CN108295790B - Poly (epichlorohydrin) polymerization reaction kettle and control method thereof - Google Patents
Poly (epichlorohydrin) polymerization reaction kettle and control method thereof Download PDFInfo
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- CN108295790B CN108295790B CN201810318354.9A CN201810318354A CN108295790B CN 108295790 B CN108295790 B CN 108295790B CN 201810318354 A CN201810318354 A CN 201810318354A CN 108295790 B CN108295790 B CN 108295790B
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- stirring shaft
- kettle
- polyepichlorohydrin
- kettle body
- stirring
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- 238000006116 polymerization reaction Methods 0.000 title claims abstract description 34
- 229920002755 poly(epichlorohydrin) Polymers 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 61
- 238000007790 scraping Methods 0.000 claims abstract description 11
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 10
- 238000001514 detection method Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 27
- 239000000178 monomer Substances 0.000 abstract description 18
- 229920000642 polymer Polymers 0.000 abstract description 8
- 239000002904 solvent Substances 0.000 description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 6
- 239000003999 initiator Substances 0.000 description 6
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- KZMGYPLQYOPHEL-UHFFFAOYSA-N Boron trifluoride etherate Chemical group FB(F)F.CCOCC KZMGYPLQYOPHEL-UHFFFAOYSA-N 0.000 description 2
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920001451 polypropylene glycol Polymers 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
- B01J19/18—Stationary reactors having moving elements inside
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/02—Polycondensates containing more than one epoxy group per molecule
- C08G59/04—Polycondensates containing more than one epoxy group per molecule of polyhydroxy compounds with epihalohydrins or precursors thereof
-
- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
-
- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00189—Controlling or regulating processes controlling the stirring velocity
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Polymerisation Methods In General (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a polymerization reaction kettle of polyepichlorohydrin, comprising: the bottom of the kettle body is hemispherical, and the upper part of the kettle body is cylindrical and is of a hollow structure; the baffle is in a circular ring shape and is arranged at the upper part of the hollow structure in a sealing way, so that the hollow structure is divided into a first hollow cavity and a second hollow cavity; the stirring shaft is arranged in the center of the kettle body, and stirring blades are arranged on the stirring shaft in a layered manner; the cross rod is in crossed connection with the stirring shaft, two ends of the cross rod are provided with bulges, and the bulges are inserted into the first hollow cavity and can rotate along the circumferential direction of the first hollow cavity; the scraping rod is vertically connected with two sides of the cross rod and is closely arranged on the inner wall of the kettle body. The polymer adhered to the inner wall surface can be scraped off, so that the reaction is more sufficient. The invention also provides a control method of the polyepichlorohydrin polymerization reaction kettle, which can control the dropping speed of the monomer and the stirring speed of the stirring shaft, so that the reaction is uniform and sufficient, and the product quality is improved.
Description
Technical Field
The invention relates to the technical field of chemistry, in particular to a poly (epichlorohydrin) polymerization reaction kettle and a control method thereof.
Background
The polymerization reaction kettle is a necessary device for industrial production of some chemical products, and the stirring form of the polymerization reaction kettle determines the efficiency of the polymerization reaction, the stability of the polymerization reaction and the quality of the products. The mechanical stability during polymerization is particularly important when a solution polymerization method is used for ECH (epichlorohydrin) polymerization. In addition to the effect of the formulation on the performance index for solution polymerization, the design of the process and reaction kettle structure is important.
The traditional polymerization reaction kettle is generally in a single stirring mode such as layered stirring, frame stirring and the like, and is characterized in that the mixing is uneven, the stirring direction force is mainly in a horizontal position, the gradient difference between the concentration of various materials from the bottom of the kettle to the liquid surface and the wall surface of the reaction kettle is large, and the mixing is uneven; in addition, as the polymerization reaction is carried out, the viscosity of the polymer in the reaction kettle is gradually increased, and a part of the polymer is adhered to the wall surface of the reaction kettle, so that the mixing is uneven, the polymerization degree and the molecular weight of the polymer are greatly different, and the heat transfer is uneven in the reaction process; meanwhile, the temperature difference of each point is larger, the reaction condition is also larger, the product quality is influenced, and the efficiency of the reaction kettle is lower.
Disclosure of Invention
The invention aims to design and develop a polypropylene oxide polymerization reaction kettle, a rotatable cross rod is arranged on a stirring shaft, scraping rods are arranged at two ends of the cross rod which are close to the inner wall of the reaction kettle, and polymers adhered to the inner wall surface can be scraped off, so that the reaction is more complete.
The invention also aims to design and develop a control method of the polyepichlorohydrin polymerization reaction kettle, which can control the dropping speed of the monomer according to the volume of the reaction kettle and the material proportion, and simultaneously control the stirring speed, so that the reaction is uniform and sufficient, and the product quality is improved.
The technical scheme provided by the invention is as follows:
a poly epichlorohydrin polymerization reaction kettle, comprising:
the bottom of the kettle body is hemispherical, the upper part of the kettle body is cylindrical, and the kettle body is of a hollow structure;
the baffle is in a circular ring shape and is arranged at the upper part of the hollow structure in a sealing way, so that the hollow structure is divided into a first hollow cavity and a second hollow cavity;
the stirring shaft is arranged in the center of the kettle body, and stirring blades are arranged on the stirring shaft in a layered manner;
the cross rod is in crossed connection with the stirring shaft, two ends of the cross rod are provided with bulges, and the bulges are inserted into the first hollow cavity and can rotate along the circumferential direction of the first hollow cavity;
the scraping rod is vertically connected with two sides of the cross rod and is closely arranged on the inner wall of the kettle body.
Preferably, the kettle further comprises an upper cover which is hemispherical, and the outer wall surface of the upper cover and the outer wall surface of the kettle body are integrally formed.
Preferably, the method further comprises:
the discharging port is arranged at the bottom of the kettle body;
the feeding hole is formed in the upper cover;
a raw material chamber which is communicated with the feed inlet;
and a control valve arranged between the raw material chamber and the feed inlet for controlling the addition of raw materials.
Preferably, the stirring device further comprises a driving motor, wherein the driving motor is arranged on the upper cover and connected with the stirring shaft, and is used for driving the stirring shaft to rotate.
Preferably, a water inlet is arranged at the lower part of one side of the kettle body, a water outlet is arranged at the upper part of the other side of the kettle body, and the water inlet and the water outlet are communicated with the second hollow cavity.
Preferably, the stirring blade is in an upward curved arc shape; round holes are uniformly formed in the stirring blades; the lower end of the scraping rod is bent inwards along the radian of the bottom of the kettle body.
Preferably, the method further comprises:
the temperature sensor is arranged on the stirring shaft and used for detecting the temperature in the kettle;
the viscosity sensor is arranged on the stirring shaft and used for detecting the viscosity of materials in the kettle;
and the controller is connected with the temperature sensor, the viscosity sensor, the control valve and the driving motor and is used for receiving detection data of the temperature sensor and the viscosity sensor and controlling the control valve and the driving motor to work.
Correspondingly, the invention also provides a control method of the polyepichlorohydrin polymerization reaction kettle, which comprises the following steps:
the controller controls the dropping rate of the monomer according to the volumes of the solvent, the catalyst and the initiator:
wherein the method comprises the steps of，v m For the drop velocity of the monomer, V m For the volume of the monomer, V i V as the volume of the initiator e V is the volume of the catalyst l The volume of the solvent is V, and the volume of the kettle body is V;
the rotational speed of the stirring shaft is controlled according to the temperature, viscosity and dropping speed of the monomer of the materials in the kettle and the molecular weight of the expected prepared polyepichlorohydrin:
wherein n is the rotation speed of the stirring shaft, T is time and t=0 when the reaction starts, M is the molecular weight of the expected prepared polyepichlorohydrin, eta is the viscosity of the materials in the kettle, tau is the number of layers of the stirring blades, and T is the temperature of the materials in the kettle.
Preferably, the volumes of solvent and monomer satisfy:
V m ＝2V l 。
preferably, the monomer is epichlorohydrin, the solvent is isopropanol, the initiator is ethylene glycol, and the catalyst is boron trifluoride diethyl ether.
The beneficial effects of the invention are as follows:
according to the polyepichlorohydrin polymerization reaction kettle, the rotatable cross rod is arranged on the stirring shaft, and the scraping rods are arranged at the two ends of the cross rod which are close to the inner wall of the reaction kettle, so that the polymers adhered to the inner wall surface can be scraped off, and the reaction is more complete.
The control method of the polyepichlorohydrin polymerization reaction kettle can control the dropping speed of the monomer according to the volume of the reaction kettle and the material proportion, and simultaneously control the stirring speed, so that the reaction is uniform and sufficient, and the product quality is improved.
Drawings
FIG. 1 is a schematic cross-sectional structural diagram of a polymerization reactor for polyepichlorohydrin.
Fig. 2 is a schematic structural view of the stirring structure according to the present invention.
FIG. 3 is a schematic diagram of the structure of the polymerization reactor for polyepichlorohydrin with the upper cover removed.
FIG. 4 is a schematic structural diagram of the polymerization reactor for polyepichlorohydrin.
Detailed Description
The present invention is described in further detail below with reference to the drawings to enable those skilled in the art to practice the invention by referring to the description.
This invention may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, but rather should be construed in breadth and scope in accordance with the appended claims. In the drawings, the size and relative sizes of structures and regions may be exaggerated for clarity.
As shown in fig. 1 to 4, the present invention provides a polymerization reactor for polyepichlorohydrin, comprising: the bottom of the kettle body 110 is hemispherical, the upper part of the kettle body is cylindrical, and the kettle body 110 is of a hollow structure; a baffle 113, which is in a shape of a circular ring and is arranged on the upper part of the hollow structure in a sealing way, and divides the hollow structure into a first hollow cavity 111 and a second hollow cavity 112; the stirring shaft 120 is arranged at the center of the kettle body 110, stirring blades 121 are arranged on the stirring shaft 120 in a layered manner, in the embodiment, the stirring blades 121 are three layers, the stirring blades 121 are in an upward curved arc shape, circular holes are uniformly formed in the stirring blades, and resistance in the stirring process is reduced; the cross rod 130 is in crossed connection with the stirring shaft 120, two ends of the cross rod 130 are provided with bulges 131, and the bulges 131 are inserted into the first hollow cavity 111 and can rotate along the circumferential direction of the first hollow cavity 111; the scraping rod 140 is vertically connected with two sides of the cross rod 130 and is closely arranged on the inner wall of the kettle body 110, in this embodiment, the lower end of the scraping rod 140 is bent inwards along the radian of the bottom of the kettle body 110, in the rotation process of the stirring shaft 120, the cross rod 130 follows the rotation of the stirring shaft 120 and drives the scraping rod 140 to rotate, so that the polymer adhered on the inner wall surface of the kettle body 110 can be scraped off, the heat transfer coefficient of the whole reaction process is stable, and the materials in the whole kettle can be stirred and cooled better, so that the reaction is uniform and stable, and the product quality is improved.
In this embodiment, the upper cover 150 is also provided with a hemispherical shape, and the outer wall surface of the upper cover is integrally formed with the outer wall surface of the kettle body 110. Of course, it also includes: a discharge port 160, which is arranged at the bottom of the kettle body 110 and is used for discharging after the reaction is completed; a feed port 151 provided on the upper cover 150; a raw material chamber 170 communicating with the feed port 151, the raw material chamber 170 storing a reaction monomer; a control valve 171 provided between the raw material chamber 170 and the feed port 151 for controlling the addition of the raw material monomer.
In this embodiment, the stirring apparatus further includes a driving motor 122 disposed on the upper cover 150 and connected to the stirring shaft 120, for driving the stirring shaft 120 to rotate.
In this embodiment, a water inlet 114 is disposed at a lower portion of one side of the kettle body 110, a water outlet 115 is disposed at an upper portion of the other side of the kettle body, the water inlet 114 and the water outlet 115 are communicated with the second hollow cavity 112, and cooling water is contained in the second hollow cavity 112 to cool materials in the kettle.
In this embodiment, the method further includes: a temperature sensor, which is arranged on the stirring shaft 120 and is used for detecting the temperature in the kettle; a viscosity sensor, which is arranged on the stirring shaft 120 and is used for detecting the viscosity of materials in the kettle; and a controller connected to the temperature sensor, the viscosity sensor, the control valve 171 and the driving motor 122, for receiving detection data of the temperature sensor and the viscosity sensor and controlling the control valve 171 and the driving motor 122 to operate.
According to the polyepichlorohydrin polymerization reaction kettle, the rotatable cross rod is arranged on the stirring shaft, and the scraping rods are arranged at the two ends of the cross rod which are close to the inner wall of the reaction kettle, so that the polymers adhered to the inner wall surface can be scraped off, and the reaction is more complete.
The invention also provides a control method of the polyepichlorohydrin polymerization reaction kettle, which comprises the following steps:
the monomer used in the invention is epichlorohydrin, the solvent is isopropanol, the initiator is ethylene glycol, and the catalyst is boron trifluoride diethyl ether;
the controller controls the dropping rate of the monomer according to the volumes of the solvent, the catalyst and the initiator:
wherein,,v m drop acceleration (L), V) of monomer m Is the volume (L), V of the monomer i Volume of initiator (L), V e Volume of catalyst (L), V l The volume (L) of the solvent and the volume (L) of the kettle body are V;
and controlling the rotating speed of the stirring shaft according to the temperature, viscosity and dropping speed of the monomer of the materials in the kettle and the molecular weight of the expected prepared polyepichlorohydrin:
wherein n is the rotation speed (r/min) of the stirring shaft, T is time (min) and t=0 when the reaction is started, M is the molecular weight (g/mol) of the expected prepared polyepichlorohydrin, eta is the viscosity (Pa.s) of the material in the kettle, tau is the number of layers of the stirring blades, and T is the temperature (DEG C) of the material in the kettle.
The volumes of the solvent and the monomer satisfy:
V m ＝2V l 。
the control method of the polyepichlorohydrin polymerization reaction kettle can control the dropping speed of the monomer according to the volume of the reaction kettle and the material proportion, and simultaneously control the stirring speed, so that the reaction is uniform and sufficient, and the product quality is improved.
Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown and described, it is well suited to various fields of use for which the invention would be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the specific details and illustrations shown and described herein, without departing from the general concepts defined in the claims and their equivalents.
Claims (7)
1. A polyepichlorohydrin polymerization reaction kettle, characterized by comprising:
the bottom of the kettle body is hemispherical, the upper part of the kettle body is cylindrical, and the kettle body is of a hollow structure;
the baffle is in a circular ring shape and is arranged at the upper part of the hollow structure in a sealing way, so that the hollow structure is divided into a first hollow cavity and a second hollow cavity;
the stirring shaft is arranged in the center of the kettle body, and stirring blades are arranged on the stirring shaft in a layered manner;
the cross rod is in crossed connection with the stirring shaft, two ends of the cross rod are provided with bulges, and the bulges are inserted into the first hollow cavity and can rotate along the circumferential direction of the first hollow cavity;
the scraping rod is vertically connected with two sides of the cross rod and is closely arranged on the inner wall of the kettle body;
the lower end of the scraping rod is bent inwards along the radian of the bottom of the kettle body, and the stirring blades are three layers.
2. The polymerization reactor for polyepichlorohydrin according to claim 1, further comprising an upper cover having a hemispherical shape, an outer wall surface of which is integrally formed with an outer wall surface of the reactor body.
3. The polyepichlorohydrin polymerization reactor according to claim 2, further comprising:
the discharging port is arranged at the bottom of the kettle body;
the feeding hole is formed in the upper cover;
a raw material chamber which is communicated with the feed inlet;
and a control valve arranged between the raw material chamber and the feed inlet for controlling the addition of raw materials.
4. The polymerization reactor for polyepichlorohydrin according to claim 3, further comprising a driving motor provided on the upper cover and connected to the stirring shaft for driving the stirring shaft to rotate.
5. The polymerization reactor for polyepichlorohydrin according to any one of claims 1 to 4, wherein a water inlet is provided at a lower portion of one side of the reactor body, a water outlet is provided at an upper portion of the other side, and the water inlet and the water outlet are communicated with the second hollow chamber.
6. The polymerization reactor for polyepichlorohydrin according to claim 5, wherein the stirring blade is an upwardly curved arc; round holes are uniformly formed in the stirring blades.
7. The polyepichlorohydrin polymerization reactor according to claim 4, further comprising:
the temperature sensor is arranged on the stirring shaft and used for detecting the temperature in the kettle;
the viscosity sensor is arranged on the stirring shaft and used for detecting the viscosity of materials in the kettle;
and the controller is connected with the temperature sensor, the viscosity sensor, the control valve and the driving motor and is used for receiving detection data of the temperature sensor and the viscosity sensor and controlling the control valve and the driving motor to work.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810318354.9A CN108295790B (en) | 2018-04-11 | 2018-04-11 | Poly (epichlorohydrin) polymerization reaction kettle and control method thereof |
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| CN201810318354.9A CN108295790B (en) | 2018-04-11 | 2018-04-11 | Poly (epichlorohydrin) polymerization reaction kettle and control method thereof |
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| CN117019042B (en) * | 2023-10-08 | 2024-01-23 | 江苏摩材之家新材料科技有限公司 | Detection device and detection method for polyacrylonitrile solution polymerization |
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| CN107225686A (en) * | 2017-07-21 | 2017-10-03 | 合肥潜望镜机械科技有限公司 | A kind of construction concrete central mix plant |
| CN207088180U (en) * | 2017-08-07 | 2018-03-13 | 韦全余 | A kind of efficient mixing arrangement of cement mortar |
| CN208161594U (en) * | 2018-04-11 | 2018-11-30 | 吉林工程技术师范学院 | A kind of Hydrin polymerization reaction kettle |
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| CN108295790A (en) | 2018-07-20 |
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