CN108295790A - A kind of Hydrin polymerization reaction kettle and its control method - Google Patents
A kind of Hydrin polymerization reaction kettle and its control method Download PDFInfo
- Publication number
- CN108295790A CN108295790A CN201810318354.9A CN201810318354A CN108295790A CN 108295790 A CN108295790 A CN 108295790A CN 201810318354 A CN201810318354 A CN 201810318354A CN 108295790 A CN108295790 A CN 108295790A
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- hydrin
- reaction kettle
- polymerization reaction
- agitating shaft
- kettle
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- 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
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- 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
Abstract
The present invention discloses a kind of Hydrin polymerization reaction kettle, including：Autoclave body, bottom are the hemisphere bodily form, and top is cylindrical and is hollow-core construction；Catch is circular ring shape sheet, is sealingly disposed in the hollow-core construction top, the hollow-core construction is divided into the first hollow cavity and the second hollow cavity；Agitating shaft is arranged at the autoclave body center, and the agitating shaft higher slice is provided with stirring blade；Cross bar is connect with the agitating shaft cross, and the cross bar is provided at both ends with protrusion, and the protrusion is inserted into first hollow cavity and can rotate in a circumferential direction along first hollow cavity；Floating rule connect with the cross bar both sides and is arranged against the inner wall of kettle vertically.The polymer being adhered on internal face can be scraped off, keep reaction more abundant.The present invention also provides a kind of control methods of Hydrin polymerization reaction kettle, can control the rate of addition of monomer and the mixing speed of agitating shaft so that reaction uniformly, fully, improves product quality.
Description
Technical field
The present invention relates to technical field of chemistry, and more particularly, the present invention relates to a kind of Hydrin polymerisations
Kettle and its control method.
Background technology
Polymerization reaction kettle is some chemical products equipment indispensable in industrialized production, and whipped form determines that polymerization is anti-
The stability and product quality of the efficiency, polymerisation answered.ECH (epoxychloropropane) polymerize when using polymerisation in solution method,
Mechanical stability when polymerization is even more important.For polymerisation in solution other than recipe-imposed performance indicator, technique and reaction kettle
Design in structure is most important.
The single whipped forms such as the stirring of traditional polymerization reaction kettle, generally layer-stepping, frame type stirring, its main feature is that mixed
Close uneven, the direction dynamics of stirring is mainly on horizontal position, bottom to liquid level and reaction kettle wall surface, various material concentrations ladders
Degree difference is very big, and mixing is uneven；Additionally, due to the progress of polymerisation, the viscosity of polymer gradually increases in reaction kettle, also can
The attachment of polymers of some is on reaction kettle wall surface so that mixing is uneven, and the degree of polymerization and molecular weight of polymer can produce
Raw larger difference, but also it is uneven to conduct heat in reaction process；Meanwhile the temperature difference of each point is also larger, reaction condition also differs
It is larger, product quality is influenced, reaction kettle is less efficient.
Invention content
It is an object of the invention to design and develop a kind of Hydrin polymerization reaction kettle, it is arranged on agitating shaft
There is rotatable cross bar, the cross bar against reaction kettle inner wall is provided at both ends with floating rule, the polymerization that can will be adhered on internal face
Object scrapes off, and keeps reaction more abundant.
Another object of the present invention is to have designed and developed a kind of control method of Hydrin polymerization reaction kettle, energy
It is enough that the rate of addition of monomer is controlled according to reaction kettle volume and material proportion, while controlling mixing speed so that reaction is uniform, fills
Point, improve product quality.
Technical solution provided by the invention is：
A kind of Hydrin polymerization reaction kettle, including：
Autoclave body, bottom are the hemisphere bodily form, and top is cylinder, and the autoclave body is hollow-core construction；
Catch is circular ring shape sheet, is sealingly disposed in the hollow-core construction top, and the hollow-core construction is divided into the
One hollow cavity and the second hollow cavity；
Agitating shaft is arranged at the autoclave body center, and the agitating shaft higher slice is provided with stirring blade；
Cross bar is connect with the agitating shaft cross, and the cross bar is provided at both ends with protrusion, and the protrusion is inserted into institute
It states in the first hollow cavity and can rotate in a circumferential direction along first hollow cavity；
Floating rule connect with the cross bar both sides and is arranged against the inner wall of kettle vertically.
Preferably, further include upper cover, be the hemisphere bodily form, outside wall surface is integrally formed with the autoclave body outside wall surface.
Preferably, further include：
Discharge port is arranged in autoclave body bottom；
Feed inlet, setting is on the cover；
Feed chamber is connected to the feed inlet；
Control valve is arranged between the feed chamber and feed inlet, the addition for controlling raw material.
Preferably, further include driving motor, setting on the cover and with the stirring axis connection, for driving
The agitating shaft rotation.
Preferably, one side lower part of the autoclave body is provided with water inlet, and another upper lateral part is provided with water outlet, the water inlet
Mouth and the water outlet are connected to second hollow cavity.
Preferably, the stirring blade is the arc being bent upwards；It is evenly arranged with circular hole on the stirring blade；Institute
Autoclave body bottom radian described in floating rule lower end edge is stated to curve inwardly.
Preferably, further include：
Temperature sensor is arranged on the stirring rod, for detecting temperature in the kettle；
Viscosity sensor is arranged on the agitating shaft, for detecting material viscosity in kettle；
Controller is connect with the temperature sensor, viscosity sensor, control valve and driving motor, for receiving
It states the detection data of temperature sensor and viscosity sensor and controls the control valve and driving motor work.
Correspondingly, the present invention also provides a kind of control methods of Hydrin polymerization reaction kettle, including：
Controller is according to the rate of addition of the fixing fabric structure monomer of solvent, catalyst and initiator：
Wherein,vmFor the rate of addition of monomer, VmFor the volume of monomer, ViTo rise
The volume of beginning agent, VeFor the volume of catalyst, VlFor the volume of solvent, V is the volume of autoclave body；
According to the rate of addition of the temperature, viscosity of material in kettle and monomer and it is expected that the Hydrin prepared point
The rotating speed of son amount control agitating shaft：
Wherein, n is the rotating speed of agitating shaft, and t=0 when t is time and starting reaction, M are the estimated poly- epoxy chloropropionate prepared
The molecular weight of alkane, η are the viscosity of material in kettle, and τ is the number of plies of stirring blade, and T is the temperature of material in kettle.
Preferably, the volume of the solvent and monomer meets：
Vm=2Vl。
Preferably, the monomer is epoxychloropropane, and solvent is isopropanol, and initiator is ethylene glycol, catalyst three
It is fluorinated borate ether.
It is of the present invention to have the beneficial effect that：
Hydrin polymerization reaction kettle of the present invention, rotatable cross bar is provided on agitating shaft, is abutted
The cross bar of reaction kettle inner wall is provided at both ends with floating rule, can scrape off the polymer being adhered on internal face, reaction is made more to fill
Point.
The control method of Hydrin polymerization reaction kettle of the present invention, can be according to reaction kettle volume and material
The rate of addition of burden control monomer, while controlling mixing speed so that reaction uniformly, fully, improves product quality.
Description of the drawings
Fig. 1 is the schematic cross-sectional view of Hydrin polymerization reaction kettle of the present invention.
Fig. 2 is the structural schematic diagram of stirring structure of the present invention.
Fig. 3 is the structural schematic diagram that Hydrin polymerization reaction kettle of the present invention removes upper cover.
Fig. 4 is the structural schematic diagram of Hydrin polymerization reaction kettle of the present invention.
Specific implementation mode
Present invention will be described in further detail below with reference to the accompanying drawings, to enable those skilled in the art with reference to specification text
Word can be implemented according to this.
The present invention can there are many different forms to implement, and should not be construed as limited to again the embodiment of this elaboration, phase
Instead, these embodiments are provided so that the disclosure will be thorough and complete.In the accompanying drawings, for clarity, structure can be exaggerated
With the size and relative size in region.
As shown in Figs 1-4, the present invention provides a kind of Hydrin polymerization reaction kettle, including：Autoclave body 110, bottom
For the hemisphere bodily form, top is cylinder, and the autoclave body 110 is hollow-core construction；Catch 113 is circular ring shape sheet, sealed set
In the hollow-core construction structure upper, the hollow-core construction is divided into the first hollow cavity 111 and the second hollow cavity 112；Agitating shaft
120, it is arranged at 110 center of the autoclave body, 120 higher slice of the agitating shaft is provided with stirring blade 121, in the present embodiment,
The stirring blade 121 is three layers, and the stirring blade 121 is the arc being bent upwards and is evenly arranged with circle on stirring blade
Hole reduces the resistance in whipping process；Cross bar 130 is connect with 120 cross of the agitating shaft, 130 both ends of the cross bar
It is provided with protrusion 131, described raised 131 are inserted into first hollow cavity 111 and can be along first hollow cavity, 111 circumferential direction
Rotation；Floating rule 140 connect with 130 both sides of the cross bar and is arranged against 110 inner wall of the autoclave body vertically, in the present embodiment,
110 bottom radian of autoclave body described in 140 lower end edge of the floating rule curves inwardly, in 120 rotary course of agitating shaft, cross bar 130 with
It is rotated with agitating shaft 120 and the floating rule 140 is driven to rotate, the polymer adhered on 110 internal face of the autoclave body can scraped
Get off so that entire reaction process heat transfer coefficient is stablized, and can carry out preferably stirring and cooling down to material in entire kettle, makes
It must react uniform, stablize, improve product quality.
Further include upper cover 150 in the present embodiment, is the hemisphere bodily form, outside wall surface and the autoclave body 110 outside wall surface one
Molding.Certainly, further include：Discharge port 160, setting is in 110 bottom of autoclave body, for discharging after the completion of reacting；Feed inlet 151,
It is arranged in the upper cover 150；Feed chamber 170 is connected to the feed inlet 151,170 storage reaction list of the feed chamber
Body；Control valve 171 is arranged between the feed chamber 170 and feed inlet 151, the addition for controlling starting monomer.
Further include driving motor 122 in the present embodiment, is arranged in the upper cover 150 and connects with the agitating shaft 120
It connects, for driving the agitating shaft 120 to rotate.
In the present embodiment, 110 1 side lower part of the autoclave body is provided with water inlet 114, and another upper lateral part is provided with water outlet
115, the water inlet 114 and the water outlet 115 are connected to second hollow cavity 112, are used in second hollow cavity 112
In accommodating cooling water, cool down to material in kettle.
In the present embodiment, further include：Temperature sensor is arranged on the stirring rod 120, warm in kettle for detecting
Degree；Viscosity sensor is arranged on the agitating shaft 120, for detecting material viscosity in kettle；Controller, with the temperature
It spends sensor, viscosity sensor, control valve 171 and driving motor 122 to connect, be passed for receiving the temperature sensor and viscosity
The detection data of sensor simultaneously controls the control valve 171 and the work of driving motor 122.
Hydrin polymerization reaction kettle of the present invention, rotatable cross bar is provided on agitating shaft, is abutted
The cross bar of reaction kettle inner wall is provided at both ends with floating rule, can scrape off the polymer being adhered on internal face, reaction is made more to fill
Point.
The present invention also provides a kind of control methods of Hydrin polymerization reaction kettle, including：
Monomer used in the present invention is epoxychloropropane, and solvent is isopropanol, and initiator is ethylene glycol, catalyst three
It is fluorinated borate ether；
Controller is according to the rate of addition of the fixing fabric structure monomer of solvent, catalyst and initiator：
Wherein,vmFor the rate of addition (L) of monomer, VmFor the volume (L) of monomer,
ViFor the volume (L) of initiator, VeFor the volume (L) of catalyst, VlFor the volume (L) of solvent, V is the volume (L) of autoclave body；
The rate of addition of temperature, viscosity and monomer further according to material in kettle and it is expected that the Hydrin prepared
Molecular weight controls the rotating speed of agitating shaft：
Wherein, n is the rotating speed (r/min) of agitating shaft, and t=0 when t is time (min) and starting reaction, M are estimated prepare
Hydrin molecular weight (g/mol), η is the viscosity (Pas) of material in kettle, and τ is the number of plies of stirring blade, and T is
The temperature (DEG C) of material in kettle.
The volume of the solvent and monomer meets：
Vm=2Vl。
The control method of Hydrin polymerization reaction kettle of the present invention, can be according to reaction kettle volume and material
The rate of addition of burden control monomer, while controlling mixing speed so that reaction uniformly, fully, improves product quality.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and legend shown and described herein.
Claims (10)
1. a kind of Hydrin polymerization reaction kettle, which is characterized in that including：
Autoclave body, bottom are the hemisphere bodily form, and top is cylinder, and the autoclave body is hollow-core construction；
Catch is circular ring shape sheet, is sealingly disposed in the hollow-core construction top, and the hollow-core construction is divided into the first sky
The chambers of the heart and the second hollow cavity；
Agitating shaft is arranged at the autoclave body center, and the agitating shaft higher slice is provided with stirring blade；
Cross bar is connect with the agitating shaft cross, and the cross bar is provided at both ends with protrusion, and the protrusion is inserted into described the
It can rotate in a circumferential direction in one hollow cavity and along first hollow cavity；
Floating rule connect with the cross bar both sides and is arranged against the inner wall of kettle vertically.
2. Hydrin polymerization reaction kettle as described in claim 1, which is characterized in that further include upper cover, be hemisphere
The bodily form, outside wall surface are integrally formed with the autoclave body outside wall surface.
3. Hydrin polymerization reaction kettle as claimed in claim 2, which is characterized in that further include：
Discharge port is arranged in autoclave body bottom；
Feed inlet, setting is on the cover；
Feed chamber is connected to the feed inlet；
Control valve is arranged between the feed chamber and feed inlet, the addition for controlling raw material.
4. Hydrin polymerization reaction kettle as claimed in claim 3, which is characterized in that further include driving motor, set
Set on the cover and with the stirring axis connection, for driving the agitating shaft to rotate.
5. the Hydrin polymerization reaction kettle as described in any one of claim 1-4, which is characterized in that the autoclave body
One side lower part is provided with water inlet, and another upper lateral part is provided with water outlet, the water inlet and the water outlet and described second
Hollow cavity is connected to.
6. Hydrin polymerization reaction kettle as claimed in claim 5, which is characterized in that the stirring blade is to be bent up
Bent arc；It is evenly arranged with circular hole on the stirring blade；Autoclave body bottom radian curves inwardly described in the floating rule lower end edge.
7. Hydrin polymerization reaction kettle as claimed in claim 4, which is characterized in that further include：
Temperature sensor is arranged on the stirring rod, for detecting temperature in the kettle；
Viscosity sensor is arranged on the agitating shaft, for detecting material viscosity in kettle；
Controller is connect with the temperature sensor, viscosity sensor, control valve and driving motor, for receiving the temperature
The detection data of degree sensor and viscosity sensor simultaneously controls the control valve and driving motor work.
8. a kind of control method of Hydrin polymerization reaction kettle, which is characterized in that including：
Controller is according to the rate of addition of the fixing fabric structure monomer of solvent, catalyst and initiator：
Wherein,vmFor the rate of addition of monomer, VmFor the volume of monomer, ViFor initiator
Volume, VeFor the volume of catalyst, VlFor the volume of solvent, V is the volume of autoclave body；
According to the rate of addition of the temperature, viscosity of material in kettle and monomer and it is expected that the Hydrin prepared molecular weight
Control the rotating speed of agitating shaft：
Wherein, n is the rotating speed of agitating shaft, and t=0 when t is time and starting reaction, M are the estimated Hydrin prepared
Molecular weight, η are the viscosity of material in kettle, and τ is the number of plies of stirring blade, and T is the temperature of material in kettle.
9. the control method of Hydrin polymerization reaction kettle as claimed in claim 8, which is characterized in that the solvent and
The volume of monomer meets：
Vm=2Vl。
10. the control method of Hydrin polymerization reaction kettle as claimed in claim 9, which is characterized in that the monomer
For epoxychloropropane, solvent is isopropanol, and initiator is ethylene glycol, and catalyst is boron trifluoride ether.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810318354.9A CN108295790B (en) | 2018-04-11 | 2018-04-11 | Poly (epichlorohydrin) polymerization reaction kettle and control method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810318354.9A CN108295790B (en) | 2018-04-11 | 2018-04-11 | Poly (epichlorohydrin) polymerization reaction kettle and control method thereof |
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| Publication Number | Publication Date |
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| CN108295790A true CN108295790A (en) | 2018-07-20 |
| CN108295790B CN108295790B (en) | 2023-09-08 |
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| CN201810318354.9A Active CN108295790B (en) | 2018-04-11 | 2018-04-11 | Poly (epichlorohydrin) polymerization reaction kettle and control method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117019042A (en) * | 2023-10-08 | 2023-11-10 | 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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| Publication number | Publication date |
|---|---|
| CN108295790B (en) | 2023-09-08 |
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