CN117427572A - Reactor for large-scale continuous production of PVB and continuous production method - Google Patents
Reactor for large-scale continuous production of PVB and continuous production method Download PDFInfo
- Publication number
- CN117427572A CN117427572A CN202311180250.3A CN202311180250A CN117427572A CN 117427572 A CN117427572 A CN 117427572A CN 202311180250 A CN202311180250 A CN 202311180250A CN 117427572 A CN117427572 A CN 117427572A
- Authority
- CN
- China
- Prior art keywords
- reaction
- gallery
- heat preservation
- temperature control
- corridor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000010924 continuous production Methods 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 216
- 238000004321 preservation Methods 0.000 claims abstract description 137
- 238000003756 stirring Methods 0.000 claims abstract description 42
- 239000007853 buffer solution Substances 0.000 claims abstract description 24
- 239000011347 resin Substances 0.000 claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- 229920005989 resin Polymers 0.000 claims abstract description 14
- 238000007599 discharging Methods 0.000 claims abstract description 13
- 230000000694 effects Effects 0.000 claims abstract description 3
- 239000012429 reaction media Substances 0.000 claims description 77
- 239000002994 raw material Substances 0.000 claims description 37
- 238000002156 mixing Methods 0.000 claims description 29
- 239000002245 particle Substances 0.000 claims description 29
- 238000005452 bending Methods 0.000 claims description 25
- 239000007788 liquid Substances 0.000 claims description 18
- 238000005273 aeration Methods 0.000 claims description 17
- 239000000047 product Substances 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 13
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 claims description 12
- 230000006872 improvement Effects 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 9
- 230000035484 reaction time Effects 0.000 claims description 9
- 230000009471 action Effects 0.000 claims description 7
- 238000011010 flushing procedure Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000003377 acid catalyst Substances 0.000 claims description 4
- 230000014759 maintenance of location Effects 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 230000001502 supplementing effect Effects 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 150000002373 hemiacetals Chemical class 0.000 claims description 3
- 230000003472 neutralizing effect Effects 0.000 claims description 3
- 230000036632 reaction speed Effects 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 239000013589 supplement Substances 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 2
- 239000012530 fluid Substances 0.000 claims description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 43
- 239000004372 Polyvinyl alcohol Substances 0.000 description 21
- 229920002451 polyvinyl alcohol Polymers 0.000 description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 239000002131 composite material Substances 0.000 description 6
- 238000007790 scraping Methods 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 239000005543 nano-size silicon particle Substances 0.000 description 4
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 239000010410 layer Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 210000003298 dental enamel Anatomy 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000005336 safety glass Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
-
- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/087—Heating or cooling the reactor
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F16/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical
- C08F16/02—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical by an alcohol radical
- C08F16/04—Acyclic compounds
- C08F16/06—Polyvinyl alcohol ; Vinyl alcohol
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/01—Processes of polymerisation characterised by special features of the polymerisation apparatus used
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/28—Condensation with aldehydes or ketones
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention provides a reactor for large-scale continuous production of PVB and a continuous production method, which comprises a reactor and a control system and is characterized in that: the reactor is a multi-gallery reactor and comprises a feeding system, a multi-stage temperature control buffer system, a multi-stage heat preservation reaction system, a plug flow stirring system, a bend stirring system, a gas viscosity removing system, a temperature control system and a discharging system which are controlled by a control system. The feeding system is connected with the multi-stage temperature control buffer system, the multi-stage temperature control buffer system is connected with the multi-stage heat preservation reaction system in a crossing way through the bend stirring system, each temperature control gallery is connected with each heat preservation reaction gallery in a multi-stage series connection mode to form a plurality of roundabout turning galleries, the temperature control galleries and the heat preservation reaction galleries are internally provided with the plug flow stirring system and the temperature control system, and the gas viscosity removing system adopts the impact effect of high-speed flowing gas to remove viscosity. The continuous production method can realize the continuous production of PVB, and reduces the resin wall sticking and the loss to the reactor wall in the production process.
Description
Technical Field
The invention belongs to the technical field of chemical production equipment, relates to improvement of PVB production technology, and in particular relates to a reactor for large-scale continuous production of PVB and a continuous production method.
Background
Polyvinyl butyral (PVB) resins are polymeric compounds that are synthesized catalytically from polyvinyl alcohol (PVA) and n-butyraldehyde in the presence of an acid catalyst, and which are in the form of white or pale yellow flowable powders or granules. PVB resins of different properties determine their suitable context, and high viscosity PVB resins are processed into PVB films, which are used as interlayers for safety glass interlayers, with their high viscosity properties to fix the glass in its intact form to the film surface. PVB resins of other properties are widely used in coating adhesives, ceramic decals, aluminum foil papers, and the like.
PVB is generally produced in a specific reactor or reactor, and is formed into a vortex in the reactor or reactor by adjusting the temperature, stirring speed, or the like.
At present, the stirring method is that after PVA and n-butyraldehyde react, the PVA and n-butyraldehyde start to be separated out in a solvent through different treatment processes, and certain external force interference needs to be applied in a separation stage, so that PVB is prevented from being separated out and adhered to form a block, and the subsequent treatment is not facilitated.
Chinese patent (application number 202021574543.1) discloses a closed enamel reactor for inorganic nano-modified PVB resin powder, which adopts a closed enamel reactor, wherein a filter screen type stirring blade in the reactor can reduce the possibility of caking in the reaction medium, but for part of resin, possibly due to vortex formed by stirring, the edge of the vortex is adhered to the inner surface of the reactor, and then separated out, the part of resin can be driven to fall into a solution due to less formation amount without contacting with the stirring blade, and the production quality of the subsequent PVB can be affected along with gradual accumulation.
Chinese patent (application number: 202020053572.7) discloses a high-speed mixing device for PVB raw materials, which adopts a mode of stirring and uniformly mixing PVB raw materials at an ultra-high speed, but along with the increase of stirring rate, raw material foam generated in the stirring process may be spread over the whole tank body, so that PVB is also partially separated out on the tank body and is difficult to reenter solution.
Chinese patent (application number: 202120036931.2) discloses an anti-sticking scraping plate of a reaction kettle, which is used for scraping and removing substances possibly adhered to the inner wall of the reaction kettle by an external magnetic adsorption device to adsorb a scraping knife inside the reaction kettle.
Chinese patent (application number: 202110842040.0) discloses a reaction kettle with anti-adhesion function for non-finished petroleum production, which scrapes off raw materials adhered to the inner wall of the reaction kettle in the stirring process in a mode of internally arranging a mechanical scraping plate, so that the raw materials are prevented from adhering to the inner wall. Although the two measures can solve the problem of raw material sticking to the wall, the use of the mechanical mechanism can generate certain loss on the inner wall of the reaction kettle.
At present, most of existing reaction devices related to PVB preparation are reaction kettles or other similar reactors and improved equipment, different raw materials are added at different stages, and meanwhile, certain external force influence (such as stirring and the like) is applied in the whole process to reduce agglomeration of resin in the reaction process. At present, in the PVB production process, an integrated reactor is adopted to complete the reaction, and equipment and production technology for large-scale PVB production are less disclosed.
Therefore, how to design a reactor for large-scale continuous production of PVB and a continuous production method can realize continuous production of PVB, and resin wall sticking and loss to the reactor wall are reduced in the production process. This is a technical problem to be solved in the art.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and provides a reactor for large-scale continuous production of PVB and a continuous production method thereof, which can realize continuous production of PVB and reduce resin wall sticking and loss on the reactor wall in the production process.
The invention aims at realizing the following technical scheme:
the utility model provides a PVB large-scale continuous production's reactor, includes reactor and control system, its characterized in that, the reactor be many corridor reactor, many corridor reactor include by control system control's feed system, multistage accuse temperature buffer system, multistage heat preservation reaction system, plug flow mixing system, bend mixing system, gas removes gluey system, accuse temperature system and ejection of compact system, feed system with multistage accuse temperature buffer system meets, multistage accuse temperature buffer system with multistage heat preservation reaction system passes through bend mixing system cross connection, with each accuse temperature corridor in the multistage accuse temperature buffer system with each heat preservation reaction corridor in the multistage heat preservation reaction system connects and forms the many corridor of roundabout turn, each accuse temperature corridor and each heat preservation reaction corridor are inside all to be equipped with plug flow mixing system, each accuse temperature corridor and each heat preservation reaction corridor's bottom all is equipped with accuse temperature system, gas removes gluey system including setting up on accuse Wen Langdao inner wall and each heat preservation reaction corridor is used for preventing through the high-speed aeration high-pressure aeration effect with a plurality of external air vent.
The improvement of the technical scheme is as follows: the feeding system comprises a primary feeding hole and at least 4 secondary feeding holes, wherein a feeding auxiliary flow pushing device is arranged below the primary feeding hole, the discharging system comprises a large bending gallery and a discharging hole, a screen is arranged on the large bending gallery, a coarse product collecting box is arranged at the position close to the discharging hole, the large bending gallery is C-shaped, one end of the large bending gallery is connected with one end of the primary feeding hole arranged in the temperature control gallery in the multi-stage temperature control buffer system, the other end of the large bending gallery is connected with the last outlet end of the reaction gallery in the multi-stage heat preservation reaction system, and the inside of the large bending gallery at least comprises 3 flow pushing devices used for pushing products after the reaction to the discharging hole through the large bending gallery.
Further improvement of the technical scheme is as follows: the plug flow stirring system comprises plug flow stirrers arranged in the temperature control corridor and the heat preservation reaction corridor, at least three-stage plug flow is arranged in each temperature control corridor and each heat preservation reaction corridor, each stage of plug flow comprises two plug flow stirrers arranged at the bottom, and each plug flow stirrer is provided with three plug flow stirring paddles for improving the mixing efficiency of raw materials at different positions in a reaction medium and controlling the plug flow velocity accurately and stably.
Further improvement of the technical scheme is as follows: the bend stirring system comprises at least 7 bend stirring areas, each bend stirring area comprises two spiral stirrers, and the full mixing of the reaction raw materials at each stage above and the flow direction control of the liquid medium in the multi-gallery reactor are realized through the alternate coordination control of the two spiral stirrers.
Further improvement of the technical scheme is as follows: the temperature control corridor in the multi-stage temperature control buffer system comprises a first-stage temperature control corridor, a second-stage temperature control corridor Wen Langdao, a third-stage temperature control corridor and a fourth-stage temperature control corridor, wherein the temperature control system arranged on the inner side wall and the bottom of each temperature control corridor comprises a high-power heat exchange tube, temperature directional control is realized on each temperature control corridor through liquid with different temperatures in the high-power heat exchange tube, and a plurality of plug flow stirrers are arranged in each temperature control corridor and are used for realizing effective mixing and flow rate control of reaction raw materials; the heat preservation reaction corridor in the multistage heat preservation reaction system comprises a first-stage heat preservation reaction corridor, a second-stage heat preservation reaction corridor, a third-stage heat preservation reaction corridor and a fourth-stage heat preservation reaction corridor, the temperature control system configured on the inner side wall and the bottom of each heat preservation reaction corridor comprises a low-power heat exchange tube for supplementing heat loss, the temperature control system configured on the inner side wall of each heat preservation reaction corridor comprises a heat preservation layer for preserving heat of liquid in the heat preservation reaction corridor, and the control of reaction time is realized through the flow velocity control of a plurality of plug flow stirrers in the heat preservation reaction corridor.
Further improvement of the technical scheme is as follows: the primary feed inlet of the feed system is positioned at the feed end of the primary control Wen Langdao, the connection turning part of the temperature control gallery and the heat preservation reaction gallery realizes the flow direction conversion of the reaction medium through a spiral stirrer, and the secondary feed inlet is arranged above the spiral stirrer.
Further improvement of the technical scheme is as follows: the spiral stirrer adopts a multi-section annular spiral stirrer, so that the change of the flow speed and the flow quantity of the reaction medium is realized, the compact layout of the whole reactor is realized, and the space is saved.
The invention relates to a continuous production method of a reactor for large-scale continuous production of PVB, which is characterized by comprising the following steps:
adding the primary raw material PVA and different reaction raw materials in each intermediate reaction stage into a temperature control gallery and a heat preservation reaction gallery in a multi-gallery reactor from each stage of feed inlets in a feed system, and realizing effective mixing and flow rate control of the reaction raw materials by matching a plug flow stirring system with a bend stirring system; the temperature control system controls the temperature in the temperature control gallery and the heat preservation reaction gallery so as to ensure that the reaction raw materials react at a proper reaction speed and reaction time, PVA resin separated out in the reaction process is partially adhered on the inner walls of the temperature control gallery and the heat preservation reaction gallery, air is blown into a plurality of aeration holes on the inner wall of the temperature control Wen Langdao and the inner wall of the heat preservation reaction gallery by an external high-pressure fan in the air viscosity removing system, and the viscosity removing is realized by the impact of the high-speed flowing air on the inner walls of the temperature control gallery and the heat preservation reaction gallery; and (3) the PVB particles prepared after the reaction is finished are sent out from a discharge hole by a discharge system and are collected for standby, so that the large-scale continuous production of PVB is finished.
The improvement of the technical scheme is as follows: the continuous production method comprises the following specific steps of:
step 1: adding each temperature control gallery and each heat preservation reaction gallery in the multi-gallery reactor
Introducing a reaction medium;
step 2: adding primary raw material PVA from a primary feed inlet of a feed system, driving the PVA to flow along with a reaction medium through a plug flow stirrer below the primary feed inlet, raising the temperature of the reaction medium to at least 95 ℃ in a primary control Wen Langdao through the heat of high-power heat exchange pipes arranged at the bottom and the side wall, realizing flow rate control by controlling the power of the plug flow stirrer, further controlling the hydraulic retention time to reach the time required by PVA dissolution, and completely dissolving the primary raw material PVA when the primary raw material PVA reaches a spiral stirrer at a joint turning part of a primary temperature control gallery and a primary heat preservation reaction gallery;
step 3: adding nano modified materials into a secondary feed inlet above a spiral stirrer at the joint turning part of the primary temperature control gallery and the primary heat preservation reaction gallery, and primarily mixing PVA with the temperature reaching A ℃ in the primary heat preservation reaction gallery, wherein small functional heat exchange pipes arranged at the bottom and the side wall can supplement less heat lost in the flowing process, and the nano modified materials are fully mixed when reaching the tail end of the primary heat preservation reaction gallery along with the operation of the plug flow stirrer; the temperature range of A is: 90-105 ℃;
step 4: the flow direction and the flow speed are changed through a spiral stirrer at the joint turning part of the first-stage heat-preserving reaction gallery 4 and the second-stage temperature-controlling gallery, the reaction medium enters the second-stage temperature-controlling gallery, the continuous flow of the reaction medium is realized through an internal multi-stage plug flow stirrer, the reaction medium is rapidly cooled by using high-power heat exchange pipes arranged at the bottom and the side wall, and the temperature of the reaction medium is reduced to B ℃ when the reaction medium reaches the tail end; the temperature range of B is as follows: 15-30 ℃;
step 5: the flow speed and the flow direction of the reaction medium are changed through a spiral stirrer at the joint turning part of the secondary temperature control gallery and the secondary heat preservation reaction gallery, n-butyraldehyde is added through a secondary charging port above, the reaction medium is mixed in the secondary heat preservation reaction gallery, the reaction medium is basically uniformly mixed when reaching the spiral stirrer at the joint turning part of the secondary heat preservation reaction gallery and the tertiary temperature control gallery, and then the flow speed and the flow direction of the reaction medium are changed through the spiral stirrer at the joint;
step 6: in the three-stage temperature control reaction corridor, the reaction medium is quickly cooled to C ℃ through the inner wall and the low-power heat exchange pipes arranged at the bottom, the flow speed and the flow direction of the reaction medium are changed under the action of the spiral stirrer at the joint turning part of the three-stage temperature control reaction corridor 7 and the three-stage heat preservation reaction corridor, meanwhile, an acid catalyst required by the reaction is added at the upper secondary feed port, the hemiacetal reaction is carried out in the three-stage heat preservation reaction corridor, at the moment, the viscosity of the reaction medium is increased, part of particles are separated out in the reaction medium, the reaction medium at the liquid level contacts with the inner wall of the three-stage heat preservation reaction corridor and begins to adhere to the inner wall of the three-stage heat preservation reaction corridor, an external high-pressure fan in the gas viscosity removing system blows out high-speed airflow to an aeration hole on the inner wall of the three-stage heat preservation reaction corridor, solid particles adhered to the inner wall of the three-stage heat preservation reaction corridor are blown back to the reaction medium, the particles are scattered under the action of the push stirrer, and the particle size is reduced, and the particle size continues to flow along with the reaction medium; the time required for the reaction is completed when the reaction reaches the spiral stirrer of the joint turning part of the three-stage heat preservation reaction gallery and the four-stage temperature control gallery; the temperature range of C is-5-30 ℃;
step 7: heating the reaction medium to D ℃ in the four-stage temperature control gallery by using a high-power heat exchange tube, forming PVB particles more and more, generating solid particles at the interface, blowing the solid particles back to the reaction medium by using an aeration hole, continuously entering a spiral stirrer at the joint turning part of the four-stage temperature control gallery and the four-stage heat preservation reaction gallery, and adding other neutralizing substances to realize system neutrality; the temperature range of D is: 30-80 ℃;
step 8: and (3) carrying out final heat preservation in the four-stage heat preservation reaction gallery, and simultaneously, carrying out coarse flushing on the product PVB by using external water flow, wherein the final product flows back to the reaction medium, the product and the flushing fluid through the large-bending gallery, and liquid and solid separation is realized by using a screen at a discharge port, so that the obtained PVB particles are collected into a coarse product collecting box to wait for further treatment.
Further, the nano modified material comprises nano titanium dioxide, nano silicon dioxide, nano aluminum oxide, nano zinc oxide, nano aluminum oxide and modified composite materials thereof; preferably, the nano titanium dioxide composite modified material or the nano silicon dioxide composite modified material. In addition, the reaction medium is usually water.
The invention has the advantages and positive effects that:
1. compared with the prior equipment used in the PVB production process, the invention has larger difference, and most of the prior reactors are integrated reactors, and the improvement and improvement of the PVB production and other processes are realized by carrying out various reformation and innovation on the internal structure of the tank body. The invention adopts a large-scale multi-gallery reactor and adopts a mode of multistage serial connection and combination connection, so that different reactions can be realized in different reaction temperature sections when the reaction raw materials flow through the whole reaction gallery, and finally, the reaction products are collected and used at a discharge port.
2. The invention realizes a large-scale PVB continuous production process, namely, the PVB product is directly collected at an outlet by feeding at one side of a feed inlet and realizing specific hydraulic retention time, namely, reaction time by utilizing the cooperation of the length of a gallery and the flow velocity in the gallery.
3. The invention also adopts an innovative viscosity-removing method for the problem of sticking the wall of the product or intermediate product possibly occurring in the raw material production process, the inner wall of the gallery is highly provided with the aeration holes for unidirectional air inlet, and the high-speed air flow generated by the external high-pressure fan is used for removing the viscosity of the gas on the resin stuck on the wall, so that compared with the physical scraping and viscosity removing in the prior art, the physical friction loss of the wall of the reactor is reduced, and the like.
Drawings
Fig. 1 is a top view of a multiple gallery reactor for large scale continuous production of PVB in accordance with the present invention;
fig. 2 is a cross-sectional view taken along A-A of fig. 1.
The numbers in the figures are: 1. a primary feed inlet; 2. a primary control Wen Langdao; 3. a helical agitator; 4. a first-stage heat-preserving reaction gallery; 5. a secondary control Wen Langdao; 6. a secondary heat preservation reaction gallery; 7. three-stage control Wen Langdao; 8. three-stage heat-preserving reaction galleries; 9. a heat preservation layer; 10. a high-power heat exchange tube; 11. a plug flow stirrer; 12. a fourth-level heat-preservation reaction gallery; 13. four-stage control Wen Langdao; 14. a large bending gallery; 15. a screen; 16. a crude product collection box; 17. a secondary feed port; 18. a low-power heat exchange tube; 19. and (5) exposing the pores.
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings:
referring to fig. 1 and 2, an embodiment of a multi-gallery reactor for large-scale continuous production of PVB according to the present invention includes a reactor and a control system, wherein the reactor is a multi-gallery reactor, and the multi-gallery reactor includes a feeding system, a multi-stage temperature-control buffer system, a multi-stage thermal-insulation reaction system, a plug flow stirring system, a bend stirring system, a gas viscosity removing system, a temperature control system, and a discharging system controlled by the control system. The feeding system is connected with the multi-stage temperature control buffer system, the multi-stage temperature control buffer system is connected with the multi-stage heat preservation reaction system in a crossing manner through the bend stirring system, each temperature control gallery in the multi-stage temperature control buffer system is connected with each heat preservation reaction gallery in the multi-stage heat preservation reaction system in a multi-stage series manner to form a plurality of roundabout turning galleries, each temperature control gallery and each heat preservation reaction gallery are internally provided with the plug flow stirring system, the bottoms of each temperature control gallery and each heat preservation reaction gallery are respectively provided with the temperature control system, the gas viscosity removing system comprises a plurality of aeration holes 19 arranged on the inner wall of each temperature control Wen Langdao and the inner wall of each heat preservation reaction gallery and an external high-pressure fan connected with each aeration hole 19 through a pipeline, and is used for removing viscosity by adopting the impact action of high-speed flowing gas, and a one-way valve is arranged in the pipeline connected with the aeration holes 19 and used for preventing reaction medium from flowing backwards.
Further, the feeding system comprises a primary feeding hole 1 and at least 4 secondary feeding holes 19, and a feeding auxiliary impeller is arranged below the primary feeding hole 1. The discharging system comprises a large-bending gallery 14 and a discharging hole, wherein the discharging hole is formed in the large-bending gallery 14, a screen 15 is arranged on the discharging hole, and a coarse product collecting box 16 is arranged close to the discharging hole. The large bending gallery 14 is C-shaped, one end of the large bending gallery 14 is connected with one end of the primary feed inlet 1 arranged in the temperature control gallery in the multi-stage temperature control buffer system, the other end of the large bending gallery 14 is connected with the last outlet end of the heat preservation reaction gallery in the multi-stage heat preservation reaction system, and the inside of the large bending gallery 14 at least comprises 3 plug flow stirrers 11 for pushing the reacted product to the discharge port through the large bending gallery 14.
Still further, above-mentioned plug flow mixing system is including setting up control temperature corridor with the plug flow agitator 11 in the heat preservation reaction corridor, every control temperature corridor with every be equipped with at least tertiary plug flow in the heat preservation reaction corridor, every one-level plug flow includes two plug flow agitators 11 that set up in the bottom, is equipped with three plug flow stirring rake on every plug flow agitator 11 for realize the raw materials mixing efficiency improvement and the plug flow velocity control of different positions in the reaction medium accurate stability.
Still further, above-mentioned bend stirring system includes 7 at least bend stirring district, and including two spiral agitator 3 in every bend stirring district, through the alternate cooperation control of two spiral agitator 3, realizes the intensive mixing of the reaction raw materials of each stage above and the liquid medium flow direction control in the many corridor reactor.
Specifically: the temperature control corridor in the multi-stage temperature control buffer system comprises a first-stage temperature control corridor 2, a second-stage temperature control corridor 5, a third-stage temperature control corridor 7 and a fourth-stage temperature control corridor Wen Langdao and the temperature control system configured on the inner bottoms and the side walls of each control Wen Langdao (2, 5, 7 and 13) comprises a high-power heat exchange tube 10, temperature orientation control is realized on each temperature control corridor through liquid with different temperatures in the high-power heat exchange tube 10, and a plurality of plug flow stirrers 11 are arranged in each control Wen Langdao (2, 5, 7 and 13) and are used for realizing effective mixing and flow rate control of reaction raw materials. The heat-insulating reaction corridor in the multi-stage heat-insulating reaction system comprises a first-stage heat-insulating reaction corridor 4, a second-stage heat-insulating reaction corridor 6, a third-stage heat-insulating reaction corridor 8 and a fourth-stage heat-insulating reaction corridor 12, the temperature control system configured at the bottom and the side wall of each heat-insulating reaction corridor (4, 6, 8 and 12) comprises a low-power heat exchange tube 18 for supplementing heat loss, the temperature control system configured at the inner side wall of each heat-insulating reaction corridor (4, 6, 8 and 12) comprises a heat-insulating layer 9 for insulating liquid in the heat-insulating reaction corridor (4, 6, 8 and 12), and the control of the reaction time is realized through the flow speed control of a plurality of push flow stirrers 11 in the heat-insulating reaction corridor (4, 6, 8 and 12).
Further, the primary feed inlet 1 of the feed system is located at the feed end of the primary temperature control gallery 2, and the connection turning parts of the adjacent control Wen Langdao (2, 5, 7, 13) and the heat insulation reaction galleries (4, 6, 8, 12) realize the flow direction conversion of the reaction medium through the spiral stirrer 3, and the secondary feed inlet 17 is arranged above the spiral stirrer 3.
Preferably, the spiral stirrer 3 adopts a multi-section annular spiral stirrer, so that the change of the flow speed and the flow rate of the reaction medium is realized, the compact layout of the whole multi-gallery reactor is realized, and the space is saved.
The invention relates to a specific embodiment of a continuous production method of a reactor for the large-scale continuous production of PVB, which comprises the following steps:
adding the primary raw material PVA and different reaction raw materials in each intermediate reaction stage into a temperature control gallery and a heat preservation reaction gallery in a multi-gallery reactor from each stage of feed inlets in a feed system, and realizing effective mixing and flow rate control of the reaction raw materials by matching a plug flow stirring system with a bend stirring system; the temperature control system controls the temperature in the temperature control gallery and the heat preservation reaction gallery so as to ensure that the reaction raw materials react at a proper reaction speed and reaction time, PVA resin separated out in the reaction process is partially adhered on the inner walls of the temperature control gallery and the heat preservation reaction gallery, air is blown into a plurality of aeration holes 19 on the inner wall of the temperature control Wen Langdao and the inner wall of the heat preservation reaction gallery by an external high-pressure fan in the air viscosity removing system, and the viscosity removing is realized by the impact of the high-speed flowing air on the inner walls of the temperature control gallery and the heat preservation reaction gallery; and (3) the PVB particles prepared after the reaction is finished are sent out from a discharge hole by a discharge system and are collected for standby, so that the large-scale continuous production of PVB is finished.
Referring to fig. 1 and 2, in an embodiment of a continuous production method of the reactor for large-scale continuous production of PVB, a control system controls operations of a feeding system, a multi-stage temperature control buffer system, a multi-stage thermal insulation reaction system, a plug flow stirring system, a bend stirring system, a gas viscosity removing system, a temperature control system and a discharging system, and the continuous production method comprises the following specific steps:
step 1: adding each temperature control gallery and each heat preservation reaction gallery in the multi-gallery reactor
Introducing a reaction medium;
step 2: adding primary raw material PVA from a primary feed inlet 1 of a feed system, driving the PVA to flow along with a reaction medium through a plug flow stirrer 11 below the primary feed inlet 1, raising the temperature of the reaction medium to at least 95 ℃ in a primary temperature control gallery 2 through the heat of a high-power heat exchange tube 10 arranged at the bottom and the side wall, controlling the power of the plug flow stirrer 11 to realize flow rate control, further controlling the time required by hydraulic retention time to dissolve the PVA, and completely dissolving the PVA when the PVA reaches a spiral stirrer at the joint turning part of the primary temperature control gallery 2 and the primary heat preservation reaction gallery 4;
step 3: adding nano modified materials into a secondary feed inlet 17 above a spiral stirrer 3 at the joint turning part of a primary temperature control gallery 2 and a primary heat preservation reaction gallery 4, and primarily mixing PVA which has reached A ℃ in the primary heat preservation reaction gallery 4, wherein small functional heat exchange pipes 18 arranged at the bottom and the side wall can supplement less heat lost in the flowing process, and along with the operation of a plug flow stirrer 11, the sufficient mixing with the nano modified materials is basically realized when the PVA reaches the tail end of the primary heat preservation reaction gallery 4; the temperature range of A is: 90-105 ℃;
step 4: the flow direction and the flow speed are changed through the spiral stirrer 3 of the joint turning part of the first-stage heat-preservation reaction gallery 4 and the second-stage control Wen Langdao, the reaction medium enters the second-stage heat-control gallery 5, the continuous flow of the reaction medium is realized through the internal multi-stage plug flow stirrer 11, the reaction medium is rapidly cooled by using the high-power heat exchange tubes 10 arranged at the bottom and the side wall, and the temperature of the reaction medium is reduced to B ℃ when the reaction medium reaches the tail end; the temperature range of B is as follows: 15-30 ℃;
step 5: the flow speed and the flow direction of the reaction medium are changed through the spiral stirrer 3 of the connection turning part of the secondary temperature control gallery 5 and the secondary heat preservation reaction gallery 6, n-butyraldehyde is added through the upper secondary feed inlet 10, the reaction medium is mixed in the secondary heat preservation reaction gallery 6, the uniform mixing is basically realized when the reaction medium reaches the spiral stirrer 3 of the connection turning part of the secondary heat preservation reaction gallery 6 and the tertiary control Wen Langdao 7, and then the flow speed and the flow direction of the reaction medium are changed through the spiral stirrer 3;
step 6: in the three-stage temperature control reaction corridor 7, high-power heat exchange pipes 10 arranged at the bottom and the side walls are used for realizing rapid cooling to C ℃, the flow speed and the flow direction of the reaction medium are changed under the action of a spiral stirrer 3 at the joint turning part of the three-stage temperature control reaction corridor 7 and the three-stage heat preservation reaction corridor 8, meanwhile, an acid catalyst required by the reaction is added at a secondary feed inlet 17 above, a hemiacetal reaction is carried out in the three-stage heat preservation reaction corridor 8, at the moment, the viscosity of the reaction medium is increased, part of particles are separated out from the reaction medium, the reaction medium at the liquid level contacts with the inner wall of the three-stage heat preservation reaction corridor 8 to start to adhere to the inner wall of the three-stage heat preservation reaction corridor 8, an external high-pressure fan in the gas viscosity removing system blows out high-speed airflow to an aeration hole 19 on the inner wall of the three-stage heat preservation reaction corridor 8, solid particles adhered to the inner wall of the three-stage heat preservation reaction corridor 8 are blown back into the reaction medium, and the particles are scattered under the action of a push flow stirrer 11, and the particle size is reduced to continue to flow along with the reaction medium; the reaction time is required when the reaction reaches the spiral stirrer 3 of which the three-level heat-preserving reaction gallery 8 is connected with the four-level control Wen Langdao 13; the temperature range of C is-5-30 ℃;
step 7: heating the reaction medium to D ℃ by using a high-power heat exchange tube 10 in a fourth-level temperature control gallery 13, forming PVB particles more and more, generating solid particles at an interface, blowing the solid particles back to the reaction medium by using an aeration hole 19, continuously entering a spiral stirrer 3 of a joint turning part of the fourth-level temperature control Wen Langdao and the fourth-level heat preservation reaction gallery 12, and adding other neutralizing substances to realize system neutrality; the temperature range of D is: 30-80 ℃;
step 8: and when final heat preservation is carried out in the four-stage heat preservation reaction gallery 12, the product PVB is subjected to rough flushing by using external water flow, the final product flows back to the reaction medium, the product and the flushing liquid through the large-bending gallery 14, the liquid and the solid are separated by using the screen 15 at the discharge port, and the obtained PVB particles are collected into the rough product collecting box 16 to wait for further treatment.
Further, the nano modified material comprises nano titanium dioxide, nano silicon dioxide, nano aluminum oxide, nano zinc oxide, nano aluminum oxide and modified composite materials thereof; preferably, the nano titanium dioxide composite modified material or the nano silicon dioxide composite modified material. In addition, the reaction medium is usually water.
The above description is not intended to limit the invention to the particular embodiments disclosed, but to limit the invention to the particular embodiments disclosed, and any variations, modifications, additions or substitutions within the spirit and scope of the invention will become apparent to those skilled in the art.
Claims (10)
1. The utility model provides a PVB large-scale continuous production's reactor, includes reactor and control system, its characterized in that, the reactor be many corridor reactor, many corridor reactor include by control system control's feed system, multistage accuse temperature buffer system, multistage heat preservation reaction system, plug flow mixing system, bend mixing system, gas removes gluey system, accuse temperature system and ejection of compact system, feed system with multistage accuse temperature buffer system meets, multistage accuse temperature buffer system with multistage heat preservation reaction system passes through bend mixing system cross connection, with each accuse temperature corridor in the multistage accuse temperature buffer system with each heat preservation reaction corridor in the multistage heat preservation reaction system connects and forms the many corridor of roundabout turn, each accuse temperature corridor and each heat preservation reaction corridor are inside all to be equipped with plug flow mixing system, each accuse temperature corridor and each heat preservation reaction corridor's bottom all is equipped with accuse temperature system, gas removes gluey system including setting up on accuse Wen Langdao inner wall and each heat preservation reaction corridor is used for preventing through the high-speed aeration high-pressure aeration effect with a plurality of external air vent.
2. The reactor for large-scale continuous production of PVB of claim 1, wherein the feed system comprises a primary feed inlet and at least 4 secondary feed inlets, a feed auxiliary impeller is arranged below the primary feed inlet, the discharge system comprises a large-bending gallery and a discharge outlet, the discharge outlet is arranged on the large-bending gallery, a screen is arranged on the discharge outlet, a coarse product collecting box is arranged near the discharge outlet, the large-bending gallery is in a C shape, one end of the large-bending gallery is connected with one end of the multistage temperature control buffer system, provided with the primary feed inlet, the other end of the large-bending gallery is connected with the final outlet end of the thermal reaction gallery in the multistage thermal reaction system, and the interior of the large-bending gallery at least comprises 3 impeller agitators for pushing the product after the reaction to the discharge outlet through the large-bending gallery.
3. The reactor for large-scale continuous production of PVB of claim 2, wherein the plug flow stirring system comprises plug flow stirrers arranged in the temperature control gallery and the thermal insulation reaction gallery, at least three stages of plug flow are arranged in each temperature control gallery and each thermal insulation reaction gallery, each stage of plug flow comprises two plug flow stirrers arranged at the bottom, and each plug flow stirrer is provided with three plug flow stirring paddles for realizing improvement of raw material mixing efficiency and accurate and stable plug flow speed control of different parts in a reaction medium.
4. A reactor for the mass continuous production of PVB according to any one of claims 1-3 wherein said bend stirring system comprises at least 7 bend stirring zones, each bend stirring zone comprising two helical stirrers, whereby adequate mixing of the reaction materials at each stage above and flow control of the liquid medium in the multi-gallery reactor is achieved by alternate coordination control of the two helical stirrers.
5. A reactor for large-scale continuous production of PVB according to claim 2 or 3, wherein the temperature control galleries in the multi-stage temperature control buffer system comprise a primary temperature control gallery, a secondary temperature control gallery Wen Langdao, a tertiary temperature control gallery and a quaternary temperature control gallery, the temperature control system configured on the inner side wall and the bottom of each temperature control gallery comprises a high-power heat exchange tube, the temperature orientation control of each temperature control gallery is realized through the liquid with different temperatures in the high-power heat exchange tube, and a plurality of plug flow stirrers are arranged in each temperature control gallery for realizing the effective mixing and flow rate control of the reaction raw materials; the heat preservation reaction corridor in the multistage heat preservation reaction system comprises a first-stage heat preservation reaction corridor, a second-stage heat preservation reaction corridor, a third-stage heat preservation reaction corridor and a fourth-stage heat preservation reaction corridor, the temperature control system configured on the inner side wall and the bottom of each heat preservation reaction corridor comprises a low-power heat exchange tube for supplementing heat loss, the temperature control system configured on the inner side wall of each heat preservation reaction corridor comprises a heat preservation layer for preserving heat of liquid in the heat preservation reaction corridor, and the control of reaction time is realized through the flow velocity control of a plurality of plug flow stirrers in the heat preservation reaction corridor.
6. The reactor for large-scale continuous production of PVB according to claim 4, wherein the temperature control galleries in the multi-stage temperature control buffer system comprise a primary temperature control gallery, a secondary temperature control gallery Wen Langdao, a tertiary temperature control gallery and a quaternary temperature control gallery, the temperature control system configured on the inner side wall and the bottom of each temperature control gallery comprises a high-power heat exchange tube, temperature directional control is realized on each temperature control gallery through liquid with different temperatures in the high-power heat exchange tube, and a plurality of plug flow stirrers are arranged in each temperature control gallery for realizing effective mixing and flow rate control of reaction raw materials; the heat preservation reaction corridor in the multistage heat preservation reaction system comprises a first-stage heat preservation reaction corridor, a second-stage heat preservation reaction corridor, a third-stage heat preservation reaction corridor and a fourth-stage heat preservation reaction corridor, the temperature control system arranged at the bottom of each heat preservation reaction corridor comprises a low-power heat exchange tube and is used for supplementing heat loss, the temperature control system arranged inside the side wall of each heat preservation reaction corridor comprises a heat preservation layer and is used for preserving heat of liquid in the heat preservation reaction corridor, and the control of reaction time is realized through the flow velocity control of a plurality of plug flow stirrers in the heat preservation reaction corridor.
7. The reactor for large-scale continuous production of PVB of claim 5, wherein the primary feed inlet of the feed system is positioned at a feed end of the primary control Wen Langdao, the joint turning part of the temperature control gallery and the thermal insulation reaction gallery realizes flow direction conversion of the reaction medium by a spiral stirrer, and the secondary feed inlet is arranged above the spiral stirrer.
8. The reactor for large-scale continuous production of PVB of claim 7 wherein said helical agitator comprises a multi-stage annular helical agitator.
9. A continuous process for the production of PVB in a reactor for large-scale continuous production according to any one of claims 1-8 comprising the steps of:
adding the primary raw material PVA and different reaction raw materials in each intermediate reaction stage into a temperature control gallery and a heat preservation reaction gallery in a multi-gallery reactor from each stage of feed inlets in a feed system, and realizing effective mixing and flow rate control of the reaction raw materials by matching a plug flow stirring system with a bend stirring system; the temperature control system controls the temperature in the temperature control gallery and the heat preservation reaction gallery so as to ensure that the reaction raw materials react at a proper reaction speed and reaction time, PVA resin separated out in the reaction process is partially adhered on the inner walls of the temperature control gallery and the heat preservation reaction gallery, air is blown into a plurality of aeration holes on the inner wall of the temperature control Wen Langdao and the inner wall of the heat preservation reaction gallery by an external high-pressure fan in the air viscosity removing system, and the viscosity removing is realized by the impact of the high-speed flowing air on the inner walls of the temperature control gallery and the heat preservation reaction gallery; and (3) the PVB particles prepared after the reaction is finished are sent out from a discharge hole by a discharge system and are collected for standby, so that the large-scale continuous production of PVB is finished.
10. The continuous process for the production of reactors for the large-scale continuous production of PVB according to claim 9, wherein the operation of the feeding system, the multistage temperature-controlled buffer system, the multistage thermal reaction system, the plug flow stirring system, the bend stirring system, the gas viscosity-removing system, the temperature-controlled system and the discharging system is controlled by a control system, and the continuous process comprises the following specific steps:
step 1: adding reaction medium into each temperature control gallery and each heat preservation reaction gallery in the multi-gallery reactor;
step 2: adding primary raw material PVA from a primary feed inlet of a feed system, driving the PVA to flow along with a reaction medium through a plug flow stirrer below the primary feed inlet, raising the temperature of the reaction medium to at least 95 ℃ in a primary control Wen Langdao through the heat of high-power heat exchange pipes arranged at the bottom and the side wall, realizing flow rate control by controlling the power of the plug flow stirrer, further controlling the hydraulic retention time to reach the time required by PVA dissolution, and completely dissolving the primary raw material PVA when the primary raw material PVA reaches a spiral stirrer at a joint turning part of a primary temperature control gallery and a primary heat preservation reaction gallery;
step 3: adding nano modified materials into a secondary feed inlet above a spiral stirrer at the joint turning part of the primary temperature control gallery and the primary heat preservation reaction gallery, and primarily mixing PVA with the temperature reaching A ℃ in the primary heat preservation reaction gallery, wherein small functional heat exchange pipes arranged at the bottom and the side wall can supplement less heat lost in the flowing process, and the nano modified materials are fully mixed when reaching the tail end of the primary heat preservation reaction gallery along with the operation of the plug flow stirrer; the temperature range of A is: 90-105 ℃;
step 4: the flow direction and the flow speed are changed through a spiral stirrer at the joint turning part of the first-stage heat-preserving reaction gallery 4 and the second-stage temperature-controlling gallery, the reaction medium enters the second-stage temperature-controlling gallery, the continuous flow of the reaction medium is realized through an internal multi-stage plug flow stirrer, the reaction medium is rapidly cooled by using high-power heat exchange pipes arranged at the bottom and the side wall, and the temperature of the reaction medium is reduced to B ℃ when the reaction medium reaches the tail end; the temperature range of B is as follows: 15-30 ℃;
step 5: the flow speed and the flow direction of the reaction medium are changed through a spiral stirrer at the joint turning part of the secondary temperature control gallery and the secondary heat preservation reaction gallery, n-butyraldehyde is added through a secondary charging port above, the reaction medium is mixed in the secondary heat preservation reaction gallery, the reaction medium is basically uniformly mixed when reaching the spiral stirrer at the joint turning part of the secondary heat preservation reaction gallery and the tertiary temperature control gallery, and then the flow speed and the flow direction of the reaction medium are changed through the spiral stirrer at the joint;
step 6: in the three-stage temperature control reaction corridor, the reaction medium is quickly cooled to C ℃ through the inner wall and the low-power heat exchange pipes arranged at the bottom, the flow speed and the flow direction of the reaction medium are changed under the action of the spiral stirrer at the joint turning part of the three-stage temperature control reaction corridor 7 and the three-stage heat preservation reaction corridor, meanwhile, an acid catalyst required by the reaction is added at the upper secondary feed port, the hemiacetal reaction is carried out in the three-stage heat preservation reaction corridor, at the moment, the viscosity of the reaction medium is increased, part of particles are separated out in the reaction medium, the reaction medium at the liquid level contacts with the inner wall of the three-stage heat preservation reaction corridor and begins to adhere to the inner wall of the three-stage heat preservation reaction corridor, an external high-pressure fan in the gas viscosity removing system blows out high-speed airflow to an aeration hole on the inner wall of the three-stage heat preservation reaction corridor, solid particles adhered to the inner wall of the three-stage heat preservation reaction corridor are blown back to the reaction medium, the particles are scattered under the action of the push stirrer, and the particle size is reduced, and the particle size continues to flow along with the reaction medium; the time required for the reaction is completed when the reaction reaches the spiral stirrer of the joint turning part of the three-stage heat preservation reaction gallery and the four-stage temperature control gallery; the temperature range of C is-5-30 ℃;
step 7: heating the reaction medium to D ℃ in the four-stage temperature control gallery by using a high-power heat exchange tube, forming PVB particles more and more, generating solid particles at the interface, blowing the solid particles back to the reaction medium by using an aeration hole, continuously entering a spiral stirrer at the joint turning part of the four-stage temperature control gallery and the four-stage heat preservation reaction gallery, and adding other neutralizing substances to realize system neutrality; the temperature range of D is: 30-80 ℃;
step 8: and (3) carrying out final heat preservation in the four-stage heat preservation reaction gallery, and simultaneously, carrying out coarse flushing on the product PVB by using external water flow, wherein the final product flows back to the reaction medium, the product and the flushing fluid through the large-bending gallery, and liquid and solid separation is realized by using a screen at a discharge port, so that the obtained PVB particles are collected into a coarse product collecting box to wait for further treatment.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202311180250.3A CN117427572A (en) | 2023-09-13 | 2023-09-13 | Reactor for large-scale continuous production of PVB and continuous production method |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202311180250.3A CN117427572A (en) | 2023-09-13 | 2023-09-13 | Reactor for large-scale continuous production of PVB and continuous production method |
Publications (1)
Publication Number | Publication Date |
---|---|
CN117427572A true CN117427572A (en) | 2024-01-23 |
Family
ID=89552365
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202311180250.3A Pending CN117427572A (en) | 2023-09-13 | 2023-09-13 | Reactor for large-scale continuous production of PVB and continuous production method |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN117427572A (en) |
-
2023
- 2023-09-13 CN CN202311180250.3A patent/CN117427572A/en active Pending
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN207970852U (en) | A kind of hydrogenation reaction kettle | |
AU2020267320B2 (en) | Built-in micro interfacial enhanced reaction system and process for pta production with px | |
EP2252391B1 (en) | Vortex mixer and method of obtaining a supersaturated solution or slurry | |
US9095836B2 (en) | Multiphase catalytic tower-type impinging-stream reactor | |
CN201046396Y (en) | Non-rotary vertical cyclic liquid knockout reactor | |
CN101525140B (en) | Method for preparing A-type zeolite by using two-phase block flow microreactor | |
CN117427572A (en) | Reactor for large-scale continuous production of PVB and continuous production method | |
CN113292459B (en) | Continuous nitration method of guanidine nitrate | |
CN103832986A (en) | Preparation method for polyphosphoric acid | |
CN104941554B (en) | A kind of high efficiency reactor | |
CN1076216C (en) | Continuous stirring polymerizing reactor tower | |
CN218901857U (en) | Device for continuously producing high-solid-content polymer products | |
KR100993160B1 (en) | Polyvinylacetal resin and process for producing the same | |
CN111377834A (en) | Continuous preparation method of acetoacetamidosulfonic acid triethylamine | |
CN107837781B (en) | Reaction kettle for strong exothermic reaction | |
CN216936047U (en) | Sulfonation reactor for preparing liquid detergent sulfonic acid | |
CN215877290U (en) | Low-cost enamel kettle for medicine production and processing | |
CN213803581U (en) | Continuous oxidation production reaction device | |
CN210545133U (en) | In-kettle heat exchange polymerization reaction system for strong exothermic polymerization reaction | |
WO2007098637A1 (en) | A prepolycondensation reactor | |
CN208406979U (en) | Novel whole polycondensation vessel | |
CN203750548U (en) | Continuous production equipment of catalysts | |
CN215353466U (en) | Oxidation reactor for back-mixing preheating feeding | |
CN208115748U (en) | A kind of chemosynthesis reaction device of medicine intermediate pyridinedicarboxylic acid | |
US11607663B2 (en) | Strengthening oxidation system of external micro-interfacial unit for producing PTA with PX |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination |