CN114573735A - Integrated device for preparing epoxidized natural rubber, and method and application thereof - Google Patents
Integrated device for preparing epoxidized natural rubber, and method and application thereof Download PDFInfo
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Abstract
The invention relates to an integrated device for preparing epoxidized natural rubber, a method and application thereof, wherein the device comprises a reaction tank body and a multi-module double-screw extruder; the multi-module double-screw extruder is connected with a discharge port of the reaction tank body. The device is corrosion-resistant, the control by temperature change is effectual to possess the epoxidation natural rubber preparation facilities of functions such as steam flocculation, washing, drying, utilize the device can control reaction temperature within 3 ℃ of settlement temperature, and can realize quick solidification, drying and obtain final dry glue product after the reaction finishes.
Description
Technical Field
The invention relates to the field of rubber preparation, in particular to an integrated device for preparing epoxidized natural rubber, a method and 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', has various advantages, determines that the natural rubber becomes an elastomer with excellent comprehensive performance, is widely applied to various industries such as transportation, national defense and military industry, medical treatment and health, aerospace and the like, and is a green and renewable general rubber with the widest application. However, natural rubber is a rubber with a non-polar structure, which causes poor performances such as solvent resistance, aging resistance, wet skid resistance, air tightness and the like, and further limits the wide application of the natural rubber. The double bonds on the molecular chain of the natural rubber 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 natural rubber is increased.
Among various methods for modifying natural rubber, the epoxidation modification of natural rubber is the most promising method among them. Through epoxidation modification, partial double bonds on a natural rubber molecular chain are randomly substituted by polar epoxy bonds, so that the excellent performance of the natural rubber is kept, 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, the natural rubber can be used as an automobile tyre, a high-performance truck tire, a damping and shock-absorbing material, a bicycle inner tube and the like, and can be compounded with materials such as PVC, NBR and the like.
Many research institutions both at home and abroad carry out detailed research on the preparation, structure, performance, application and the like of the epoxidized natural rubber. Commercial grades of epoxidized natural rubber are now available in both thailand and malaysia for use on high performance tire tread adhesives and further export to the world. However, one of the obstacles to further expanding the applications of epoxidized natural rubber is the production cost. Firstly, because the production process has higher requirement on temperature control, the thermal conductivity of the reaction kettle is good, and the peroxyformic acid is used as an oxidant and has higher requirement on corrosion resistance of equipment, the common stainless steel reaction kettle has strong thermal conductivity but no corrosion resistance, and the corrosion-resistant reaction kettle made of noble metal has extremely high cost; secondly, the latex needs to be flocculated into blocks in the rubber production process for further processing, but the epoxidized natural latex is difficult to flocculate by using a common mode (adding acid, adding high-valence metal salt and the like) due to the addition of a large amount of surfactant, and the cost is extremely high if the latex is flocculated by using solvents such as methanol, ethanol and the like; thirdly, the latex post-treatment needs dehydration and drying, and the traditional hot air drying method needs long time, low production efficiency and high cost, so how to reduce the production cost of the epoxidized natural rubber is a problem to be solved urgently.
Disclosure of Invention
Aiming at the problems of high requirements on temperature control and corrosion resistance, high cost and the like of a preparation device of epoxidized natural rubber in the prior art, the invention provides the epoxidized natural rubber preparation device which has the advantages of corrosion resistance, good temperature control effect and functions of steam flocculation, water washing, drying and the like, the reaction temperature can be controlled within +/-3 ℃ of the set temperature by utilizing the device, and quick solidification and drying can be realized after the reaction is finished to obtain a final dry rubber product.
One of the purposes of the invention is to provide a drying integrated device for preparing epoxidized natural rubber, which comprises a reaction tank body 1 and a multi-module double-screw extruder; the multi-module double-screw extruder is connected with a discharge port of the reaction tank body.
In the technical scheme, the multi-module double-screw extruder sequentially comprises a steam solidifying section 2, a water washing section 3 and a drying section 4 according to a feeding sequence.
In the technical scheme, the steam solidification section comprises a feed inlet 8, a steam inlet 9 and a flocculation screw module, and the flocculation screw module is specifically designed in such a way that the clearance between a screw and a charging barrel is 0.3-0.4 mm, and the clearance between screws is 1.5-2 mm; the length of the screw is 1-1.5 m.
Among the above-mentioned technical scheme, the washing section includes water inlet 10 and washing screw module, and the concrete design of washing screw module is that screw rod and feed cylinder clearance are 0.3 ~ 0.4mm, and the screw rod clearance is 1 ~ 1.2mm, and screw rod length is 1 ~ 1.5 m.
In the technical scheme, the drying section comprises a vacuum pump air exhaust opening 11 and a drying screw module, the drying screw module is specifically designed to have a screw and cylinder clearance of 0.3-0.4 mm, a screw clearance of 1-1.2 mm and a screw length of 2-3 m.
In the technical scheme, the length ratio of the steam solidifying section to the water washing section to the drying section is 1 (1-1.2) to 2-2.2, preferably 1:1: 2; wherein the length of the steam solidified section is less than or equal to 1.5 m.
The steam coagulation section is used for directly contacting high-temperature steam with latex to enable the latex to be demulsified and coagulated, and forwards conveying the rubber obtained by steam flocculation; the water washing section washes out residual reagent in the rubber block by water flow under the shearing and mixing of the screw; and in the drying section, the moisture of the rubber block is extruded out through high-temperature shearing and extrusion, and the residual moisture is pumped out by using a vacuum pump, so that the dried rubber is finally obtained.
Among the above-mentioned technical scheme, be equipped with feed inlet 5 on the cover at the 1 top of the retort body, pass the cover and set up (mixing) shaft 6, the upper end of (mixing) shaft 6 links to each other with the outer motor of cover, and the lower extreme stretches into the jar internally, is connected with stirring vane.
In the technical scheme, a discharge port 7 of the reaction tank body 1 is connected with a feed port 8 of a steam solidification section 2 of the double-screw extruder, and a steam inlet 9 is arranged at the upper part of the steam solidification section; the upper part of the washing section 3 is provided with a water inlet 10; the upper part of the drying section 4 is provided with a vacuum air pump exhaust opening 11, and the tail part is provided with a discharge opening 12.
In the technical scheme, the reaction tank body 1 is provided with a hollow outer interlayer, the outer interlayer is provided with an outer interlayer water outlet pipe and an outer interlayer water inlet pipe, and the outer interlayer, the water outlet pipe and the water inlet pipe form an independent water circulation pipeline. The temperature of the circulating pipeline water is 30-50 ℃.
In the above technical scheme, be equipped with condensation circulating water inlet 13 and outer intermediate layer water piping connection on the outer intermediate layer, be equipped with condensation circulating water outlet 14 and outer intermediate layer water piping connection on the outer intermediate layer, condensation circulating water outlet 14 position is higher than condensation circulating water inlet 13 position.
In the technical scheme, the inner layer of the reaction tank body 1 is made of enamel materials, and the enamel materials with the thickness of 0.8-2cm are further preferably selected; the outer layer of the tank body is made of metal materials, and stainless steel materials are further preferred.
In the technical scheme, the coating inside the charging barrel of the multi-module double-screw extruder is subjected to anti-corrosion treatment, and preferably, the coating is a polytetrafluoroethylene coating.
In the technical scheme, the surfaces of the screws and the screw blocks in the multi-module double-screw extruder are subjected to anti-corrosion treatment, and stainless steel screws or polytetrafluoroethylene screws are preferably selected. The screw block is further preferably a Cr12MoV material meshing block, and the surface of the screw block is subjected to anticorrosion treatment to prevent the screw block from being corroded by latex with strong acidity.
In the technical scheme, the stirring blades are double-folded blade paddle type stirring blades; the rotation speed is 100r/min or more, preferably 100-120 r/min.
In the above technical scheme, the motor is a turbine speed reducer.
Another object of the present invention is to provide a process for producing epoxidized natural rubber.
In the technical scheme, the reaction temperature of the reaction tank body is 35-45 ℃, and is preferably 38-42 ℃.
In the technical scheme, the reaction time of the reaction tank body is 4-15 hours, and preferably 6-12 hours.
In the technical scheme, the steam pressure in the steam solidifying section is 0.5-0.7MPa, the steam introducing amount is 50-60Kg/h, and the steam temperature is 140-.
In the technical scheme, the temperature of the water washing section is 20-30 ℃, and preferably room temperature.
In the above technical scheme, the heating temperature of the twin-screw in the drying section is 110-120 ℃, and preferably 115-120 ℃.
In the technical scheme, the screw rotating speed of the multi-module double-screw extruder is 10-25 r/min, and preferably 10-15 r/min.
Compared with the prior art, the invention has the following beneficial effects: the inner layer of the reaction tank is an enamel coating, so that the cost is low, the heat-conducting property is good, and the corrosion of the peroxyformic acid can be effectively resisted. The multi-module double-screw extruder connected with the reaction tank in series has the functions of steam flocculation, water washing and drying, so that the flocculation cost is reduced, and the influence of the addition of a flocculating agent on the rubber performance is avoided; and the double screws and the vacuum pump are combined to dehydrate and dry the rubber, so that the drying effect is good, the efficiency is high, and the continuous and full-production chain preparation of the epoxidized natural rubber product is finally realized.
The method realizes the whole process from reaction to solidification to final water washing and drying, solves the problems of strong corrosion of the epoxidized natural latex to equipment, difficult flocculation and high flocculation cost, can rapidly dehydrate and dry the rubber block to carry out continuous production, simplifies the production flow, reduces the production cost and greatly improves the production efficiency.
300kg of materials are fed once by adopting the device, and the epoxy degree of the epoxidized natural rubber with the epoxy degree of less than 25mol percent can be controlled within +/-2 percent of a theoretical value; the epoxidization degree of the epoxidized natural rubber with the epoxidization degree of 25-60 mol% can be controlled within +/-3% of a theoretical value. The precision is slightly higher than that of the prior art by 1-2 percentage points. The accuracy of the epoxy level is higher because the temperature control is finer.
Drawings
FIG. 1 is a schematic view of the structure of the apparatus of the present invention.
1-a reaction tank body; 2-steam flocculation section; 3-water washing section; 4-a drying section; 5-a feed inlet; 6-stirring shaft; 7-a discharge hole of the tank body; 8-steam flocculation section feed inlet; 9-a steam inlet; 10-water inlet; 11-a vacuum air pump pumping port; 12-a discharge hole; 13-condensation circulating water inlet; 14 condensation circulating water outlet.
Detailed Description
While the present invention will be described in detail with reference to the following examples, it should be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the present invention.
The integrated device for preparing epoxidized natural rubber used in the embodiment of the present invention is specifically shown in fig. 1. The invention relates to a drying integrated device for preparing epoxidized natural rubber, which comprises a reaction tank body 1 and a multi-module double-screw extruder; the multi-module double-screw extruder is connected with a discharge port of the reaction tank body.
The multi-module double-screw extruder sequentially comprises a steam solidifying section 2, a water washing section 3 and a drying section 4 according to the feeding sequence.
The steam solidification section comprises a feed inlet 8, a steam inlet 9 and a flocculation screw module, and the flocculation screw module is specifically designed in such a way that the clearance between a screw and a charging barrel is 0.35mm, and the clearance between screws is 1.5 mm; the length of the screw is 1.5 m; the washing section comprises a water inlet 10 and a washing screw module, and the washing screw module is specifically designed to have a screw-material barrel gap of 0.35mm, a screw-material barrel gap of 1mm and a screw length of 1.5 m; the drying section comprises a vacuum pump air suction opening 11 and a drying screw module, the drying screw module is specifically designed to have a screw and material cylinder gap of 0.35mm, a screw gap of 1mm and a screw length of 3 m.
A feed inlet 5 is formed in a tank cover at the top of the reaction tank body 1, a stirring shaft 6 is arranged through the tank cover, the upper end of the stirring shaft 6 is connected with a turbine speed reducing motor outside the tank cover, and the lower end of the stirring shaft extends into the tank body and is connected with a double-hinge paddle type stirring blade; the rotating speed is 120 r/min.
A discharge port 7 of the reaction tank body 1 is connected with a feed port 8 of a steam solidification section 2 of the double-screw extruder, and a steam inlet 9 is arranged at the upper part of the steam solidification section; the upper part of the washing section 3 is provided with a water inlet 10; the upper part of the drying section 4 is provided with a vacuum air pump pumping hole 11, and the tail part is provided with a discharge hole 12.
The reactor tank body 1 is provided with a hollow outer interlayer, the outer interlayer is provided with an outer interlayer water outlet pipe and an outer interlayer water inlet pipe, and the outer interlayer, the water outlet pipe and the water inlet pipe form an independent water circulation pipeline. The temperature of the circulating pipeline water is 40 ℃. The outer interlayer is provided with a condensation circulating water inlet 13 connected with an outer interlayer water inlet pipe, the outer interlayer is provided with a condensation circulating water outlet 14 connected with an outer interlayer water outlet pipe, and the position of the condensation circulating water outlet 14 is higher than the position of the condensation circulating water inlet 13.
The inner layer of the reaction tank body 1 is made of enamel materials with the thickness of 1 cm; the outer layer of the tank body is made of stainless steel material. And the coating inside the charging barrel of the multi-module double-screw extruder is subjected to anti-corrosion treatment, and the coating is a polytetrafluoroethylene coating. The surface of a stainless steel screw in the multi-module double-screw extruder is subjected to anti-corrosion treatment; the screw block is a Cr12MoV material meshing block, and the surface of the screw block is subjected to anti-corrosion treatment.
Example 1
When the device is used, 300kg of materials are firstly added into a reaction tank body 1 of the device, circulating water with the temperature of 40 ℃ is introduced into an interlayer of the device to heat the materials, a motor is started to drive a stirring shaft 6 to rotate, and the circulating water in the interlayer exchanges heat with the materials under the condition of continuous stirring and rotation, so that the temperature of the materials is gradually increased to the temperature of 40 ℃ required by the reaction and is maintained at +/-3 ℃. The reaction time was set to 6 hours to prepare an epoxidized natural rubber having an epoxidization degree of 25%. After the set reaction time is reached, adding a neutralizing agent to terminate the reaction, discharging the materials into a steam solidification section 2, wherein the steam pressure in the steam solidification section is 0.5MPa, the steam introduction amount is 30Kg/h, the steam temperature is 120 ℃, and the high-temperature steam entering from a steam inlet 9 is directly contacted with latex to break the emulsion and solidify the latex. The solidified rubber block enters the water washing section 3 at room temperature, and residual reagent in the rubber block is washed out by water flow entering from the water inlet 10 under the shearing and mixing of the screw. And (3) feeding the washed rubber block into a drying section 4, wherein the temperature of the drying section is 110 ℃, extruding the moisture of the rubber block through high-temperature shearing extrusion, pumping out the residual moisture through an air pumping port 11 by using a vacuum pump, and then discharging the moisture from a discharge port 12, wherein the rotating speed of a screw of the multi-module double-screw extruder is 20r/min, so as to obtain the solidified and dried epoxidized natural rubber ENR 25B. The epoxide content obtained after nuclear magnetic testing of the prepared epoxidized natural rubber was 23.6%, which was within a theoretical range of ± 2%.
Example 2
When the device is used, 300kg of materials are firstly added into a reaction tank body 1 of the device, circulating water with the temperature of 40 ℃ is introduced into an interlayer of the device to heat the materials, a motor is started to drive a stirring shaft 6 to rotate, and the circulating water in the interlayer exchanges heat with the materials under the condition of continuous stirring and rotation, so that the temperature of the materials is gradually increased to the temperature of 40 ℃ required by the reaction and is maintained at +/-3 ℃. The reaction time was set to 12 hours to prepare an epoxidized natural rubber having an epoxidization degree of 50%. After the set reaction time is reached, adding a neutralizing agent to terminate the reaction, discharging the materials into a second steam flocculation section 2, wherein the steam pressure in the steam coagulation section is 0.5MPa, the steam introduction amount is 30Kg/h, the steam temperature is 120 ℃, and the high-temperature steam entering from a steam inlet 9 is utilized to directly contact latex to break emulsion and coagulate the latex. The solidified rubber block enters the water washing section 3 at room temperature, and residual reagent in the rubber block is washed out by water flow entering from the water inlet 10 under the shearing and mixing of the screw. And (3) feeding the washed rubber block into a drying section 4, wherein the temperature of the drying section is 110 ℃, extruding the moisture of the rubber block through high-temperature shearing extrusion, pumping out the residual moisture through an air pumping port 11 by using a vacuum pump, and then discharging the moisture from a discharge port 12, wherein the rotating speed of a screw of the multi-module double-screw extruder is 20r/min, so as to obtain the solidified and dried epoxidized natural rubber ENR 50B. The epoxide content of the prepared epoxidized natural rubber after nuclear magnetic testing was 51.9%, which was within. + -. 3% of the theoretical value.
Comparative test example
The ENR25C and the ENR50C are prepared by adopting a traditional preparation process. 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 block by using a creper, and after washing, moving the rubber block into an oven to dry to obtain the product.
Table 1 shows the comparison of the performance of ENR25B and ENR50B prepared by the apparatus of the present invention compared to the performance of ENR25C and ENR50C obtained by the conventional preparation process. Wherein the epoxy degree and the proportion of ring-opening substances are characterized by adopting a nuclear magnetic resonance hydrogen spectrum, and the aging performance is characterized under the condition of 100 ℃/48 h. The traditional process has complicated production flow and poor continuity, and the direct heating flocculation can aggravate side reaction and is not beneficial to the stability of products, and the washing effect of a crepe machine is inferior to that of a double screw. 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 faster flocculation process of the invention reduces the ring-opening reaction in the flocculation process, the control of the epoxy degree and the inhibition of the side reaction are obviously better than the traditional process; the aging performance test of the rubber and the rubber is carried out at 150 ℃ for 48 hours, and the invention is obviously superior to the traditional process because the twin-screw water washing is adopted to better remove the acid remained in the rubber.
TABLE 1
| Degree of epoxidation | Open ring ratio of matter | Rate of deterioration of aging properties | ||
| Example 1 | ENR25B | 23.6 | 0.3％ | 31.6％ |
| Conventional process | ENR25C | 26.8 | 0.62％ | 35.3％ |
| Example 2 | ENR50B | 51.9 | 1.5％ | 42.9％ |
| Conventional process | ENR50C | 53.6 | 2.6％ | 47.2％ |
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (10)
1. An integrated device for preparing epoxidized natural rubber comprises a reaction tank body and a multi-module double-screw extruder; the multi-module double-screw extruder is connected with a discharge port of the reaction tank body.
2. The apparatus of claim 1, wherein said multi-module twin screw extruder comprises, in order of feed, a steam-condensing section, a water-washing section, and a drying section.
3. The apparatus of claim 2,
the steam solidification section comprises a feed inlet, a steam inlet and a flocculation screw module, wherein a clearance between a screw and a charging barrel in the flocculation screw module is 0.3-0.4 mm, a clearance between screws is 1.5-2 mm, and the length of the screw is 1-1.5 m;
the washing section comprises a water inlet and a washing screw module, the clearance between a screw and a charging barrel in the washing screw module is 0.3-0.4 mm, the clearance between the screws is 1-1.2 mm, and the length of the screw is 1-1.5 m;
the drying section comprises a vacuum pump exhaust opening and a drying screw module, the clearance between a screw and a charging barrel in the drying screw module is 0.3-0.4 mm, the clearance between the screws is 1-1.2 mm, and the length of the screw is 2-3 m;
the length ratio of the steam solidifying section to the water washing section to the drying section is 1 (1-1.2) to 2-2.2; wherein the length of the steam solidified section is less than or equal to 1.5 m.
4. The apparatus of claim 1,
a feed inlet is formed in the tank cover at the top of the reaction tank body, a stirring shaft is arranged through the tank cover, the upper end of the stirring shaft is connected with a motor outside the tank cover, and the lower end of the stirring shaft extends into the tank body and is connected with a stirring blade; and/or the presence of a gas in the gas,
the discharge port of the reaction tank body is connected with the feed port of the steam solidifying section of the double-screw extruder, and the upper part of the steam solidifying section is provided with a steam inlet; the upper part of the washing section is provided with a water inlet; the upper part of the drying section is provided with a vacuum air pump exhaust port, and the tail part is provided with a discharge port; and/or the presence of a gas in the atmosphere,
the reactor tank body is provided with a hollow outer interlayer, the outer interlayer is provided with an outer interlayer water outlet pipe and an outer interlayer water inlet pipe, and the outer interlayer, the water outlet pipe and the water inlet pipe form an independent water circulation pipeline.
5. The device according to claim 4, wherein the outer interlayer is provided with a condensed circulating water inlet connected with a water inlet pipe of the outer interlayer, the outer interlayer is provided with a condensed circulating water outlet connected with a water outlet pipe of the outer interlayer, and the position of the condensed circulating water outlet is higher than the position of the condensed circulating water inlet.
6. The apparatus of claim 1,
the inner layer of the reaction tank body is made of enamel materials, and the enamel materials with the thickness of 0.8-2cm are further preferably selected; the outer layer of the tank body is made of a metal material, and is preferably made of a stainless steel material; and/or the presence of a gas in the atmosphere,
the inside of the charging barrel of the multi-module double-screw extruder is subjected to anti-corrosion treatment, and a polytetrafluoroethylene coating is preferably selected as the coating; and/or the presence of a gas in the gas,
the surfaces of the screws and the screw blocks in the multi-module double-screw extruder are subjected to anti-corrosion treatment, and stainless steel screws or polytetrafluoroethylene screws are preferably selected.
7. The apparatus of claim 1, wherein the stirring blade is a double-folded paddle stirring blade; and/or the motor is a turbine speed reducer.
8. An integrated apparatus for producing epoxidized natural rubber, a method for producing epoxidized natural rubber according to any one of claims 1 to 7.
9. The method of claim 8,
the reaction temperature of the reaction tank body is 35-45 ℃, and preferably 38-42 ℃; and/or the presence of a gas in the gas,
the reaction time of the reaction tank body is 4-15 hours, and preferably 6-12 hours.
10. The method of claim 8,
the steam pressure in the steam solidifying section is 0.5-0.7MPa, the steam introducing amount is 50-60Kg/h, and the steam temperature is 140-170 ℃; and/or
The temperature of the washing section is 20-30 ℃, and room temperature is preferred;
the heating temperature of the twin-screw in the drying section is 110-120 ℃, and the preferable temperature is 115-120 ℃;
the screw rotating speed of the multi-module double-screw extruder is 10-25 r/min, and preferably 10-15 r/min.
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| CN109569477A (en) * | 2018-11-09 | 2019-04-05 | 杨建强 | A kind of Screw Extrusion-autoclave stirring combination type reactor and its application |
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