CN111875719A - Micro-interface reinforced reaction system and method for preparing rubber - Google Patents
Micro-interface reinforced reaction system and method for preparing rubber Download PDFInfo
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- CN111875719A CN111875719A CN202010555082.1A CN202010555082A CN111875719A CN 111875719 A CN111875719 A CN 111875719A CN 202010555082 A CN202010555082 A CN 202010555082A CN 111875719 A CN111875719 A CN 111875719A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 46
- 229920001971 elastomer Polymers 0.000 title claims abstract description 45
- 239000005060 rubber Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 48
- 239000002994 raw material Substances 0.000 claims abstract description 45
- 239000000463 material Substances 0.000 claims abstract description 37
- 239000007791 liquid phase Substances 0.000 claims abstract description 25
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- 238000005728 strengthening Methods 0.000 claims abstract description 20
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- 238000001035 drying Methods 0.000 claims abstract description 18
- 238000007701 flash-distillation Methods 0.000 claims abstract description 12
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- 238000007599 discharging Methods 0.000 claims abstract description 4
- 239000004816 latex Substances 0.000 claims description 16
- 229920000126 latex Polymers 0.000 claims description 16
- 238000000926 separation method Methods 0.000 claims description 16
- 238000001704 evaporation Methods 0.000 claims description 14
- 230000008020 evaporation Effects 0.000 claims description 14
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- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000000499 gel Substances 0.000 abstract 2
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- 239000007789 gas Substances 0.000 description 18
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- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 241000196324 Embryophyta Species 0.000 description 7
- -1 ethylene, propylene, butadiene Chemical class 0.000 description 5
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- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical class [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 1
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- 230000008676 import Effects 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical group [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
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- 239000002861 polymer material Substances 0.000 description 1
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- 229910052700 potassium Inorganic materials 0.000 description 1
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- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000010092 rubber production Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical group [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/01—Processes of polymerisation characterised by special features of the polymerisation apparatus used
Abstract
The invention provides a micro-interface strengthening reaction system and a method for preparing rubber. The reaction system comprises: the gas-phase polymerization reactor comprises a mixing tank and a polymerization reactor, wherein the mixing tank is provided with a gas-phase raw material inlet and a mixed raw material outlet, the side wall of the polymerization reactor is provided with a feeding hole, and the bottom of the polymerization reactor is provided with a discharging hole; the mixed raw material outlet is connected with a micro-interface generator, and the micro-interface generator is connected with the feeding hole; the flash distillation device is connected to the discharge gate, the flash distillation device connects the strip tower, the flocculating tank is connected to the bottom of strip tower, the grain groove that gels is connected to the bottom of flocculating tank, the grain tank bottom that gels goes out to connect the drying cabinet. According to the invention, the micro-interface generator is connected to the side wall of the polymerization reactor, so that on one hand, the mass transfer area between a gas phase material and a liquid phase material is increased, the gas utilization rate is high, the reaction efficiency is improved, and the energy consumption is reduced; on the other hand, gas-liquid phase mixing is more uniform, and the obtained rubber molecular weight polymerization degree is more uniform.
Description
Technical Field
The invention relates to the technical field of rubber preparation, in particular to a micro-interface strengthening reaction system and a micro-interface strengthening reaction method for preparing rubber.
Background
The rubber is a high-elasticity polymer material with reversible deformation, is rich in elasticity at room temperature, can generate large deformation under the action of small external force, can recover the original shape after the external force is removed, can be divided into two types of natural rubber and synthetic rubber, the natural rubber is prepared by extracting colloid from plants such as rubber trees, rubber grasses and the like and then processing, and the synthetic rubber is obtained by polymerizing various monomers.
At present, a stirred bed reactor, a kettle reactor, a tubular reactor, a tower reactor and the like are generally adopted in a rubber production process as polymerization reactors, however, the provided phase interface area and mass transfer coefficient are limited, the gas utilization rate is low, so that the reaction efficiency is low, the reaction performance is difficult to obtain breakthrough improvement, and the overall efficiency of the reaction is further influenced; in addition, the uneven distribution of molecular weight caused by uneven mixing between gas and liquid phases, and the low polymerization degree of the obtained rubber affect the quality of products.
Disclosure of Invention
The first purpose of the invention is to provide a micro-interface reinforced reaction system for preparing rubber, which increases the mass transfer area between gas-phase and liquid-phase materials on one hand, has high gas utilization rate, improves the reaction efficiency and reduces the energy consumption by connecting a micro-interface generator on the side wall of a polymerization reactor; on the other hand, gas-liquid phase mixing is more uniform, the obtained rubber molecular weight polymerization degree is more uniform, and the product quality is improved.
The second purpose is to provide a micro-interface strengthening reaction method for preparing rubber by adopting the micro-interface strengthening reaction system, and the rubber obtained by reaction has good quality and high yield.
In order to realize the purpose of the invention, the following technical scheme is adopted:
the invention provides a micro-interface strengthening reaction system for preparing rubber, which comprises a mixing tank and a polymerization reactor, wherein the mixing tank is provided with a gas-phase raw material inlet and a mixed raw material outlet, the side wall of the polymerization reactor is provided with a feeding hole, and the bottom of the polymerization reactor is provided with a discharging hole; the mixed raw material outlet is connected with a micro-interface generator, and the micro-interface generator is connected with the feeding hole; flash distillation plant is connected to the discharge gate in order to be used for the unreacted raw materials and material of flash separation polymerization in-process, flash distillation plant's top is connected with the condenser, flash distillation plant's bottom is provided with and is used for the export of glue solution exhaust isolate resultant, isolate resultant exit linkage stripper is in order to be used for turning into the latex with the glue solution, the latex is followed the bottom of stripper is gone out and is got into the flocculating tank in order to be used for turning into the latex into the pulp, the pulp goes out the entering glue grain groove in order to be used for getting rid of the moisture in the micelle from the bottom of flocculating tank, the micelle goes out the entering drying cabinet in order to be used for getting rid of the micelle.
Further, in the micro-interface reinforced reaction system for preparing rubber, the bottom of the micro-interface generator is provided with a liquid-phase material inlet, the top of the micro-interface generator is connected with a circulating pipe, and the circulating pipe is connected with a condenser and is used for recycling unreacted raw materials and materials which are separated by the flash evaporation device through flash evaporation. And an emulsifier, an activator and a catalyst are introduced into the liquid-phase material inlet.
Further, among the above-mentioned micro-interface strengthening reaction system of preparation rubber, flash distillation device is including the first flash tank and the second flash tank that establish ties in proper order, most unreacted raw materials and the material that first flash tank was used for flash separation, the second flash tank is used for residual unreacted raw materials and the material that flash separation goes out, the separation product export sets up the bottom of second flash tank. By arranging two flash tanks in series, unreacted raw materials and materials can be separated by flash evaporation to the maximum extent under the condition of controlling the production cost.
Further, in the above-mentioned micro-interface strengthening reaction system for preparing rubber, a buffer tank is arranged between the discharge port and the flash evaporation device, the buffer tank is used for buffering a product generated by a reaction in the polymerization reactor, and the product is buffered in the buffer tank so as to enable a more stable feeding to avoid fluctuation and further improve the safety.
Further, in the micro-interface reinforced reaction system for preparing rubber, the first flash tank and the top of the second flash tank are connected with the condenser at the same time. Unreacted raw materials and materials separated by the first flash tank and the second flash tank through flash evaporation are condensed and liquefied by the condenser and then are introduced into the micro-interface generator through the circulating pipe for recycling, so that the production cost is reduced.
Further, in the micro-interface reinforced reaction system for preparing rubber, the drying box is connected with the collecting box and used for collecting the prepared rubber.
Further, in the micro-interface reinforced reaction system for preparing rubber, the top of the stripping tower is provided with an exhaust pipe.
A micro-interface strengthening reaction method for preparing rubber comprises the following steps:
mixing and dispersing the gas-phase raw material and the liquid-phase material into micro bubbles, carrying out polymerization reaction, then carrying out flash evaporation, gas stripping, flocculation, gelling and finally drying.
Further, in the micro-interface strengthening reaction method for preparing the rubber, under the condition of adding the initiator, the temperature of the polymerization reaction is 45-55 ℃; the polymerization temperature is 5-7 ℃ without the addition of initiator.
Further, in the micro-interface strengthening reaction method for preparing the rubber, the pressure of the polymerization reaction is 0.25-0.3 MPa.
It will be appreciated by those skilled in the art that the micro-interface generator used in the present invention is described in the prior patents of the present inventor, such as the patents of application nos. CN201610641119.6, 201610641251.7, CN201710766435.0, CN106187660, CN105903425A, CN109437390A, CN205833127U and CN 207581700U. The detailed structure and operation principle of the micro bubble generator (i.e. micro interface generator) is described in detail in the prior patent CN201610641119.6, which describes that "the micro bubble generator comprises a body and a secondary crushing member, wherein the body is provided with a cavity, the body is provided with an inlet communicated with the cavity, the opposite first end and second end of the cavity are both open, and the cross-sectional area of the cavity decreases from the middle of the cavity to the first end and second end of the cavity; the secondary crushing member is disposed at least one of the first end and the second end of the cavity, a portion of the secondary crushing member is disposed within the cavity, and an annular passage is formed between the secondary crushing member and the through holes open at both ends of the cavity. The micron bubble generator also comprises an air inlet pipe and a liquid inlet pipe. "the specific working principle of the structure disclosed in the application document is as follows: liquid enters the micro-bubble generator tangentially through the liquid inlet pipe, and gas is rotated at a super high speed and cut to break gas bubbles into micro-bubbles at a micron level, so that the mass transfer area between a liquid phase and a gas phase is increased, and the micro-bubble generator in the patent belongs to a pneumatic micro-interface generator.
In addition, the first patent 201610641251.7 describes that the primary bubble breaker has a circulation liquid inlet, a circulation gas inlet and a gas-liquid mixture outlet, and the secondary bubble breaker communicates the feed inlet with the gas-liquid mixture outlet, which indicates that the bubble breakers all need to be mixed with gas and liquid, and in addition, as can be seen from the following drawings, the primary bubble breaker mainly uses the circulation liquid as power, so that the primary bubble breaker belongs to a hydraulic micro-interface generator, and the secondary bubble breaker simultaneously introduces the gas-liquid mixture into an elliptical rotating ball for rotation, thereby realizing bubble breaking in the rotating process, so that the secondary bubble breaker actually belongs to a gas-liquid linkage micro-interface generator. In fact, the micro-interface generator is a specific form of the micro-interface generator, whether it is a hydraulic micro-interface generator or a gas-liquid linkage micro-interface generator, however, the micro-interface generator adopted in the present invention is not limited to the above forms, and the specific structure of the bubble breaker described in the prior patent is only one of the forms that the micro-interface generator of the present invention can adopt.
Furthermore, the prior patent 201710766435.0 states that the principle of the bubble breaker is that high-speed jet flows are used to achieve mutual collision of gases, and also states that the bubble breaker can be used in a micro-interface strengthening reactor to verify the correlation between the bubble breaker and the micro-interface generator; moreover, in the prior patent CN106187660, there is a related description on the specific structure of the bubble breaker, see paragraphs [0031] to [0041] in the specification, and the accompanying drawings, which illustrate the specific working principle of the bubble breaker S-2 in detail, the top of the bubble breaker is a liquid phase inlet, and the side of the bubble breaker is a gas phase inlet, and the liquid phase coming from the top provides the entrainment power, so as to achieve the effect of breaking into ultra-fine bubbles, and in the accompanying drawings, the bubble breaker is also seen to be of a tapered structure, and the diameter of the upper part is larger than that of the lower part, and also for better providing the entrainment power for the liquid phase.
Since the micro-interface generator was just developed in the early stage of the prior patent application, the micro-interface generator was named as a micro-bubble generator (CN201610641119.6), a bubble breaker (201710766435.0) and the like in the early stage, and is named as a micro-interface generator in the later stage along with the continuous technical improvement, and the micro-interface generator in the present invention is equivalent to the micro-bubble generator, the bubble breaker and the like in the prior art, and has different names.
In summary, the micro-interface generator of the present invention belongs to the prior art, although some bubble breakers belong to the type of pneumatic bubble breakers, some bubble breakers belong to the type of hydraulic bubble breakers, and some bubble breakers belong to the type of gas-liquid linkage bubble breakers, the difference between the types is mainly selected according to the different specific working conditions, and in addition, the connection between the micro-interface generator and the reactor and other equipment, including the connection structure and the connection position, is determined according to the structure of the micro-interface generator, which is not limited.
Compared with the prior art, the micro-interface strengthening reaction system for preparing rubber has the advantages that the micro-interface generator is connected to the side wall of the polymerization reactor, so that the mass transfer area between gas-phase and liquid-phase materials is increased, the gas utilization rate is high, the reaction efficiency is improved, and the energy consumption is reduced; on the other hand, gas-liquid phase mixing is more uniform, the obtained rubber molecular weight polymerization degree is more uniform, and the product quality is improved.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
FIG. 1 is a schematic structural diagram of a micro-interfacial strengthening reaction system for preparing rubber according to an embodiment of the present invention.
In the figure:
1-a mixing tank; 11-gas phase raw material inlet;
12-mixed raw material outlet; 2-a polymerization reactor;
21-a micro-interface generator; 22-liquid phase material inlet;
23-a feed inlet; 24-a discharge hole;
3-a buffer tank; 4-a flash evaporation device;
41-a first flash tank; 42-a second flash tank;
43-separation product outlet; 5-a condenser;
51-circulation pipe; 6-a stripping tower;
61-an exhaust pipe; 7-a flocculating tank;
8-a gelatinized granule tank; 9-drying oven;
10-collecting box.
Detailed Description
Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art. It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Referring to fig. 1, a micro-interface reinforcing reaction system for preparing rubber according to an embodiment of the present invention includes: blending tank 1 and polymerization ware 2, be provided with gaseous phase raw materials import 11 and mixed raw materials export 12 on the blending tank 1, polymerization ware 2's lateral wall has been seted up feed inlet 23, and discharge gate 24 has been seted up to the bottom, mixed raw materials export 12 is connected with micro-interface generator 21, micro-interface generator 21 with feed inlet 23 is connected, discharge gate 24 is connected flash distillation plant 4 and is used for the unreacted raw materials and material in the flash separation polymerization process, flash distillation plant 4's top is connected with condenser 5, flash distillation plant 4's bottom is provided with and is used for glue solution exhaust's separation product export 43, separation product export 43 is connected stripper 6 and is used for turning into the latex with the glue solution, the latex is followed the bottom of stripper 6 is gone out and is got into flocculating tank 7 in order to be used for turning into the latex into the pulpiness thing from flocculating tank 7's bottom, the pulpiness goes out to get into gelatinization grain tank 8 and is, the crumb exits the bottom of the crumb tank 8 into a drying box 9 for removing moisture from the crumb.
Specifically, the micro-interface generator 21 plays a role in mixing a gas-phase raw material and a liquid-phase material and dispersing and crushing the gas-phase raw material and the liquid-phase material into micro-bubbles, the gas-phase raw material and the liquid-phase material are fully emulsified in the polymerization reactor 2 and then undergo a polymerization reaction to form a polymerization reaction product, and the polymerization reaction product includes a glue solution, an unreacted raw material and a material.
In this embodiment, the bottom of the micro interface generator 21 is provided with a liquid material inlet 22, the top of the micro interface generator is connected with a circulating pipe 51, and the circulating pipe 51 is connected with a condenser 5 for recycling the unreacted raw materials and materials separated by flash evaporation.
The type of the gas phase raw material is not limited as long as the rubber can be prepared, and any one group of butadiene, butadiene and styrene, butadiene and acrylonitrile through emulsion, ethylene and propylene and the like can be selected. If the materials such as ethylene, propylene, butadiene and the like which are gaseous are added, the materials are directly introduced into the micro-interface generator 21; if liquid substances such as styrene and acrylonitrile are added, butadiene and acrylonitrile can be gasified into gas through emulsion and the like, and then the gas is introduced into the micro-interface generator 21. The gas phase raw materials are fully mixed in the mixing tank 1 and then are sent into the micro-interface generator for dispersion and crushing.
The liquid phase material comprises emulsifier, deoxidizer, reducer and chelateMixture and solvent, etc., the emulsifier is C8-C20Sodium alkyl sulfate, C8-C20Sodium alkyl benzene sulfate, potassium disproportionated rosin, sodium fatty acid, etc. or their mixture; the deoxidizer is sodium disulfite and the like; the reducing agent is ferrous sulfate or chelated iron salt and the like; the chelating agent is ethylenediamine tetraacetic acid or disodium salt thereof and the like.
An initiator can be added into the polymerization reactor 2, and the initiator is K2S208The polymerization reactor 2 is also internally provided with a temperature adjusting device, if K is added2S208In the case of the initiator, the temperature regulating device regulates the temperature in the polymerization reactor 2 to be 45 to 55 ℃; the temperature regulating device regulates the temperature in the polymerization reactor 2 to 5-7 ℃ without the addition of an initiator.
Particularly, be provided with buffer tank 3 between discharge gate 24 and the flash device 4, flash device 4 is including first flash tank 41 and the second flash tank 42 of establishing ties in proper order, first flash tank 41 lateral wall with buffer tank 3's top is connected, first flash tank 41 is used for most unreacted raw materials and the material of flash separation, second flash tank 42 is used for the remaining unreacted raw materials and the material of flash separation, separation product export 43 sets up the bottom of second flash tank 42.
Further, the buffer tank 3 is used for buffering a product generated by the reaction in the polymerization reactor 2, and the product is buffered in the buffer tank 3, so that the more stable feeding is prevented from fluctuating, and the safety is improved.
Further, the first flash tank 41 and the top of the second flash tank 42 are connected with the condenser 5, unreacted raw materials and materials separated by the first flash tank 41 and the second flash tank 42 through flash evaporation are condensed and liquefied by the condenser 5 and then are introduced into the micro-interface generator 21 through the circulating pipe 51 for recycling, the utilization rate of reaction raw materials is increased, and the production cost is reduced.
Specifically, the glue solution discharged from the separated product outlet 43 at the bottom of the second flash tank 42 enters the stripping tower 6, the stripping tower 6 is used for converting the glue solution into latex, and the top of the stripping tower 6 is provided with an exhaust pipe 61 for discharging steam generated in the stripping process in the stripping tower 6.
In this example, the bottom of the column was heated directly with 0.1MPa of steam, the pressure at the top of the column was 12.9kPa, the temperature at the top of the column was 50 ℃, steam was discharged from the top of the column through the vent line 61, and a latex was obtained at the bottom of the column.
Specifically, the latex exits from the bottom outlet of the stripping tower 6 into a flocculation tank 7, and 24% to 26% of a salt solution is added to the flocculation tank 7 for demulsifying the latex into a slurry.
Further, the pulp goes out from the bottom of the flocculating tank 7 and enters a gelatinized granule tank 8, dilute sulfuric acid with the concentration of 0.5 percent by mass is added into the gelatinized granule tank 8, and a stirrer is further arranged in the gelatinized granule tank 8 to generate colloidal particles under the violent stirring of the stirrer.
Specifically, the colloidal particles are discharged from the bottom of the colloidal particle tank 8 and enter a drying box 9, the drying box 9 is a double-layer crawler type and is divided into a plurality of drying chambers, the heating temperature is controlled respectively, the highest temperature in each drying chamber is 90 ℃, and the outlet of each drying chamber is 70 ℃. The track is made for porous corrosion resistant plate, for preventing the micelle bonding, can spray the silicone oil solution at the feed end, and the micelle is scraped down by the scraper at the terminal of upper track and is fallen into second layer track and continue to pass through the drying chamber and dry, and the drying is accomplished promptly to the moisture content of rubber product < 0.1%.
In particular, a collecting box 10 is also included, said collecting box 10 being connected to said drying box 9, said collecting box 10 being intended to collect the rubber produced.
The operation and principle of the reaction system for producing rubber of the present invention will be briefly described below.
Gas-phase raw materials for synthesizing rubber enter a mixing tank from a gas-phase raw material inlet 11, are mixed in the mixing tank 1 and then are discharged from a mixed raw material outlet 12, the mixed raw materials entering through a feeding hole 23 and liquid-phase materials (comprising an emulsifier, a deoxidizer, a reducing agent, a chelating agent, a solvent and the like) entering through a liquid-phase material inlet 22 are mixed in a micro-interface generator 21 and then are dispersed and crushed into micro-bubbles, and the micro-bubbles after dispersion and crushing are introduced into a polymerization reactor 2 for full emulsification and then are subjected to polymerization reaction to obtain a polymerization reaction product; the polymerization reaction product enters the first flash tank 41 through a discharge hole 24 at the bottom of the polymerization reactor 2 for flash separation of most unreacted raw materials and materials in the polymerization reaction product, then enters the second flash tank 42 through a bottom outlet of the first flash tank 41 for flash separation of residual unreacted raw materials and materials to prepare a glue solution, and the unreacted raw materials enter the micro interface generator 21 for recycling after being condensed and liquefied by a condenser 5 connected with the tops of the first flash tank 41 and the second flash tank 42; the glue solution enters the stripping tower 6 through a separation product outlet 43 to be used for converting the glue solution into latex, and water vapor is discharged from an exhaust pipe 61 at the top of the stripping tower 6; the latex exits from the bottom of the stripper 6 into the flocculator tank 7 for converting the latex to a slurry; the pulp exits from the bottom of the flocculator tank 7 into the gelling crumb tank 8 for conversion of the pulp into colloidal particles; the colloidal particles are discharged from the bottom of the colloidal particle tank 8 and enter the drying box 9 to remove moisture in the colloidal particles; the colloidal particles with the moisture removed enter a collection box 10 to finish the preparation of the rubber. Wherein, under the condition that the initiator is added into the polymerization reactor 2, the temperature of the polymerization reaction is 45-55 ℃; in the case of polymerization reactor 2 without addition of initiator, the polymerization temperature is from 5 to 7 ℃.
Therefore, the micro-interface strengthening reaction system for preparing rubber of the invention increases the mass transfer area between gas-phase and liquid-phase materials on one hand by connecting the micro-interface generator 21 with the side wall of the polymerization reactor 2, has high gas utilization rate, improves the reaction efficiency and reduces the energy consumption; on the other hand, gas-liquid phase mixing is more uniform, the obtained rubber molecular weight polymerization degree is more uniform, and the product quality is improved.
So far, the technical solutions of the present invention have been described in connection with the preferred embodiments shown in the drawings, but it is easily understood by those skilled in the art that the scope of the present invention is obviously not limited to these specific embodiments. Equivalent changes or substitutions of related technical features can be made by those skilled in the art without departing from the principle of the invention, and the technical scheme after the changes or substitutions can fall into the protection scope of the invention.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention; various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A micro-interface reinforced reaction system for preparing rubber is characterized by comprising a mixing tank and a polymerization reactor, wherein the mixing tank is provided with a gas-phase raw material inlet and a mixed raw material outlet, the side wall of the polymerization reactor is provided with a feeding hole, and the bottom of the polymerization reactor is provided with a discharging hole;
the mixed raw material outlet is connected with a micro-interface generator, and the micro-interface generator is connected with the feeding hole;
flash distillation plant is connected to the discharge gate in order to be used for the unreacted raw materials and material of flash separation polymerization in-process, flash distillation plant's top is connected with the condenser, flash distillation plant's bottom is provided with and is used for the export of glue solution exhaust isolate resultant, isolate resultant exit linkage stripper is in order to be used for turning into the latex with the glue solution, the latex is followed the bottom of stripper is gone out and is got into the flocculating tank in order to be used for turning into the latex into the pulp, the pulp goes out the entering glue grain groove in order to be used for getting rid of the moisture in the micelle from the bottom of flocculating tank, the micelle goes out the entering drying cabinet in order to be used for getting rid of the micelle.
2. The micro-interface reinforced reaction system for preparing rubber according to claim 1, wherein the micro-interface generator is provided with a liquid phase material inlet at the bottom, and is connected with a circulating pipe at the top, and the circulating pipe is connected with a condenser for recycling unreacted raw materials and materials separated by flash evaporation of the flash evaporation device.
3. The micro-interface strengthening reaction system for preparing rubber according to claim 2, wherein the flash device comprises a first flash tank and a second flash tank which are connected in series in sequence, the first flash tank is used for flash-separating most of the unreacted raw materials and materials, the second flash tank is used for flash-separating the residual unreacted raw materials and materials, and the separation product outlet is arranged at the bottom of the second flash tank.
4. The micro-interface reinforcing reaction system for preparing rubber according to claim 3, wherein a buffer tank is arranged between the discharge port and the flash evaporation device, and the side wall of the first flash evaporation tank is connected with the top of the buffer tank.
5. The micro-interface reinforcing reaction system for preparing rubber of claim 4, wherein the first flash tank and the top of the second flash tank are connected with the condenser at the same time.
6. The system of claim 1, wherein the drying oven is connected to a collection box.
7. The micro-interface reinforcing reaction system for preparing rubber according to claim 1, wherein the top of the stripping tower is provided with an exhaust pipe.
8. The micro-interfacial strengthening reaction method of preparing rubber using the micro-interfacial strengthening reaction system of any one of claims 1 to 7, comprising the steps of:
mixing and dispersing the gas-phase raw material and the liquid-phase material into micro bubbles, carrying out polymerization reaction, then carrying out flash evaporation, gas stripping, flocculation, gelling and finally drying.
9. The micro-interfacial strengthening reaction method for preparing rubber according to claim 8, wherein the temperature of the polymerization reaction is 45-55 ℃ with the addition of the initiator; the polymerization temperature is 5-7 ℃ without the addition of initiator.
10. The micro-interfacial strengthening reaction method for preparing rubber according to claim 8, wherein the pressure of the polymerization reaction is 0.25 to 0.3 MPa.
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| CN102532414A (en) * | 2011-12-21 | 2012-07-04 | 宁波顺泽橡胶有限公司 | Nitrile rubber production process |
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| CN110804112A (en) * | 2019-12-09 | 2020-02-18 | 大庆石化工程有限公司 | Reactant recycling system and chemical reaction system |
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| CN102532414A (en) * | 2011-12-21 | 2012-07-04 | 宁波顺泽橡胶有限公司 | Nitrile rubber production process |
| CN103483483A (en) * | 2012-06-11 | 2014-01-01 | 中国石油化工集团公司 | Stripping device and stripping method for butyl rubber |
| CN106268544A (en) * | 2016-08-05 | 2017-01-04 | 南京大学 | Tower ultra-fine bubble reactor |
| CN207271230U (en) * | 2017-09-05 | 2018-04-27 | 杭州富阳凯尔化工有限公司 | A kind of degasser for latex |
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Application publication date: 20201103 |