CN115212839B - Purification device and purification method for prenyl alcohol production - Google Patents
Purification device and purification method for prenyl alcohol production Download PDFInfo
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- CN115212839B CN115212839B CN202210947068.5A CN202210947068A CN115212839B CN 115212839 B CN115212839 B CN 115212839B CN 202210947068 A CN202210947068 A CN 202210947068A CN 115212839 B CN115212839 B CN 115212839B
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- 238000000746 purification Methods 0.000 title claims abstract description 99
- ASUAYTHWZCLXAN-UHFFFAOYSA-N prenol Chemical compound CC(C)=CCO ASUAYTHWZCLXAN-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 9
- 238000007789 sealing Methods 0.000 claims abstract description 79
- 238000006243 chemical reaction Methods 0.000 claims abstract description 68
- 230000007246 mechanism Effects 0.000 claims abstract description 50
- 238000007599 discharging Methods 0.000 claims abstract description 9
- 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 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 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
- -1 polyoxymethylene Polymers 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 6
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 6
- 241001330002 Bambuseae Species 0.000 claims description 6
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 6
- 239000011425 bamboo Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000001816 cooling 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
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 3
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 3
- 235000019800 disodium phosphate Nutrition 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 239000001488 sodium phosphate Substances 0.000 claims description 3
- 230000002035 prolonged effect Effects 0.000 claims 1
- 230000000694 effects Effects 0.000 description 8
- 238000010586 diagram Methods 0.000 description 4
- 238000009434 installation Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 239000012295 chemical reaction liquid Substances 0.000 description 3
- 238000006073 displacement reaction Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling 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
- 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
- 230000008676 import Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002728 pyrethroid Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000013599 spices Nutrition 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
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 prenyl alcohol production, wherein the purification device comprises a base, a support column is arranged on the base, a fixed mounting ring is arranged at the top of the support column, a purification reaction kettle is arranged 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 trapezoid groove is arranged on the purification reaction kettle, the top cover is matched with the trapezoid 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, pressure release and air replacement discharging operation in the purification process are realized by combining the longitudinal swinging assembly and the circumferential rotating assembly, and the purification reaction kettle is stirred, so that 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 fragrances and the like. The isopentenol was colorless liquid having a density of 0.85g/cm3 (20 ℃ C.) and a boiling point of 140.2 ℃ C. The isopentenol is mainly used as a basic raw material for producing efficient low-toxicity pesticide pyrethroid and citral series essence and spice. The productivity of the global isopentenol reaches about 10-20 kt/a at present, the German BASF company is located in the ludwigiko factory and is the biggest manufacturer of the isopentenol in the world at present, and the mode of import or self-production and self-use is mainly adopted in China at present to consume the isopentenol about 3kt/a. The isopentenol can be obtained by reacting isobutene with formaldehyde. Adding 95% polyformaldehyde into a stainless steel autoclave, taking disodium hydrogen phosphate as a catalyst, adding tertiary butanol, replacing air in a reactor with nitrogen, adding isobutene, heating to 200 ℃ under stirring for reaction for 4 hours, and cooling, discharging and distilling to obtain 3-methyl-2-butenol, wherein the yield can reach 85%.
When the isopentenol is prepared, the isopentenol needs to be purified to achieve high-purity isopentenol, in the purification process of the isopentenol, several materials are required to be subjected to a mixing reaction for distillation purification, the materials are not uniformly mixed at present, the mixing efficiency is low, and the subsequent separation of the catalyst is difficult.
Disclosure of Invention
The invention aims to provide a purification device and a purification method for producing prenyl alcohol, which are used for solving the problems in the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the utility model provides a purification device is used in prenyl alcohol production, includes the base, be provided with the support column on the base, 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 release mechanism and exhaust mechanism on the top cap, be provided with vertical swing subassembly and circumference rotary assembly between purification reation kettle and the fixed mounting ring.
As a further scheme of the invention: the locking mechanism comprises a locking handle arranged at the center of the top cover, the locking handle is connected with a locking rod, the bottom of the locking rod is provided with a bottom plate, the locking rod is provided with a locking plate on the upper side of the bottom plate, the outer ring of the bottom of the locking rod is provided with locking threads, the locking plate is in threaded installation with the locking rod through the locking threads, the edge of the locking plate is provided with a matching flange, the inner ring of the purification reaction kettle is provided with a locking matching block, the locking matching block is provided with a matching groove, the matching flange is matched with the matching groove, and the bottom of the matching groove is provided with a locking groove.
As still further aspects of the invention: the locking mechanism further comprises a sealing assembly, the sealing assembly comprises a first sealing groove arranged on 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 arranged on the upper side of the locking plate at the outer ring position of the locking rod, a second sealing ring matched with the second sealing groove is arranged at the bottom of the top cover, and the second sealing ring is fixedly arranged between the bottom of the top cover and the bottom of the top cover.
As still further aspects of the invention: the pressure release mechanism comprises a pressure release outer cylinder, be provided with the air duct on the top cap, the upper end extension of air duct sets up, threaded connection between air duct upper end outside and the pressure release outer cylinder, the outer lane of pressure release outer cylinder is provided with the hexagonal outer lane, the central axis position in the pressure release outer cylinder is provided with the pressure release inner cylinder, evenly be provided with venthole one on the lateral wall of pressure release inner cylinder, pressure release inner cylinder and air duct intercommunication, the top of pressure release outer cylinder 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 shutoff board has been cup jointed to the cooperation circle upside, be provided with the sealing ring on the inner wall of pressure release outer cylinder, threaded rod outer lane between roof and the shutoff board is provided with the tight spring in top, be provided with venthole two on the pressure release outer cylinder lateral wall of sealing ring upside.
As still further aspects of the invention: the second air outlet hole is arranged in a downward inclined mode, and a third sealing ring is arranged between the pressure release outer cylinder and the top plate.
As still further aspects of the invention: the exhaust mechanism comprises a replacement pipe arranged on the top plate, an internal thread is arranged in the replacement pipe, an external thread is arranged on the outer ring of the replacement pipe, and a sealing sleeve is arranged at the top of the replacement pipe in a matched mode.
As still further aspects of the invention: the inside of purification reation kettle is provided with the catalyst and accomodates the subassembly, the catalyst is accomodates the subassembly and is including setting up the inside catalyst section of thick bamboo at the purification reation kettle, the outer lane and the bottom of 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 catalyst section of thick bamboo is provided with the go-between, the rings have been cup jointed on the go-between, the rings pass through fixed connection between jib and the locking plate.
As still further aspects of the invention: the longitudinal swinging component comprises a mounting column arranged on the side edge of the purification reaction kettle, the tail end of the mounting column is provided with a swinging ball, the swinging ball is connected with the swinging frame, a swinging groove is formed in the swinging ball, and the swinging groove is arranged above and below the swinging 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 still further aspects of the invention: the circumferential rotating assembly comprises a fixed plate arranged on a fixed mounting ring, a driving gear is arranged on the fixed plate, a window is arranged on the side edge of the fixed mounting ring, the driving gear is meshed with an annular gear ring on the inner side of the fixed mounting ring through the window, a ball bearing is arranged on the lower portion of the inner side of the fixed mounting ring, a bearing groove is formed in the bottom of the annular gear ring, and the bearing groove is matched with the ball bearing.
The purification method of the purification device for producing the prenyl alcohol comprises the following steps:
s1, injecting 95% polyoxymethylene into a purification reaction kettle, containing disodium phosphate in 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 the 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, and then cooling, discharging and distilling to obtain the isopentenol.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the invention, the purification reaction kettle is combined with the top cover and the locking mechanism to seal, the pressure release mechanism and the exhaust mechanism are matched to realize pressure release and air replacement discharge operation in the purification process, and the longitudinal swinging assembly and the circumferential rotating assembly are combined to longitudinally swing and circumferentially rotate the purification reaction kettle, 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, and the locking handle is rotated at the moment, so that the locking plate moves towards the top plate, and sealing and locking between the top plate and the locking plate are realized. In order to guarantee sealing effect, set up sealed recess one on the bottom plate, set up sealing washer one in the downside of locking board simultaneously, the upside of locking board sets up sealed recess two, sets up sealing washer two in the downside of roof, when locking board and roof are close to each other and lock, provides sealing reliability between locking board, roof, the locking post.
(3) Set up the air duct on the top cap, combine the hexagonal outer lane that the outer lane of pressure release urceolus set up to make threaded connection between pressure release urceolus and the air duct and screw, when needs pressure release, rotatory exhaust handle for the cooperation circle of threaded rod bottom reciprocates, and the shutoff board separates between the sealing ring under the effect of tight spring in top, thereby realizes venthole one to venthole two's pressure release exhaust operation, when needs are sealed, rotatory exhaust handle makes the cooperation rise, drives the shutoff board and reciprocates, makes mutually supporting between shutoff board and the sealing ring, thereby accomplishes sealed operation. The displacement tube is downwards arranged, so that the displacement tube is inserted into the reaction liquid, nitrogen is introduced into the displacement tube, the pressure release mechanism is simultaneously opened, and air in the purification reaction kettle is outwards discharged through an upward air discharge method, so that the reaction process is prevented from being influenced by the air. In order to separate the catalyst and the product rapidly after the reaction is finished, the catalyst particles are stored by the catalyst cylinder and separated from the product after the reaction is finished along with the opening of the top cover.
(4) The purification reaction kettle can shake along the swinging groove, and the swinging spring is arranged in the swinging groove, so that the purification reaction kettle can be kept in a horizontal state after stopping moving, and the discharging operation is facilitated. The driving gear and the annular gear ring are combined to drive the annular gear ring to rotate, 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 prenyl alcohols.
FIG. 2 is a schematic diagram of the internal structure of a purification reaction kettle in a purification device for producing prenyl alcohols.
FIG. 3 is a schematic view showing the installation structure of a catalyst cartridge in a purification apparatus for producing prenyl alcohols.
FIG. 4 is a schematic diagram showing the installation structure of a locking matching block in a purifying device for prenyl alcohol production.
Fig. 5 is a schematic distribution diagram of a locking mechanism, a pressure release mechanism and an exhaust mechanism in a purifying device for prenyl alcohol production.
Fig. 6 is an enlarged schematic view of fig. 5 at a.
Fig. 7 is an enlarged schematic view of the structure at B in fig. 5.
Fig. 8 is an enlarged schematic view of fig. 5 at C.
FIG. 9 is a schematic view showing the structure of a longitudinally oscillating assembly in a purifying apparatus for producing prenyl alcohols.
FIG. 10 is a schematic view showing the structure of a circumferential rotating member in a purifying apparatus for producing prenyl alcohols.
In the figure: 1 a base, 2 a support column, 3 a purification reaction kettle, 4 a top cover, 5 a locking mechanism, 6 a pressure relief mechanism, 7 an exhaust mechanism, 8 a mounting column, 80 a swing ball, 9 a swing frame, 90 a swing groove, 91 swinging springs, 10 fixed mounting rings, 100 ball bearings, 11 annular gear rings, 110 bearing grooves, 12 heating strips, 13 catalyst cylinders, 14 fixing plates, 140 driving gears and 15 discharging 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 guide pipes, 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 propping springs, 611 air outlet holes II and 612 top plates; 70 replacement tube, 71 internal thread, 72 external thread, 73 sealing sleeve; 130 connecting ring, 131 hanging ring, 132 hanging rod.
Detailed Description
In the description of the present invention, it should be understood that the terms "longitudinal," "transverse," "upper," "lower," "top," "bottom," "inner," "outer," and the like indicate or are based on the orientation or positional relationship shown in the drawings, merely to facilitate description of the invention and to simplify the description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the invention.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
In the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communicated with the inside of two elements or the interaction relationship of the two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
The technical scheme of the patent is further described in detail below with reference to the specific embodiments.
Example 1:
as shown in fig. 1, fig. 3, fig. 4, fig. 5 and fig. 6, the on-line screen storage device comprises a 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, the top of purification reation kettle 3 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 support 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 release mechanism 6 and exhaust mechanism 7 on the top cap 4, be provided with vertical swing subassembly and circumference rotary assembly between purification reation kettle 3 and the fixed mounting ring 10.
Specifically, purification reation kettle 3 combines top cap 4 and locking mechanism 5, seals, cooperates pressure release mechanism 6 and exhaust mechanism 7 to realize the pressure release and the air replacement discharge operation in the purification process, combines vertical swing subassembly and circumference rotating assembly to carry out vertical swing and circumference rotary drive to purification reation kettle 3 to the realization is stirred purification reation kettle 3, promotes reaction efficiency.
As shown in fig. 6, the locking mechanism 5 comprises a locking handle 50 arranged at the center of the top cover 4, the locking handle 50 is connected with a locking rod 51, a bottom plate 52 is installed at the bottom end of the locking rod 51, a locking plate 40 is arranged on the upper side of the bottom plate 52 by the locking rod 51, a locking thread 53 is arranged on the outer ring of the bottom of the locking rod 51, the locking plate 40 is in threaded installation with the locking rod 51 through the locking thread 53, a matching flange 41 is arranged on the edge of the locking plate 40, a locking matching block 30 is arranged on the inner ring of the purification reaction kettle 3, a matching groove 32 is arranged on the locking matching block 30, the matching flange 41 is matched with the matching groove 32, and a locking groove 31 is arranged at the bottom of the matching groove 32.
Specifically, the locking plate 40 is placed along the fitting flange 41 into the fitting groove 32 of the locking fitting block 30, 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 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, a first sealing ring 55 is fixedly disposed on the locking plate 40 at a position corresponding to the first sealing groove 54, a second sealing groove 56 is disposed on the upper side of the locking plate 40 at an outer ring position of the locking rod 51, a second sealing ring 57 matched with the second sealing groove 56 is disposed on 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 on 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, a second sealing ring 57 is formed on the lower side of the top plate 612, and 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 mutually close to each other for locking.
Example 2:
this embodiment combines fig. 7, 8 to give on the basis of embodiment 1, relief mechanism 6 includes pressure release urceolus 64, be provided with air duct 62 on the top cap 4, the upper end extension of air duct 62 sets up, threaded connection between air duct 62 upper end outside and the pressure release urceolus 64, the outer lane of pressure release urceolus 64 is provided with hexagonal outer lane 65, the central axis position in the pressure release urceolus 64 is provided with pressure release inner tube 66, evenly be provided with venthole one 660 on the lateral wall of pressure release inner tube 66, pressure release inner tube 66 and air duct 62 intercommunication, the top of pressure release urceolus 64 is provided with roof 612, be provided with threaded rod 61 on the roof 612, threaded rod 61's end connection has exhaust handle 60, threaded rod 61's bottom is connected with cooperation circle 68, the shutoff board 69 has been cup jointed to the cooperation circle 68 upside, be provided with sealing ring 67 on the inner wall of pressure release urceolus 64, be provided with top tight spring 610 between roof 612 and the shutoff circle 69 threaded rod 61, be provided with two ventholes 611 on the lateral wall of the urceolus 64 of sealing ring 67 upside.
Specifically, set up air duct 62 on top cap 4, combine the hexagonal outer lane 65 that pressure release urceolus 64 outer lane set up to make between pressure release urceolus 64 and the air duct 62 threaded connection and screw, when needs pressure release, rotatory exhaust handle 60 makes the cooperation circle 68 of threaded rod 61 bottom move downwards, shutoff board 69 separates under the effect of tight spring 610 with sealing ring 67, thereby realize venthole 660 to venthole two 611's pressure release exhaust operation, when needs are sealed, rotatory exhaust handle 60 makes cooperation circle 68 rise, drive shutoff board 69 and moves up, make the cooperation between shutoff board 69 and the sealing ring 67, thereby accomplish sealing operation.
The second air outlet hole 611 is arranged in a downward inclined manner, and a third sealing ring 63 is arranged between the pressure release outer cylinder 64 and the top plate 612.
As shown in fig. 8, the exhaust mechanism 7 includes a displacing pipe 70 disposed on a top plate 612, an internal thread 71 is disposed inside the displacing pipe 70, an external thread 72 is disposed on an outer ring of the displacing pipe 70, and a sealing sleeve 73 is cooperatively mounted on a top of the displacing pipe 70.
Specifically, 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, meanwhile, the pressure release mechanism 6 is opened, and air in the purification reaction kettle 3 is discharged outwards by an upward air discharge method, so that the reaction progress is prevented from being influenced by the air.
As shown in fig. 2, the inside of the purification reaction kettle 3 is provided with a catalyst storage component, the catalyst storage component comprises a catalyst cylinder 13 arranged inside the purification reaction kettle 3, an outer ring and a bottom of the catalyst cylinder 13 are uniformly provided with sieve holes, the diameter of the sieve holes is smaller than the diameter of catalyst particles, 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 a locking plate 40 through a hanging rod 132.
Specifically, in order to separate the catalyst and the product quickly after the end of the reaction, the catalyst particles are stored in the catalyst cartridge 13, and are separated from the product as the top cover 4 is opened after the end of the reaction.
Example 3:
the embodiment is based on embodiment 1 and embodiment 2, and is presented with reference to fig. 9 and 10, the longitudinal swinging component comprises a mounting column 8 arranged at the side edge of the purification reaction kettle 3, the tail end of the mounting column 8 is provided with a swinging ball 80, the swinging ball 80 is connected with a swinging frame 9, a swinging groove 90 is arranged in 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 9, 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 groove 90, sets up swing spring 91 in the swing groove 90, can keep in the horizontality after purification reation kettle 3 stops the motion, the ejection of compact operation of being convenient for.
The circumferential rotating assembly comprises a fixed plate 14 arranged on a fixed mounting ring 10, a driving gear 140 is arranged on the fixed plate 14, a window is arranged on the 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 formed in the bottom of the annular gear ring 11, and the bearing groove 110 is matched with the ball bearing 100.
Specifically, the driving gear 140 and the annular gear ring 11 are combined to drive the annular gear ring 11 to rotate, so that the purification reaction kettle 3 rotates around the axis, and the stirring reaction effect is realized.
The purification method of the purification device for producing the prenyl alcohol comprises the following steps:
s1, injecting 95% polyoxymethylene into the purification reaction kettle 3, containing disodium phosphate in a catalyst cylinder 13 at the bottom of a locking plate 40, and locking a top plate 612 with the purification reaction kettle 3 through a locking mechanism 5;
s2, opening an exhaust mechanism 7 through an exhaust handle 60, and filling nitrogen into the purification reaction kettle 3 by combining a replacement pipe 70 to replace air in the purification reaction kettle 3 from the exhaust mechanism 7;
s3, injecting isobutene into the purification reaction kettle 3, powering on the heating strip 12, heating the purification reaction kettle 3 to 200 ℃ for 4 hours, and then cooling, discharging and distilling to obtain the isopentenol.
The working principle of the embodiment of the invention is as follows:
as shown in fig. 1-10, the purification reaction kettle 3 is combined with the top cover 4 and the locking mechanism 5 to be sealed, the pressure release and the air replacement discharging operation in the purification process are realized by matching the pressure release mechanism 6 and the exhaust mechanism 7, and the purification reaction kettle 3 is longitudinally swung and circumferentially rotationally driven by combining the longitudinal swinging component and the circumferential rotating component, so that the purification reaction kettle 3 is stirred, and the reaction efficiency is improved. The locking plate 40 is placed along the fitting flange 41 into the fitting groove 32 of the locking fitting block 30 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 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, a second sealing ring 57 is formed on the lower side of the top plate 612, and 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 mutually close to each other for locking. The air duct 62 is arranged on the top cover 4, the hexagonal outer ring 65 combined with the outer ring of the pressure relief outer cylinder 64 is used for enabling the pressure relief outer cylinder 64 to be in threaded connection with the air duct 62 and screwed, when pressure relief is needed, the exhaust handle 60 is rotated, the matching ring 68 at the bottom of the threaded rod 61 moves downwards, the plugging plate 69 is separated from the sealing ring 67 under the action of the jacking spring 610, pressure relief and exhaust operation from the first air outlet hole 660 to the second air outlet hole 611 is achieved, when sealing is needed, the exhaust handle 60 is rotated, the matching ring 68 is lifted, the plugging plate 69 is driven to move upwards, the plugging plate 69 and the sealing ring 67 are matched with each other, and sealing operation is completed. 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 release mechanism 6 is opened, and air in the purification reaction kettle 3 is discharged outwards by an upward air discharge method, so that the reaction progress is prevented from being influenced by the air. In order to separate the catalyst and the product rapidly after the end of the reaction, the catalyst particles are stored by the catalyst cartridge 13 and separated from the product as the top cover 4 is opened after the end of the reaction. The purification reaction kettle 3 can shake along the swinging groove 90, and the swinging spring 91 is arranged in the swinging groove 90, so that the purification reaction kettle 3 can be kept in a horizontal state after stopping moving, and the discharging operation is facilitated. The driving gear 140 and the annular gear ring 11 are combined to drive the annular gear ring 11 to rotate, so that the purification reaction kettle 3 rotates around the axis, and the stirring reaction effect is realized.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (7)
1. The utility model provides a purification device is used in prenyl alcohol production, includes base (1), be provided with support column (2) on base (1), fixed collar (10) are installed at the top of support column (2), install purification reation kettle (3) in fixed collar (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 relief mechanism (6) and exhaust mechanism (7) on top cap (4), be provided with vertical swing subassembly and circumference rotary assembly between purification reation kettle (3) and fixed collar (10).
The inside of purification reation kettle (3) is provided with catalyst and accomodates the subassembly, catalyst accomodates the subassembly and includes catalyst section of thick bamboo (13) that set up inside purification reation kettle (3), outer lane and the bottom of catalyst section of thick bamboo (13) evenly are provided with the sieve mesh, the diameter of sieve mesh is less than catalyst particle diameter, the top of catalyst section of thick bamboo (13) is provided with go-between (130), rings (131) have been cup jointed on go-between (130), rings (131) are through fixed connection between jib (132) and locking plate (40); the longitudinal swinging assembly comprises a mounting column (8) arranged at the side edge of the purification reaction kettle (3), the tail end of the mounting column (8) is provided with a swinging ball (80), the swinging ball (80) is connected with a swinging frame (9), a swinging groove (90) is formed in 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 annular gear ring, and the swing frame (9) is fixedly connected with the inner ring of the annular gear ring (11); the circumferential rotating assembly comprises a fixed plate (14) arranged on a fixed mounting ring (10), a driving gear (140) is arranged on the fixed plate (14), a window is formed in the 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 formed in the bottom of the annular gear ring (11), and the bearing groove (110) is matched with the ball bearing (100).
2. The purifying device for prenyl alcohol production according to claim 1, characterized in that the locking mechanism (5) comprises a locking handle (50) arranged at the center of the top cover (4), the locking handle (50) is connected with a locking rod (51), a bottom plate (52) is arranged at the bottom end of the locking rod (51), a locking plate (40) is arranged on the upper side of the bottom plate (52) of the locking rod (51), a locking thread (53) is arranged on the outer ring of the bottom of the locking rod (51), the locking plate (40) is installed with the locking rod (51) through the locking thread (53), a matching flange (41) is arranged at the edge of the locking plate (40), a locking matching block (30) is arranged on the inner ring of the purifying reaction kettle (3), a matching groove (32) is arranged on the locking matching block (30), the matching flange (41) is matched with the matching groove (32), and a locking groove (31) is arranged at the bottom of the matching groove (32).
3. The purifying device for prenyl alcohol production according to claim 2, wherein the locking mechanism (5) further comprises a sealing assembly, the sealing assembly comprises a first sealing groove (54) arranged on 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 arranged on the upper side of the locking plate (40) at the outer ring position of the locking rod (51), a second sealing ring (57) 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 between the bottom of the top cover (4).
4. The purification device for prenyl alcohol production according to claim 1, wherein the pressure release mechanism (6) comprises a pressure release outer cylinder (64), an air duct (62) is arranged on the top cover (4), the upper end of the air duct (62) is prolonged, the outer side of the upper end of the air duct (62) is in threaded connection with the pressure release outer cylinder (64), the outer ring of the pressure release outer cylinder (64) is provided with a hexagonal outer ring (65), the central axis position in the pressure release outer cylinder (64) is provided with a pressure release inner cylinder (66), the side wall of the pressure release inner cylinder (66) is uniformly provided with an air outlet hole I (660), the pressure release inner cylinder (66) is communicated with the air duct (62), the top of the pressure release outer cylinder (64) is provided with a top plate (612), the top plate (612) is provided with a threaded rod (61), the end of the air duct (61) is connected with an exhaust handle (60), the bottom end of the threaded rod (61) is connected with a matching ring (68), the upper side of the matching ring (68) is sleeved with a plate (69), the side of the inner wall of the outer cylinder (64) is uniformly provided with an air outlet hole I (660), the top plate (612) is communicated with the top plate (610), and a second air outlet hole (611) is formed in the side wall of the pressure release outer cylinder (64) at the upper side of the sealing ring (67).
5. The purifying device for prenyl alcohol production according to claim 4, wherein the second air outlet hole (611) is provided obliquely downward, and a third sealing ring (63) is provided between the pressure release outer cylinder (64) and the top plate (612).
6. The purifying device for prenyl alcohol production according to claim 1, characterized in that the exhaust mechanism (7) comprises a replacement tube (70) arranged on a top plate (612), an internal thread (71) is arranged inside the replacement tube (70), an external thread (72) is arranged on the outer ring of the replacement tube (70), and a sealing sleeve (73) is mounted on the top of the replacement tube (70) in a matched manner.
7. A purification method using the purification apparatus for prenol production according to any one of claims 1 to 6, characterized by comprising the steps of:
s1, injecting 95% polyoxymethylene into a purification reaction kettle (3), containing disodium phosphate in 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 an exhaust mechanism (7) through an exhaust handle (60), and filling nitrogen into the purification reaction kettle (3) by combining a replacement pipe (70) to replace 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 ℃ for 4 hours, and then cooling, discharging and distilling to obtain the isopentenol.
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