CN114621364B - Device for preparing epoxidized natural rubber by multi-kettle serial connection, and preparation method and application thereof - Google Patents

Device for preparing epoxidized natural rubber by multi-kettle serial connection, and preparation method and application thereof Download PDF

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CN114621364B
CN114621364B CN202011433593.2A CN202011433593A CN114621364B CN 114621364 B CN114621364 B CN 114621364B CN 202011433593 A CN202011433593 A CN 202011433593A CN 114621364 B CN114621364 B CN 114621364B
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tank body
reaction
solidification
controlled
stirring
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CN114621364A (en
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张立群
宋维晓
卢咏来
吴晓辉
丁小芳
王梓轩
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Hainan Natural Rubber Industry Group Co ltd
Beijing University of Chemical Technology
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Hainan Natural Rubber Industry Group Co ltd
Beijing University of Chemical Technology
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08CTREATMENT OR CHEMICAL MODIFICATION OF RUBBERS
    • C08C19/00Chemical modification of rubber
    • C08C19/04Oxidation
    • C08C19/06Epoxidation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • B01J19/0013Controlling the temperature of the process
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/02Apparatus characterised by being constructed of material selected for its chemically-resistant properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The invention relates to a device for preparing epoxidized natural rubber by multi-kettle serial connection, and a preparation method and application thereof, wherein the device comprises three tanks which are sequentially connected in series: the first reaction tank body, the second cooling tank body and the third solidification tank body. The device is a natural rubber latex epoxidation reaction device with high safety, corrosion resistance and good temperature control effect, the reaction temperature can be controlled within the range of +/-3 ℃ of the set temperature by using the device, and rapid solidification can be realized after the reaction is finished.

Description

Device for preparing epoxidized natural rubber by multi-kettle serial connection, and preparation method and application thereof
Technical Field
The invention relates to the field of rubber preparation, in particular to a device for preparing epoxidized natural rubber by multi-kettle serial connection and a method application thereof.
Background
The natural rubber has high elasticity, high stretching strength, good insulativity, plasticity, tear resistance and wear resistance, can generate better adhesive force with other materials, has the characteristic of 'stretching crystallization', and has various advantages to determine that the natural rubber becomes an elastomer with excellent comprehensive performance, is widely used in various industries such as transportation, national defense and military industry, medical and health, aerospace and the like, and is the most widely applied and green renewable general rubber. However, natural rubber is a rubber with a nonpolar structure, which results in poor solvent resistance, aging resistance, wet skid resistance, air tightness and the like, and further limits the wide application thereof. The double bonds on the molecular chain are modified by a chemical method, so that the performance of the natural rubber can be effectively improved, the application of the natural rubber is expanded, and the added value of the product is increased.
Among various modification methods of natural rubber, epoxidation modification of natural rubber is one of the most promising and practical methods. Through epoxidation modification, partial double bonds on a molecular chain of the natural rubber are randomly replaced by polar epoxy bonds, so that on one hand, the excellent performance of the natural rubber is maintained, on the other hand, the polarity of the natural rubber is increased, and the glass transition temperature of the natural rubber is increased, so that the performances of solvent resistance, air tightness, wet skid resistance and the like of the natural rubber are greatly improved, and the natural rubber can be used as an automobile cover tire, a high-performance load-carrying tire, a damping vibration-absorbing material, a bicycle inner tube and the like, and can be compounded with materials such as PVC, NBR and the like.
In the prior art, the reaction device for preparing the epoxidized natural rubber only uses one reaction kettle, the reaction device is a large-sized reaction kettle with a stirring device, which is externally connected with a cooling water temperature control unit, after the reaction is finished, latex is discharged from the reaction kettle, is transferred into a heating tank for flocculation, and a condensing device is not arranged in the latex transferring process to terminate the reaction.
Many research institutions at home and abroad have conducted extensive researches on preparation, structure, performance, application and the like of epoxidized natural rubber. Today, both thailand and malaysia have commercial grades of epoxidized natural rubber applied to high performance tire tread stock and further exported worldwide. However, at present, no industrial-grade epoxidized natural rubber production line exists in China, mainly because the ring-opening reaction of epoxy groups is sensitive to temperature, the requirement on temperature control is high in the production process of epoxidized natural rubber, the viscosity of a reaction system can be increased along with the extension of reaction time, the heat transfer efficiency is reduced, the reaction is possibly accelerated automatically, the demulsification danger exists, the peroxyformic acid is used as an oxidant, the corrosion protection requirement on equipment is high, the common reaction kettle has strong heat conductivity but does not resist corrosion, the heat transfer efficiency of the reaction kettle made of corrosion-resistant materials is poor, and the precise temperature control in the production process of epoxidized natural rubber can not achieve good coordination and balance between ring-opening side reaction inhibition and corrosion resistance of production equipment. Therefore, there is a need to develop a device for preparing epoxidized natural rubber which is excellent in combination properties.
Disclosure of Invention
Aiming at the problems of high requirements on temperature control and corrosion resistance and the like of a preparation device of epoxidized natural rubber in the prior art, the invention provides a device for preparing epoxidized natural rubber by serially connecting multiple enamel kettles, which is a reaction device for epoxidation of natural rubber latex with high safety, corrosion resistance and good temperature control effect, the reaction temperature can be controlled within a range of +/-3 ℃ of a set temperature by using the device, and rapid solidification can be realized after the reaction is finished.
The invention aims to provide a device for preparing epoxidized natural rubber by serially connecting multiple enamel kettles, wherein the temperature of each kettle, the type of stirring paddles and the rotating speed of the device are adjusted according to different stages and needs of reaction, so that the corrosion resistance requirement of a tank body is met, and the control of the reaction temperature is maximally realized.
In order to achieve one of the above objects, the present invention is achieved by the following technical solutions:
the invention relates to a device for preparing epoxidized natural rubber by serially connecting multiple enamel kettles, which comprises three tanks serially connected in sequence: the first reaction tank body, the second cooling tank body and the third solidification tank body.
In the above technical scheme, set up feed inlet and discharge gate on the first retort body, its discharge gate links to each other with the feed inlet of second cooling tank, and the discharge gate of second cooling tank links to each other with the feed inlet of the third solidification tank body.
In the technical scheme, the feed inlets of the first reaction tank body and the second cooling tank body are arranged on the tank cover, and the discharge outlets are arranged at the bottom of the tank; the feed inlet of the third solidification tank body is arranged at the upper part of the side wall of the tank body.
In the above technical scheme, the first reaction tank body, the second cooling tank body and the third solidification tank body are respectively provided with a hollow outer interlayer, the outer interlayer is respectively provided with a condensate water outlet and a condensate water inlet, and each tank body outer layer, the water outlet pipe and the water inlet pipe form an independent water circulation pipeline.
In the technical scheme, the position of the condensed water outlet of the outer interlayer of the first reaction tank body is higher than the position of the condensed water inlet of the outer interlayer; the outer interlayer condensed water outlet position of the second cooling tank body is higher than the outer interlayer condensed water inlet position; and the position of an outer interlayer condensate outlet of the third solidification tank body is higher than the position of an outer interlayer condensate inlet.
In the technical scheme, the three tank bodies are provided with stirring devices; preferably, the method comprises the steps of,
the first reaction tank body and the second cooling tank body are provided with stirring shafts penetrating through the tank cover, the upper ends of the stirring shafts are connected with the motor, and the lower ends of the stirring shafts extend into the tank body and are connected with stirring blades; the third solidification tank body is provided with a stirring shaft penetrating through the middle part of the bottom of the tank body, the lower end of the stirring shaft is connected with the motor, and the upper end of the stirring shaft extends into the tank body to be connected with the stirring blade; more preferably, the process is carried out,
the stirring blades in the first reaction tank body are double-folded blade paddle stirring blades; the reaction speed is high due to the high concentration of reactants in the early reaction period, the viscosity of the latex system is low, the mechanical stability is low, the stirring requirement can be met by using the blade, the stimulation of the stirring paddle to the latex system is reduced, and latex demulsification is prevented;
the stirring blades of the second cooling tank body are anchor frame type stirring blades;
the stirring vane of the third solidification tank body is an anchor stirring vane, and because solids can appear gradually in the material in the solidification stage, the anchor stirring vane has high structural strength and large stirring force, and can assist in taking out the solidified rubber material.
In the above technical scheme, the tank cover of the third solidification tank body is an easy-to-open tank cover, and is preferably an upper lifting cover structure with a hinge arranged at the side.
In the technical scheme, the inner layers of the tank body are all enamel materials, and the enamel materials with the thickness of 0.8-2cm are further optimized; the outer layers of the tank body are all made of metal materials, and further preferably stainless steel materials.
The invention also aims to provide a device for preparing the epoxidized natural rubber by serially connecting multiple kettles, and a method for preparing the epoxidized natural rubber. The method is simple and easy to operate, and can effectively control the epoxidation degree of the reaction product and reduce the ring-opening side reaction of the epoxy group.
In order to achieve the second purpose, the invention is realized by the following technical scheme:
the method of the invention comprises the following steps: the raw materials firstly enter a first reaction tank body for reaction, then are discharged and enter a second cooling tank body for cooling, and simultaneously continue to react until the temperature of the latex is reduced to below 25 ℃; and discharging from the second cooling tank body, and feeding the discharged material into a third solidification tank body to carry out demulsification solidification on the upper liquid to obtain the epoxidized natural rubber product.
In the technical scheme, the reaction temperature of the first reaction tank body is controlled to be 40-50 ℃, preferably 40-45 ℃;
in the technical scheme, the temperature of the cooling reaction in the second cooling tank body is controlled to be 20-25 ℃, preferably 20-22 ℃;
in the above technical scheme, the temperature of solidification in the third solidification tank is controlled to be 70-80 ℃, preferably 70-75 ℃.
In the above technical scheme, when the temperature of the material in the kettle of the first reaction tank body is raised to 60 ℃, the material is discharged to the second cooling tank body, preferably the reaction time in the first reaction tank body is controlled to be 3-15 h, more preferably 6-12 h; the rotation speed of the stirring blades in the first reaction tank body is controlled to be 100-120 r/min, preferably 100-110 r/min;
according to the technical scheme, when the second cooling tank body is cooled to reach the required epoxy degree, the neutralizing agent is added and then discharged to the third solidification tank body. The epoxy degree determination is based on a DSC empirical curve, i.e., the epoxy degree is estimated from the change in Tg in the reaction.
Preferably, the cooling reaction time in the second cooling tank body is controlled to be 1-2 h, more preferably 1h; the rotation speed of the stirring blade in the second cooling tank body is controlled to be 70-100 r/min, preferably 80-100 r/min.
In the technical scheme, after the latex in the third solidification tank body is solidified completely, the tank can be opened for taking materials. The latex was judged to be completely coagulated as the latex solution became clear and the solid-liquid phases were completely separated.
Preferably, the coagulation time of the latex in the third coagulation tank is controlled to be 2-4 hours, preferably 3-4 hours; the rotation speed of the stirring blade in the third solidification tank body is controlled to be 30-50 r/min, preferably 40-50 r/min. The material taking mode is to use a crane to hoist out the solidified and agglomerated glue after the tank cover is opened.
Compared with the prior art, the invention has the following beneficial effects: the inner layer of the reaction tank is made of enamel material, so that the corrosion of peroxyformic acid can be effectively resisted, the heat conductivity of the reaction tank is reduced, the control capability of the reaction tank on the reaction temperature is enhanced through the series connection of a plurality of kettles, the set temperatures of the kettles are different and are used for different stages of reaction, the material adding stage in the early stage of reaction has low reaction speed, and the reaction speed is increased by rapidly increasing the temperature of the first reaction tank body; in the middle and later stage of the reaction, on one hand, the heat release of the materials is large, the viscosity is large, the heat transfer efficiency is low, the reaction is continuously and automatically accelerated, on the other hand, when the addition of the neutralizing agent is used for terminating the epoxidation reaction, a great deal of heat release is generated, the demulsification risk is increased, the temperature of the materials is required to be rapidly reduced through a second cooling tank body, so that the preset reaction time is safely reached, the epoxidation degree of the reaction product can be effectively controlled, and the ring-opening reaction degree of epoxy groups is reduced; and in the solidification stage at the later stage of the reaction, the reaction temperature is quickly raised to 20-30 ℃ above the cloud point of the used stabilizer by the high temperature of the third solidification tank body, so that the purpose of quickly solidifying the latex is achieved.
According to the invention, continuous preparation from reaction to solidification is realized through the series connection of a plurality of tanks, and according to different stages and requirements of the reaction, the temperature of each tank, the type of stirring paddles and the rotating speed are regulated, so that not only is the corrosion resistance requirement of the tank body met, but also the control of the reaction temperature is maximally realized, and further the epoxidation degree of a reaction product is effectively controlled and the ring-opening side reaction of an epoxy group is reduced.
300kg of the device is fed once, and the epoxidation degree of the epoxidized natural rubber with the epoxidation degree less than 25mol percent can be controlled to be +/-2% of the theoretical value; the epoxidation degree of the epoxidized natural rubber with the epoxidation degree of 25-60 mol percent can be controlled to be +/-3% of theoretical value, and the precision is slightly higher than that of the prior art by 1-2 percent. The accuracy of the epoxy degree is also higher as the temperature control is finer.
Drawings
Fig. 1 is a schematic structural view of the device of the present invention.
1-a first reaction tank body; 2-a second cooling tank; 3-a third solidification tank; 4-a first feed inlet; 5-a second feed inlet; 6-a first stirring shaft; 7-a second stirring shaft; 8-a first discharge hole; 9-a second feed inlet; 10-a second discharge port; 11-a third stirring shaft; 12-a first condensate outlet; 13-a second condensate outlet; 14-a third condensate outlet; 15-a first condensate inlet; 16-a second condensate inlet; 17-a third condensate inlet; 18-a can lid; 19-a first stirring blade; 20-a second stirring blade; 21-third stirring vane.
Detailed Description
The present invention is described in detail below with reference to specific embodiments, and it should be noted that the following embodiments are only for further description of the present invention and should not be construed as limiting the scope of the present invention, and some insubstantial modifications and adjustments of the present invention by those skilled in the art from the present disclosure are still within the scope of the present invention.
The integrated device for preparing the epoxidized natural rubber used in the embodiment of the invention is shown in fig. 1.
The invention relates to a device for preparing epoxidized natural rubber by serially connecting multiple enamel kettles, which comprises three tanks serially connected in sequence: a first reaction tank 1, a second cooling tank 2 and a third solidification tank 3.
In the above technical scheme, the first reaction tank body 2 is provided with the feed inlet 4 and the discharge outlet 8, the discharge outlet 8 is connected with the feed inlet 5 of the second cooling tank 2, and the discharge outlet 10 of the second cooling tank 2 is connected with the feed inlet 9 of the third solidification tank body 3.
In the technical scheme, the feed inlets of the first reaction tank body and the second cooling tank body are arranged on the tank cover, and the discharge outlets are arranged at the bottom of the tank; the feed inlet of the third solidification tank body is arranged at the upper part of the side wall of the tank body.
In the above technical scheme, the first reaction tank body, the second cooling tank body and the third solidification tank body are respectively provided with a hollow outer interlayer, the outer interlayers are respectively provided with condensate outlets 12, 13 and 14 and condensate inlets 15, 16 and 17, and the outer layers of the tanks, the water outlet pipe and the water inlet pipe form independent water circulation pipelines.
In the above technical solution, the position of the outer interlayer condensate outlet 12 of the first reaction tank 1 is higher than the position of the outer interlayer condensate inlet 15; the position of the outer interlayer condensate outlet 13 of the second cooling tank body 2 is higher than the position of the outer interlayer condensate inlet 16; the position of the outer interlayer condensate outlet 14 of the third solidification tank body 3 is higher than the position of the outer interlayer condensate inlet 17.
In the technical scheme, the three tank bodies are provided with stirring devices; preferably, the method comprises the steps of,
the first reaction tank body 1 and the second cooling tank body 2 are provided with stirring shafts 6 and 7 penetrating through the tank cover, the upper ends of the stirring shafts 6 and 7 are connected with a motor, and the lower ends extend into the tank body and are connected with stirring blades; the third solidification tank body 3 is provided with a stirring shaft 11 penetrating through the middle part of the bottom of the tank body, the lower end of the stirring shaft 11 is connected with a motor, and the upper end of the stirring shaft extends into the tank body to be connected with stirring blades; more preferably, the process is carried out,
the stirring blades 19 in the first reaction tank body are double-hinge paddle stirring blades;
the stirring blade 20 of the second cooling tank body is an anchor frame type stirring blade;
the stirring blade 11 of the third solidification tank body is an anchor stirring blade.
In the above technical solution, the tank cover 18 of the third solidification tank body is an upper cover-lifting structure with a hinge at a side edge.
In the technical scheme, the inner layers of the tank body are enamel materials with the thickness of 1 cm; the outer layer of the tank body is made of stainless steel.
Example 1
300kg of materials are added into the first reaction tank body 1, circulating water at 40 ℃ is introduced into an interlayer of the first reaction tank body to heat the materials, a motor of the tank body 1 is started to drive a stirring shaft 6 and stirring blades 19 to rotate, the rotating speed of the stirring blades 19 is controlled to be 100r/min, and under the condition of continuous stirring and rotation, the circulating water in the interlayer and the materials exchange heat, so that the temperature of the materials is gradually increased to 40 ℃ required by reaction and maintained at +/-3 ℃, and the total reaction time is predicted to be 6 hours, so that the epoxidized natural rubber with the epoxy degree of 25% is prepared. Along with the progress of the reaction, the epoxidation reaction begins to emit a large amount of heat, after 5 hours of reaction, the viscosity of the material begins to increase, the heat exchange efficiency is reduced, the temperature of the material begins to inevitably rise, when the temperature of the material in the kettle rises to 60 ℃, the material is discharged into the second cooling tank body 2, a motor is started, the stirring shaft 7 and the stirring blade 20 are driven to rotate, the rotating speed of the stirring blade 20 is controlled to 80r/min, 25 ℃ circulating water is introduced into an interlayer of the material to cool the material, the temperature difference of the interlayer is relatively low, the heat generated by the reaction can be rapidly exchanged to the outside, so that the temperature of the material is kept constant, after the cooling time reaches the preset total reaction time of 6 hours, a neutralizer is added to terminate the reaction, the material is discharged into the third solidification tank body 3, the motor is started, the stirring shaft 21 and the stirring blade 11 are driven to rotate, the rotating speed of the stirring blade 11 is controlled to be 40r/min, and the circulating water at 80 ℃ is introduced into the interlayer of the stirring blade, after the latex is completely solidified, and finally the tank cover 18 is opened to discharge the solidified, so that the natural ENR25 is obtained after the rubber is demulsified. The epoxy degree obtained after nuclear magnetic testing of the prepared epoxidized natural rubber is 24.1 percent and accords with the range of +/-2 percent of theoretical value.
Example 2
200kg of materials are added into the first reaction tank body 1, circulating water at 40 ℃ is introduced into an interlayer of the first reaction tank body to heat the materials, a motor of the tank body 1 is started to drive a stirring shaft 6 and stirring blades 19 to rotate, the rotating speed of the stirring blades 19 is controlled at 110r/min, and under the condition of continuous stirring and rotation, the circulating water in the interlayer and the materials exchange heat, so that the temperature of the materials is gradually increased to 40 ℃ required by reaction and maintained at +/-3 ℃, and the total reaction time is estimated to be 12 hours, so that the epoxidized natural rubber with the epoxy degree of 50% is prepared. Along with the progress of the reaction, the epoxidation reaction begins to emit a large amount of heat, after 11 hours of reaction, the viscosity of the material begins to increase, the heat exchange efficiency is reduced, the temperature of the material begins to inevitably rise, when the temperature of the material in the kettle rises to 60 ℃, the material is discharged into the second cooling tank body 2, a motor is started, the stirring shaft 7 and the stirring blades 20 are driven to rotate, the rotating speed of the stirring blades 20 is controlled to be 100r/min, 25 ℃ circulating water is introduced into an interlayer of the stirring shaft 7 and the stirring blades, the material is cooled, the temperature difference is relatively large, the heat generated by the reaction can be rapidly exchanged to the outside, the temperature of the material is kept constant, after the cooling time reaches the preset reaction time of 12 hours, the neutralizer is added to terminate the reaction, the material is discharged into the third solidification tank body 3, the motor is started, the stirring shaft 11 and the stirring blades 21 are driven to rotate, the rotating speed of the stirring blades 21 is controlled to be 40r/min, the circulating water at 80 ℃ is introduced into the interlayer of the stirring blades, the latex is totally demulsified and solidified under the double effects of heat and stirring, and finally the tank cover 18 is opened to discharge the solidified epoxy rubber ENR50B is obtained. The epoxy degree obtained after nuclear magnetic testing of the prepared epoxidized natural rubber is 48.2 percent and accords with the range of +/-3 percent of theoretical value.
Comparative example 1
ENR25C and ENR50C were prepared using conventional preparation techniques. The traditional process comprises the following steps: and after the epoxidation reaction is finished in the reaction kettle, directly heating and flocculating, extruding and washing the flocculated rubber blocks by using a crepe machine, and transferring the washed rubber blocks into an oven for drying to obtain the product.
The performance of the preparation of ENR25B and ENR50B using the apparatus of the present invention is shown in table 1 as compared to the performance of ENR25C and ENR50C obtained by conventional preparation processes. Compared with the traditional process, the epoxy degree of the invention is more stable and the ring opening ratio (side reaction ratio) is smaller, because the invention transfers the material to the cooling tank body to reduce the material reaction rate when the ring opening reaction is most severe in the middle of the reaction, thereby effectively inhibiting the occurrence of the side reaction, and the control of the epoxy degree and the inhibition of the side reaction are obviously superior to the traditional process.
TABLE 1
Epoxy degree Ring-opened matter ratio
ENR25B 24.1 0.9%
ENR25C 27.6 3.7%
ENR50B 48.2 2.1%
ENR50C 53.9 6.3%
The above-described embodiment is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the technical aspects set forth in the claims.

Claims (12)

1. The device for preparing the epoxidized natural rubber by serially connecting multiple kettles is characterized by comprising three tanks which are serially connected in sequence: the first reaction tank body, the second cooling tank body and the third solidification tank body; the three tank bodies are provided with stirring devices, the first reaction tank body and the second cooling tank body are provided with stirring shafts penetrating through the tank cover, the upper ends of the stirring shafts are connected with a motor, the lower ends of the stirring shafts extend into the tank body and are connected with stirring blades, the stirring blades in the first reaction tank body are double-folded blade type stirring blades, and the stirring blades in the second cooling tank body are anchor frame type stirring blades; the third solidification tank body is provided with a stirring shaft penetrating through the middle part of the bottom of the tank body, the lower end of the stirring shaft is connected with the motor, the upper end of the stirring shaft stretches into the tank body and is connected with the stirring blade, and the stirring blade of the third solidification tank body is an anchor stirring blade; the temperature of the first reaction tank body is controlled to be 40-45 ℃, the reaction time is controlled to be 6-12 hours, and the rotating speed of the stirring blade is controlled to be 100-110 r/min; the temperature of the second cooling tank body is controlled to be 20-22 ℃, and the rotating speed of the stirring blade is controlled to be 80-100 r/min; the temperature of the third solidification tank body is controlled to be 70-75 ℃, the solidification time is controlled to be 3-4 hours, and the rotation speed of the stirring blade is controlled to be 40-50 r/min.
2. The apparatus of claim 1, wherein the device comprises a plurality of sensors,
the first reaction tank body is provided with a feed inlet and a discharge outlet, the discharge outlet of the first reaction tank body is connected with the feed inlet of the second cooling tank, and the discharge outlet of the second cooling tank is connected with the feed inlet of the third solidification tank body.
3. The apparatus of claim 2, wherein the device comprises a plurality of sensors,
the feed inlets of the first reaction tank body and the second cooling tank body are arranged on the tank cover, and the discharge outlets are arranged at the bottom of the tank; the feed inlet of the third solidification tank body is arranged at the upper part of the side wall of the tank body.
4. The device according to claim 1, wherein the first reaction tank, the second cooling tank and the third solidification tank are respectively provided with a hollow outer interlayer, the outer interlayer is respectively provided with a condensed water outlet and a condensed water inlet, and the outer interlayers of the tanks, the water outlet pipe and the water inlet pipe form independent water circulation pipelines.
5. The apparatus of claim 4, wherein the outer interlayer condensate outlet position of the first reaction tank is higher than the outer interlayer condensate inlet position; the outer interlayer condensed water outlet position of the second cooling tank body is higher than the outer interlayer condensed water inlet position; and the position of an outer interlayer condensate outlet of the third solidification tank body is higher than the position of an outer interlayer condensate inlet.
6. The apparatus of claim 1, wherein the lid of the third solidification tank is an openable lid.
7. The apparatus of claim 6, wherein the lid of the third solidification tank is a flip-up lid structure with a hinge disposed at a side edge.
8. The device according to any one of claims 1 to 7, wherein the inner layers of the tank are all enamel materials; the outer layers of the tank body are all made of metal materials.
9. The device according to claim 8, wherein the inner layers of the tank are all enamel materials with the thickness of 0.8-2 cm; the outer layers of the tank body are made of stainless steel materials.
10. The apparatus for producing epoxidized natural rubber according to any one of claims 1 to 9 in multi-tank series, and a method for producing epoxidized natural rubber.
11. A process according to claim 10, characterized in that,
the raw materials firstly enter a first reaction tank body for reaction, then are discharged and enter a second cooling tank body for cooling, and simultaneously continue to react until the temperature of the latex is reduced to below 25 ℃; and discharging from the second cooling tank body, and feeding the discharged material into a third solidification tank body to carry out demulsification solidification on the upper liquid to obtain the epoxidized natural rubber product.
12. A process according to claim 11, characterized in that,
the reaction temperature of the first reaction tank body is controlled to be 40-45 ℃; and/or the number of the groups of groups,
the reaction time of the first reaction tank body is controlled to be 6-12 hours; and/or the number of the groups of groups,
the rotation speed of the stirring blades in the first reaction tank body is controlled to be 100-110 r/min; and/or the number of the groups of groups,
the temperature of the cooling reaction of the second cooling tank body is controlled to be 20-22 ℃; and/or the number of the groups of groups,
the rotation speed of the stirring blades in the second cooling tank body is controlled to be 80-100 r/min; and/or the number of the groups of groups,
the solidification temperature of the third solidification tank body is controlled to be 70-75 ℃; and/or the number of the groups of groups,
the solidification time of the third solidification tank body is controlled to be 3-4 hours; and/or the number of the groups of groups,
and the rotating speed of the stirring blade in the third solidification tank body is controlled to be 40-50 r/min.
CN202011433593.2A 2020-12-10 2020-12-10 Device for preparing epoxidized natural rubber by multi-kettle serial connection, and preparation method and application thereof Active CN114621364B (en)

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