between top cap (4) and the reation kettle, still be provided with pressure relief mechanism (6) and exhaust mechanism (7) on top cap (4), be provided with vertical swing subassembly and circumference rotation subassembly between purification reation kettle (3) and the fixed mounting ring (10).
2. The purification device for producing isopentenol, according to claim 1, wherein said locking mechanism (5) comprises a locking handle (50) disposed at the central portion of said top cover (4), said locking handle (50) is connected with a locking rod (51), said bottom plate (52) is installed at the bottom end of said locking rod (51), said locking rod (51) is provided with a locking plate (40) at the upper side of said bottom plate (52), said outer ring of the bottom of said locking rod (51) is provided with a locking thread (53), said locking plate (40) is screw-mounted with said locking rod (51) through said locking thread (53), said edge of said locking plate (40) is provided with a locking flange (41), said inner ring of said purification reaction kettle (3) is provided with a locking fitting block (30), said locking fitting block (30) is provided with a fitting groove (32), said fitting flange (41) is fitted with said fitting groove (32), and said bottom of said fitting groove (32) is provided with a locking groove (31).
3. The purification device for prenol production as claimed in claim 2, wherein the locking mechanism (5) further comprises a sealing assembly, the sealing assembly comprises a first sealing groove (54) formed in the bottom plate (52), a first sealing ring (55) is fixedly arranged on the locking plate (40) at a position corresponding to the first sealing groove (54), a second sealing groove (56) is formed in the locking plate (40) at an outer ring position of the locking rod (51), a second sealing ring (57) which is matched with the second sealing groove (56) is arranged at the bottom of the top cover (4), and the second sealing ring (57) is fixedly arranged with the bottom of the top cover (4).
4. The purifying apparatus for prenol production as recited in claim 1, the pressure relief mechanism (6) comprises a pressure relief outer cylinder (64), the top cover (4) is provided with an air duct (62), the upper end of the air duct (62) is extended, the outer side of the upper end of the air duct (62) is in threaded connection with the pressure relief outer cylinder (64), the outer ring of the pressure relief outer cylinder (64) is provided with a hexagonal outer ring (65), a pressure relief inner cylinder (66) is arranged on the central axis position in the pressure relief outer cylinder (64), the side wall of the pressure relief inner cylinder (66) is uniformly provided with first air outlet holes (660), the pressure relief inner cylinder (66) is communicated with the air duct (62), a top plate (612) is arranged at the top of the pressure relief outer cylinder (64), a threaded rod (61) is arranged on the top plate (612), an exhaust handle (60) is connected with the end part of the threaded rod (61), the bottom end of the threaded rod (61) is connected with a matching ring (68), a plugging plate (69) is sleeved on the upper side of the matching ring (68), a sealing ring (67) is arranged on the inner wall of the pressure relief outer cylinder (64), a jacking spring (610) is arranged on the outer ring of the threaded rod (61) between the top plate (612) and the blocking plate (69), and a second air outlet hole (611) is formed in the side wall of the pressure relief outer cylinder (64) on the upper side of the sealing ring (67).
5. The refining device for the production of isopentenol according to claim 4, wherein the second air outlet (611) is arranged in a downward inclination manner, and a third sealing ring (63) is arranged between the pressure relief outer cylinder (64) and the top plate (612).
6. The purification device for producing isopentenol according to claim 1, wherein said exhaust mechanism (7) comprises a replacement tube (70) disposed on a top plate (612), an internal thread (71) is disposed inside said replacement tube (70), an external thread (72) is disposed on an outer ring of said replacement tube (70), and a sealing sleeve (73) is fittingly mounted on a top portion of said replacement tube (70).
7. The purification device for the production of isopentenol according to claim 1, wherein a catalyst containing assembly is arranged inside the purification reaction kettle (3), the catalyst containing assembly comprises a catalyst cylinder (13) arranged inside the purification reaction kettle (3), sieve holes are uniformly formed in the outer ring and the bottom of the catalyst cylinder (13), the diameter of each sieve hole is smaller than the diameter of a catalyst particle, a connecting ring (130) is arranged at the top of the catalyst cylinder (13), a hanging ring (131) is sleeved on the connecting ring (130), and the hanging ring (131) is fixedly connected with a locking plate (40) through a hanging rod (132).
8. A purifying device for producing isopentenol according to claim 1, wherein the longitudinal swinging component comprises a mounting column (8) arranged at the side of the purifying reaction kettle (3), a swinging ball (80) is arranged at the end of the mounting column (8), the swinging ball (80) is connected with a swinging frame (9), a swinging groove (90) is arranged inside the swinging ball (80), and the swinging groove (90) is arranged above and below the swinging ball (80); swing springs (91) are arranged on two sides of the swing frame, and the swing frame (9) is fixedly connected with the inner ring of the annular gear ring (11).
9. The purification device for the production of isopentenol according to claim 1, wherein the circumferential rotating assembly comprises a fixing plate (14) arranged on a fixed mounting ring (10), a driving gear (140) is arranged on the fixing plate (14), a window is arranged on a side edge of the fixed mounting ring (10), the driving gear (140) is meshed with an annular gear ring (11) on the inner side of the fixed mounting ring (10) through the window, a ball bearing (100) is arranged on the lower portion of the inner side of the fixed mounting ring (10), a bearing groove (110) is arranged at the bottom of the annular gear ring (11), and the bearing groove (110) is matched with the ball bearing (100).
10. A purification method of the purification apparatus for prenol production as claimed in any one of claims 1 to 9, comprising the steps of:
s1, injecting 95% polyformaldehyde into a purification reaction kettle (3), filling disodium phosphate into a catalyst cylinder (13) at the bottom of a locking plate (40), and locking a top plate (612) and the purification reaction kettle (3) through a locking mechanism (5);
s2, opening the exhaust mechanism (7) through an exhaust handle (60), filling nitrogen into the purification reaction kettle (3) in combination with a replacement pipe (70), and replacing air in the purification reaction kettle (3) from the exhaust mechanism (7);
s3, injecting isobutene into the purification reaction kettle (3), electrifying the heating strip (12), heating the purification reaction kettle (3) to 200 ℃, continuing for 4 hours, cooling, discharging and distilling to obtain the prenol.
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