CN213506695U - Preparation system of alpha olefin-fluorine styrene polymer - Google Patents
Preparation system of alpha olefin-fluorine styrene polymer Download PDFInfo
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- CN213506695U CN213506695U CN201921530863.4U CN201921530863U CN213506695U CN 213506695 U CN213506695 U CN 213506695U CN 201921530863 U CN201921530863 U CN 201921530863U CN 213506695 U CN213506695 U CN 213506695U
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- fluorostyrene
- alpha olefin
- olefin
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- 229920000642 polymer Polymers 0.000 title claims abstract description 99
- 238000002360 preparation method Methods 0.000 title abstract description 18
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 title description 6
- 229910052731 fluorine Inorganic materials 0.000 title description 5
- 239000011737 fluorine Substances 0.000 title description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 163
- 239000000178 monomer Substances 0.000 claims abstract description 110
- 239000004711 α-olefin Substances 0.000 claims abstract description 79
- KBKNKFIRGXQLDB-UHFFFAOYSA-N 2-fluoroethenylbenzene Chemical compound FC=CC1=CC=CC=C1 KBKNKFIRGXQLDB-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000000463 material Substances 0.000 claims abstract description 54
- 238000005406 washing Methods 0.000 claims abstract description 28
- 238000001035 drying Methods 0.000 claims abstract description 22
- 239000000654 additive Substances 0.000 claims abstract description 15
- 230000000996 additive effect Effects 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims description 30
- 239000002904 solvent Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000007790 solid phase Substances 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000003995 emulsifying agent Substances 0.000 claims description 12
- 239000003999 initiator Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000005507 spraying Methods 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- 238000005201 scrubbing Methods 0.000 claims description 4
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 4
- 239000012267 brine Substances 0.000 claims 2
- 239000000839 emulsion Substances 0.000 abstract description 39
- 239000007788 liquid Substances 0.000 abstract description 32
- 238000002156 mixing Methods 0.000 abstract description 10
- 238000006116 polymerization reaction Methods 0.000 abstract description 5
- 238000005728 strengthening Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 18
- 238000000034 method Methods 0.000 description 18
- 238000004945 emulsification Methods 0.000 description 17
- 239000000203 mixture Substances 0.000 description 17
- 230000008569 process Effects 0.000 description 13
- 229920000098 polyolefin Polymers 0.000 description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000012266 salt solution Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 229920006395 saturated elastomer Polymers 0.000 description 5
- JWVTWJNGILGLAT-UHFFFAOYSA-N 1-ethenyl-4-fluorobenzene Chemical group FC1=CC=C(C=C)C=C1 JWVTWJNGILGLAT-UHFFFAOYSA-N 0.000 description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 4
- 239000005977 Ethylene Substances 0.000 description 4
- 239000008280 blood Substances 0.000 description 4
- 210000004369 blood Anatomy 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- SUTQSIHGGHVXFK-UHFFFAOYSA-N 1,2,2-trifluoroethenylbenzene Chemical compound FC(F)=C(F)C1=CC=CC=C1 SUTQSIHGGHVXFK-UHFFFAOYSA-N 0.000 description 2
- YNQXOOPPJWSXMW-UHFFFAOYSA-N 1-ethenyl-2-fluorobenzene Chemical compound FC1=CC=CC=C1C=C YNQXOOPPJWSXMW-UHFFFAOYSA-N 0.000 description 2
- ZJSKEGAHBAHFON-UHFFFAOYSA-N 1-ethenyl-3-fluorobenzene Chemical compound FC1=CC=CC(C=C)=C1 ZJSKEGAHBAHFON-UHFFFAOYSA-N 0.000 description 2
- DPYJMQGTOTVJBV-UHFFFAOYSA-N 2,2-difluoroethenylbenzene Chemical compound FC(F)=CC1=CC=CC=C1 DPYJMQGTOTVJBV-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- -1 ethylene, propylene Chemical group 0.000 description 2
- 238000003682 fluorination reaction Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 2
- 239000013557 residual solvent Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- RVCQPFZUXLKEQS-UHFFFAOYSA-N 5-ethenyl-5-fluorocyclohexa-1,3-diene Chemical compound C=CC1(F)CC=CC=C1 RVCQPFZUXLKEQS-UHFFFAOYSA-N 0.000 description 1
- UDMUNPZCYULHBU-UHFFFAOYSA-N [F].C=Cc1ccccc1 Chemical compound [F].C=Cc1ccccc1 UDMUNPZCYULHBU-UHFFFAOYSA-N 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000003013 cytotoxicity Effects 0.000 description 1
- 231100000135 cytotoxicity Toxicity 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
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- 238000003541 multi-stage reaction Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 230000037048 polymerization activity Effects 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The utility model relates to a preparation system of alpha alkene-fluorobenzene polymer, including monomer storage tank, reaction unit, micro-interface generator, filter, washing unit, drying cabinet and heat exchanger. The utility model discloses a broken alpha olefin monomer makes it form micron order bubble of micron yardstick, each micron order bubble all can form the gas-liquid emulsion with fluorostyrene and additive intensive mixing, through with the gas-liquid double-phase intensive mixing, can guarantee alpha olefin and fluorostyrene in the system and the additive fully contacts, has improved the polymerization efficiency of system; meanwhile, the micron-sized bubbles are mixed with the materials to form gas-liquid emulsion, and the gas-liquid two-phase interfacial area is increased, the thickness of a liquid film is reduced, the mass transfer resistance is reduced, and the effect of strengthening mass transfer within a lower preset operating condition range is achieved.
Description
Technical Field
The utility model relates to a high molecular polymer technical field especially relates to a preparation system of alpha alkene-fluorobenzene ethylene polymer.
Background
The polyolefin has the advantages of no toxicity, chemical reagent resistance, excellent mechanical property and the like, thereby being widely applied, and particularly attracting people's attention in the field of preparing medical appliances. However, the polyolefin has limited its application to some extent due to its poor compatibility with blood. If the compatibility of the compound with blood is improved on the premise of not influencing the mechanical property of the compound, the improvement of the compatibility of the compound with blood is of great significance. Theoretically, the introduction of fluorine into polyolefin can improve the cytotoxicity and blood compatibility of polyolefin, and also improve the chemical stability, air tightness and other properties of polyolefin. In the prior art, fluorine element can be introduced into polyolefin by using methods such as free radical polymerization, metathesis polymerization and the like, but the material prepared by the method has poor performance and higher monomer synthesis cost. Fluorination of polyolefins is a relatively straightforward process, but this process is only effective for fluorination of the surface of materials. Furthermore, copolymerization of olefins and fluorinated olefins to produce fluorinated polyolefins is extremely difficult because the fluoromonomers not only have low polymerization activity but also often result in catalyst deactivation.
Chinese patent publication No.: CN107722155A discloses an α -olefin-fluoro styrene polymer, wherein the content of fluoro styrene structural units in the α -olefin-fluoro styrene polymer is greater than 30 mol%, the glass transition temperature of the α -olefin-fluoro styrene polymer is 0 to 110 ℃, and the average length (MSL) of a continuous fluoro styrene sequence in the α -olefin-fluoro styrene polymer is not shorter than 1 fluoro styrene structural unit. The utility model also provides a preparation method of the alpha olefin-fluoro styrene polymer. It can be seen that although the method can prepare the alpha-olefin-fluorostyrene polymer, the method cannot sufficiently mix the alpha-olefin and the fluorostyrene polymer, and the method has low material conversion rate, thereby resulting in low yield and high preparation cost of the prepared alpha-olefin-fluorostyrene polymer.
Disclosure of Invention
Therefore, the utility model provides a preparation system of alpha olefin-fluoro styrene polymer for overcome the problem that the product yield is low that leads to among the prior art alpha olefin and the unable intensive mixing of fluoro styrene polymer.
In order to solve the above problems, the present invention provides a system for preparing an α -olefin-fluorostyrene polymer, comprising:
a monomer storage tank for storing a monomer to be polymerized;
the reaction unit is connected with the monomer storage tank and is used for respectively receiving materials, a solvent and an additive;
the micro-interface generator is arranged in the reaction unit and is used for crushing the alpha olefin monomer to form micron-sized bubbles with the diameter being more than or equal to 1 mu m and less than 1 mm;
the filter is connected with the discharge port of the reaction unit and is used for filtering the mixed material output by the reaction unit;
the washing unit is connected with the solid phase outlet of the filter and is used for washing the solid phase material output by the filter;
the drying box is connected with the discharge port of the washing unit and is used for drying the washed materials;
and the heat exchangers are respectively arranged at the designated positions in the system and are used for exchanging heat for the materials.
Further, the monomer storage tank includes:
an alpha olefin storage tank for storing an alpha olefin monomer;
the fluorostyrene storage tank is used for storing fluorostyrene monomers.
Further, the reaction unit includes:
the first reaction kettle is a stirring kettle and is respectively connected with the alpha olefin storage tank and the fluorostyrene storage tank and used for respectively receiving an alpha olefin monomer and a fluorostyrene monomer;
and the second reaction kettle is a stirring kettle and is respectively connected with the alpha olefin storage tank and used for conveying the alpha olefin monomer to the interior of the second reaction kettle.
Further, an additive feeding pipe is arranged on the side wall of the first reaction kettle and used for conveying deionized water, an initiator and an emulsifier to the interior of the first reaction kettle;
further, the second reation kettle lateral wall is equipped with material inlet pipe and salt solution inlet pipe, wherein the material inlet pipe with first reation kettle discharge gate links to each other for carry the material of first reation kettle output to inside the second reation kettle, the salt solution inlet pipe is used for carrying the saturated salt solution to inside the second reation kettle.
Further, the micro-interface generator includes:
the first micro-interface generator is arranged at the bottom end in the first reaction kettle, is connected with the alpha olefin storage tank and is used for crushing alpha olefin monomers into micron-sized bubbles;
the second micro-interface generator is arranged at the bottom end in the second reaction kettle, is connected with the alpha olefin storage tank and is used for crushing alpha olefin monomers into micron-sized bubbles;
further, the heat exchangers are respectively arranged at the discharge port of the first reaction kettle and the discharge port of the second reaction kettle and used for respectively exchanging heat for the materials output by the first reaction kettle and the second reaction kettle.
Further, the washing unit includes:
a first scrubber connected to the filter for washing the alpha olefin-fluorostyrene polymer filtered by the filter;
and a second scrubber connected to the first scrubber for performing a secondary scrubbing of the alpha olefin-fluorostyrene polymer output from the first scrubber.
Furthermore, a feeding spray nozzle is arranged at the top of the first scrubber and used for spraying boiling water to the surface of the alpha olefin-fluoro styrene polymer.
Further, a feeding spray nozzle is arranged at the top of the second scrubber and used for spraying ethanol on the surface of the alpha olefin-fluoro styrene polymer.
Compared with the prior art, the utility model has the advantages that the utility model discloses a broken alpha olefin monomer makes it form micron order bubble of micron yardstick, each micron order bubble all can form the gas-liquid emulsion with fluorostyrene and additive intensive mixing, through with the gaseous-liquid double-phase intensive mixing, can guarantee alpha olefin in the system and fluorostyrene and additive intensive contact, improved the polymerization efficiency of system; meanwhile, the micron-sized bubbles are mixed with the materials to form gas-liquid emulsion, and the gas-liquid two-phase interfacial area is increased, the thickness of a liquid film is reduced, the mass transfer resistance is reduced, and the effect of strengthening mass transfer within a lower preset operating condition range is achieved.
In addition, the range of the preset operation condition can be flexibly adjusted according to different product requirements or different additives, so that the full and effective reaction is further ensured, the reaction rate is further ensured, and the purpose of strengthening the reaction is achieved.
Further, the utility model discloses a multistage reaction, through using a plurality of reactors, the conversion of the material in can effective control system makes the heat that emits when the material reaction fall into several stages and emits to effectively reduced the load of system, improved the operating efficiency of system.
In particular, stirred tanks are selected for the first reactor and the second reactor, the gas-liquid emulsion is stirred by the stirred tanks so that micron-sized bubbles in the gas-liquid emulsion and the solvent are further mixed, and the material conversion rate of the system is further improved by improving the mixing degree of the micron-sized bubbles in the solvent.
Further, still be equipped with the filter in the system, carry out the liquid-solid separation through using the mixture that the filter produced in with the reaction unit, can effectively draw out the solid phase result from the mixing material, improved the operating efficiency of system.
Especially, the system is equipped with two scrubbers, washes the material through using different solution on different scrubbers and can carry out effectual the getting rid of to the adnexed solution of remaining in material surface to the purity of result has been improved.
Especially, still be equipped with the drying cabinet in the system, dry through the material to after the washing, can further get rid of the solution on material surface to further improved the purity of system's result has improved the result productivity of system.
Especially, assigned position in the system still is equipped with the heat exchanger, sets up the heat exchanger through locating the assigned position in many places, can effectively reduce the temperature load of system in the operation process, has improved the operating efficiency of system.
Drawings
Fig. 1 is a schematic structural diagram of a preparation system of an α -olefin-fluorostyrene polymer according to the present invention.
Detailed Description
Preferred embodiments of the present invention will be described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only for explaining the technical principle of the present invention, and do not limit the scope of the present invention.
It should be noted that in the description of the present invention, the terms of direction or positional relationship indicated by the terms "upper", "lower", "left", "right", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, which are only for convenience of description, and do not indicate or imply that the device or element must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
Furthermore, it should be noted that, in the description of the present invention, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; 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 meaning of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Fig. 1 is a schematic structural diagram of a system for preparing an α -olefin-fluoro styrene polymer according to the present invention. Comprises a monomer storage tank 1, a reaction unit 2, a micro-interface generator 3, a filter 4, a washing unit 5, a drying box 6 and a heat exchanger 7. Wherein the reaction unit 2 is connected with the monomer storage tank 1 and is used for receiving the monomer raw material output by the monomer storage tank 1. The micro-interface generator 3 is arranged in the reaction unit 2 and connected with the monomer storage tank 1, and is used for crushing the alpha olefin monomer into micron-sized bubbles, and outputting the micron-sized bubbles to the reaction unit 2 after crushing. The filter 4 is connected with the reaction unit 2 and is used for filtering the materials output by the reaction unit 2. The washing unit 5 is connected to the filter 4 for washing the solid phase polymer output from the filter 4. The drying cabinet 6 is connected to the washing unit 5 for drying the washed polymer output from the washing unit 5. The heat exchangers 7 are respectively arranged at the discharge outlets of the reaction kettles of the reaction unit 2 and are used for exchanging heat of the materials output by the reaction kettles.
Before the system operates, conveying monomer raw materials into the monomer storage tank 1, and respectively adding a solvent and an additive into corresponding reaction kettles in the reaction unit 2; after the addition is finished, the system starts to operate, the monomer storage tank 1 conveys the alpha olefin monomer in the monomer raw material to the micro-interface generator 3, and the micro-interface generator 3 breaks the alpha olefin monomer into micron-sized bubbles and outputs the micron-sized bubbles to the reaction unit 2; the micron-sized bubbles are mixed with a solvent and an additive to form a gas-liquid emulsion, the mixed gas-liquid emulsion is stirred for a specified time and then is kept stand to pre-emulsify the gas-liquid emulsion, after pre-emulsification, the reaction unit 2 is heated and is continuously stirred to emulsify the gas-liquid emulsion, after emulsification, the materials are demulsified, and the demulsified materials are conveyed to the filter 4; in the conveying process, the heat exchanger 7 exchanges heat with the material to reduce the heat load of the system; the filter 4 filters the material to extract solid-phase polymers from the material, after filtration, the filter 4 conveys the solid-phase polymers to the washer 5, the washer 5 sprays a solvent to wash the solid-phase polymers, after washing, the washer 5 conveys the polymers to the drying box 6, and the drying box 6 dries the polymers to remove residual solution on the surfaces of the polymers. It will be understood by those skilled in the art that the system can be used not only for the preparation of alpha olefin-fluorostyrene polymers, but also for the polymerization of other kinds of organic materials, provided that the system is capable of achieving its specified operating conditions.
Referring to fig. 1, the monomer storage tank 1 of the present invention includes an alpha olefin storage tank 11 and a fluorostyrene storage tank 12. Wherein the alpha olefin storage tank 21 is connected to the micro-interface generator 3 for delivering the stored alpha olefin monomer to the micro-interface generator 3. The storage tank 12 for fluorostyrene is connected to the reaction unit 2 for transferring the stored fluorostyrene monomer to the reactor 2. It is understood that the sizes and materials of the α -olefin storage tank 11 and the fluorostyrene storage tank 12 are not particularly limited in this embodiment, as long as the α -olefin storage tank 11 can store the specified amount of α -olefin monomer, and the fluorostyrene storage tank 12 can store the specified amount of fluorostyrene monomer.
Specifically, the discharging pipeline of the alpha olefin storage tank 11 is provided with branches for respectively conveying the alpha olefin monomers to each reaction kettle in the reactor 2.
Referring to fig. 1, the reactor 2 of the present invention includes a first reaction vessel 21 and a second reaction vessel 22, wherein the first reaction vessel 21 is connected to the alpha olefin storage tank 11 and the fluoro-styrene storage tank 12, respectively, for receiving the alpha olefin monomer and the fluoro-styrene monomer and pre-emulsifying and emulsifying the mixture. The second reaction kettle 22 is connected to the alpha olefin storage tank 11 and the first reaction kettle 21, respectively, and is configured to receive the emulsion output by the first reaction kettle 21 and perform emulsion breaking treatment on the emulsion. When the system is operated, the first reaction kettle 21 respectively receives the alpha olefin micron-sized bubbles, the fluorostyrene monomer, the emulsifier and the deionized water, the materials are mixed to form a gas-liquid emulsion, the gas-liquid emulsion is stirred after the mixing is finished, and the gas-liquid emulsion is stirred and then stands to pre-emulsify the gas-liquid emulsion; after pre-emulsification, adding an initiator, heating the materials, continuously stirring, and standing to emulsify a gas-liquid emulsion; after emulsification, the emulsion is output to the second reaction vessel 22, the emulsion is mixed with the α -olefin micron-sized bubbles and the saturated brine to form a gas-liquid emulsion, the gas-liquid emulsion is stirred to perform emulsion breaking treatment on the gas-liquid emulsion, and the mixed material is output to the filter 4 after emulsion breaking. It is understood that the first reaction vessel 21 and the second reaction vessel 22 may be a stirred vessel, a fluidized bed reactor or other types of reactors or reaction vessels, as long as the first reaction vessel 21 and the second reaction vessel 22 can respectively reach the specified working state.
Specifically, the first reaction kettle 21 is a stirring kettle, and an additive feeding pipe is arranged on the side wall of the first reaction kettle 21 and used for respectively conveying deionized water, an emulsifier and an initiator; a fluorostyrene feeding pipe is arranged above the additive feeding pipe and is connected with the fluorostyrene storage tank 12 to convey a fluorostyrene monomer into the first reaction kettle 21; the bottom of the first reaction kettle 21 is provided with a discharge hole for outputting emulsified emulsion; a first micro-interface generator 31 is arranged on the left side of the discharge port, and the first micro-interface generator 31 is connected with the alpha olefin storage tank 11 and is used for crushing the alpha olefin monomer output from the alpha olefin storage tank 11 into micron-sized bubbles and outputting the micron-sized bubbles to the first reaction kettle 21. When the system is operated, deionized water and an emulsifier are conveyed into a first reaction kettle through an additive feeding pipe, a first micro-interface generator 31 breaks alpha olefin monomers into micron-sized bubbles and outputs the micron-sized bubbles into the first reaction kettle 21, the micron-sized bubbles, the deionized water and the emulsifier are mixed to form a gas-liquid emulsion, and at the moment, the first reaction kettle starts to stir the gas-liquid emulsion and stands after stirring to pre-emulsify the gas-liquid emulsion; and after pre-emulsification is finished, conveying an initiator through an additive feeding pipe, simultaneously heating the gas-liquid emulsion and continuously stirring, and standing after stirring to emulsify the mixed materials.
Specifically, the second reaction kettle 22 is a stirring kettle, a material feeding pipe is arranged on the side wall of the second reaction kettle 22, and the material feeding pipe is connected with the discharge port of the first reaction kettle 22 and is used for conveying the emulsion output by the first reaction kettle 21 to the inside of the second reaction kettle 22; a saline water feeding pipe is arranged above the material feeding pipe and used for conveying saturated saline water to the second reaction kettle 22; a discharge port is arranged at the bottom of the second reaction kettle 22 and used for outputting the demulsified mixed material; a second micro-interface generator 32 is arranged on the left side of the discharge port, and the second micro-interface generator 32 is connected with the alpha olefin storage tank 11 and is used for crushing the alpha olefin monomers output by the alpha olefin storage tank 11 into micron-sized bubbles and outputting the micron-sized bubbles to the second reaction kettle 22. When the system is operated, conveying excessive saturated salt solution into the second reaction kettle 22 through the salt solution feeding pipe, simultaneously conveying the emulsified emulsion into the second reaction kettle 22 through the first reaction kettle 21, and mixing the saturated salt solution and the emulsion to form a mixed solution; after mixing, the second micro-interface generator 32 breaks the alpha olefin into micron-sized bubbles and outputs the micron-sized bubbles to the second reaction kettle 22, the micron-sized bubbles and the mixed solution are mixed to form a gas-liquid emulsion, and at the moment, the second reaction kettle 22 starts to stir the gas-liquid emulsion to break the emulsion of the gas-liquid emulsion, so that the alpha olefin-fluoro styrene monomer in the gas-liquid emulsion is polymerized; after polymerization, the second reaction kettle conveys the mixed materials to the filter 4 through a discharge hole.
As shown in fig. 1, the side wall of the filter 4 of the present invention is provided with a material inlet for receiving the emulsion output from the second reaction vessel 22; the side wall of the filter 4 is also provided with a liquid phase outlet for outputting the filtered liquid phase material; the bottom of the filter 4 is provided with a solid phase outlet for outputting the solid phase α -olefin-fluoro styrene polymer to the washing unit 5. When the system is operated, after the demulsified mixed material is conveyed to the interior of the filter 4 by the second reaction kettle 22, the filter 4 filters the material to separate the solid-phase alpha olefin-fluoro styrene polymer from the mixed material; after separation, the filter 4 outputs the liquid phase material through the liquid phase outlet, the α -olefin-fluorostyrene polymer is discharged out of the filter 4 through the solid phase outlet, and the α -olefin-fluorostyrene polymer is conveyed to the washing unit 5. It is understood that the filter 4 may deliver the α -olefin-fluoro styrene polymer to the washing unit 5 by a conveyor belt, container loading and delivery or other types of delivery, as long as the filter 4 can continuously and uninterruptedly deliver the output α -olefin-fluoro styrene polymer to the washing unit 5.
With continued reference to fig. 1, the washing unit 5 of the present invention includes a first washer 51 and a second washer 52. Wherein a first scrubber 51 is connected to said filter 4 for performing a single scrubbing of the alpha olefin-fluoro styrene polymer delivered by the filter 4. The second scrubber 52 is connected to the first scrubber 51 to perform a second scrubbing of the α -olefin-fluorostyrene polymer output from the first scrubber 51. After the filter 4 delivers the α -olefin-fluorostyrene polymer to the first scrubber 51, the first scrubber 51 performs one washing of the α -olefin-fluorostyrene polymer; after the washing, the first scrubber 51 transfers the α -olefin-fluorostyrene polymer to the second scrubber 52, the second scrubber 52 performs a second washing of the α -olefin-fluorostyrene polymer, and after the washing is completed, the second scrubber 52 transfers the α -olefin-fluorostyrene polymer to the drying cabinet 6. It is to be understood that the size and type of the first scrubber 51 and the second scrubber 52 are not particularly limited in this embodiment, as long as the first scrubber 51 and the second scrubber 52 can scrub the α -olefin-fluoro styrene polymer.
Specifically, the first scrubber 51 is provided with a feed inlet at a side thereof for receiving the α -olefin-fluoro styrene polymer, and a feed nozzle at a top of the first scrubber 51 for spraying boiling water into the first scrubber 51. After the α -olefin-fluorostyrene polymer is supplied to the interior of the first scrubber 51, the first scrubber 51 supplies boiling water through the feed nozzle, and the boiling water is sprayed on the surface of the α -olefin-fluorostyrene polymer to wash the α -olefin-fluorostyrene polymer to remove residual solvent attached to the surface of the α -olefin-fluorostyrene polymer.
Specifically, the second scrubber 52 has a feed inlet at a side thereof for receiving the α -olefin-fluoro styrene polymer, and a feed nozzle at a top of the second scrubber 52 for spraying ethanol into the second scrubber 52. After the α -olefin-fluorostyrene polymer is transferred to the interior of the second scrubber 51, the second scrubber 52 transfers ethanol through the feed nozzle, and the ethanol is sprayed on the surface of the α -olefin-fluorostyrene polymer to perform a second washing on the α -olefin-fluorostyrene polymer, so as to further remove the residual solvent attached to the surface of the α -olefin-fluorostyrene polymer.
Referring to fig. 1, the drying box 6 of the present invention is a vacuum drying box for drying the α -olefin-fluoro-styrene polymer output from the second scrubber 52. When the second scrubber 52 outputs the washed α -olefin-fluorostyrene polymer to the drying box 6, the drying box 6 dries the α -olefin-fluorostyrene polymer to remove it, and after drying, the drying box 6 outputs the dried α -olefin-fluorostyrene polymer to the system. It should be understood that the drying box 6 of the present invention may be a vacuum drying box, a forced air drying box, an electronic drying box or other types of drying boxes, as long as the drying box 6 can dry the α -olefin-fluoro-styrene polymer.
In order to make the objects and advantages of the present invention more apparent, the present invention will be further described with reference to the following embodiments; it should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example one
Use the system and process of the utility model to carry out the preparation of alpha olefin-fluoro styrene polymer, wherein:
the alpha olefin monomer is ethylene, the fluorostyrene monomer is p-fluorostyrene, the solvent in the first reaction kettle is deionized water, the solvent in the second reaction kettle is saturated salt water, the emulsifier is a mixture of sodium dodecyl sulfate, sodium dodecyl sulfate and sodium dodecyl sulfate, and the initiator is hydrogen peroxide solution.
During pre-emulsification, the stirring speed of the first reaction kettle is 100 r/min; during emulsification, the stirring speed of the first reaction kettle is 300r/min, and the reaction temperature is 55 ℃; when demulsifying, the stirring speed of the second reaction kettle is 800r/min, and the reaction pressure is 1 atm.
Respectively detecting an alpha olefin monomer, a fluorostyrene monomer and an alpha olefin-fluorostyrene polymer before and after operation to obtain: the conversion rate of the alpha olefin monomer was 98.6%, the conversion rate of the fluorostyrene monomer was 98.3%, and the purity of the alpha olefin-fluorostyrene polymer was 98.8%.
Example two
Use the system and process of the utility model to carry out the preparation of alpha olefin-fluoro styrene polymer, wherein:
the alpha olefin monomer is ethylene, the fluorostyrene monomer is p-fluorostyrene, the solvent in the first reaction kettle is deionized water, the solvent in the second reaction kettle is saturated salt water, the emulsifier is a mixture of sodium dodecyl sulfate, sodium dodecyl sulfate and sodium dodecyl sulfate, and the initiator is hydrogen peroxide solution.
During pre-emulsification, the stirring speed of the first reaction kettle is 130 r/min; during emulsification, the stirring speed of the first reaction kettle is 320r/min, and the reaction temperature is 58 ℃; when demulsifying, the stirring speed of the second reaction kettle is 850r/min, and the reaction pressure is 3 atm.
Respectively detecting an alpha olefin monomer, a fluorostyrene monomer and an alpha olefin-fluorostyrene polymer before and after operation to obtain: the conversion rate of the alpha olefin monomer is 99.2%, the conversion rate of the fluorostyrene monomer is 98.6%, and the purity of the alpha olefin-fluorostyrene polymer is 99.1%.
Comparative example 1
The preparation of the α -olefin-fluorostyrene polymer was carried out by using the prior art and process, wherein the α -olefin monomer, the fluorostyrene monomer, the solvents in the reaction vessels and the operation parameters of the equipments during the system operation, which were selected in the present comparative example, were the same as those in the above examples.
Respectively detecting an alpha olefin monomer, a fluorostyrene monomer and an alpha olefin-fluorostyrene polymer before and after operation to obtain: the conversion rate of the alpha olefin monomer was 97.3%, the conversion rate of the fluorostyrene monomer was 96.9%, and the purity of the alpha olefin-fluorostyrene polymer was 97.6%.
EXAMPLE III
Use the system and process of the utility model to carry out the preparation of alpha olefin-fluoro styrene polymer, wherein:
the alpha olefin monomer is a mixture of ethylene and propylene, the fluorostyrene monomer is a mixture of o-fluorostyrene, p-fluorostyrene and m-fluorostyrene, the solvent in the first reaction kettle is deionized water, the solvent in the second reaction kettle is saturated saline, the emulsifier is a mixture of sodium dodecyl sulfate, sodium dodecyl sulfate and sodium dodecyl sulfate, and the initiator is hydrogen peroxide solution.
During pre-emulsification, the stirring speed of the first reaction kettle is 170 r/min; during emulsification, the stirring speed of the first reaction kettle is 410r/min, and the reaction temperature is 55 ℃; when demulsifying, the stirring speed of the second reaction kettle is 900r/min, and the reaction pressure is 5 atm.
Respectively detecting an alpha olefin monomer, a fluorostyrene monomer and an alpha olefin-fluorostyrene polymer before and after operation to obtain: the conversion rate of the alpha olefin monomer was 98.8%, the conversion rate of the fluorostyrene monomer was 98.5%, and the purity of the alpha olefin-fluorostyrene polymer was 98.9%.
Example four
Use the system and process of the utility model to carry out the preparation of alpha olefin-fluoro styrene polymer, wherein:
the alpha olefin monomer is a mixture of ethylene and propylene, the fluorostyrene monomer is a mixture of o-fluorostyrene, p-fluorostyrene and m-fluorostyrene, the solvent in the first reaction kettle is deionized water, the solvent in the second reaction kettle is saturated saline, the emulsifier is a mixture of sodium dodecyl sulfate, sodium dodecyl sulfate and sodium dodecyl sulfate, and the initiator is hydrogen peroxide solution.
During pre-emulsification, the stirring speed of the first reaction kettle is 220 r/min; during emulsification, the stirring speed of the first reaction kettle is 430r/min, and the reaction temperature is 60 ℃; when demulsifying, the stirring speed of the second reaction kettle is 950r/min, and the reaction pressure is 6 atm.
Respectively detecting an alpha olefin monomer, a fluorostyrene monomer and an alpha olefin-fluorostyrene polymer before and after operation to obtain: the conversion rate of the alpha olefin monomer is 99.2%, the conversion rate of the fluorostyrene monomer is 98.9%, and the purity of the alpha olefin-fluorostyrene polymer is 99.4%.
Comparative example No. two
The preparation of the α -olefin-fluorostyrene polymer was carried out by using the prior art and process, wherein the α -olefin monomer, the fluorostyrene monomer, the solvents in the reaction vessels and the operation parameters of the equipments during the system operation, which were selected in the present comparative example, were the same as those in the above example four.
Respectively detecting an alpha olefin monomer, a fluorostyrene monomer and an alpha olefin-fluorostyrene polymer before and after operation to obtain: the conversion rate of the alpha olefin monomer was 97.4%, the conversion rate of the fluorostyrene monomer was 97.1%, and the purity of the alpha olefin-fluorostyrene polymer was 97.6%.
EXAMPLE five
Use the system and process of the utility model to carry out the preparation of alpha olefin-fluoro styrene polymer, wherein:
the alpha olefin monomer is a mixture of ethylene, propylene and butylene, the fluorostyrene monomer is a mixture of difluorostyrene and trifluorostyrene, the solvent in the first reaction kettle is deionized water, the solvent in the second reaction kettle is saturated saline, the emulsifier is a mixture of sodium dodecyl sulfate, sodium dodecyl sulfate and sodium dodecyl sulfate, and the initiator is hydrogen peroxide solution.
During pre-emulsification, the stirring speed of the first reaction kettle is 260 r/min; during emulsification, the stirring speed of the first reaction kettle is 460r/min, and the reaction temperature is 56 ℃; when demulsifying, the stirring speed of the second reaction kettle is 980r/min, and the reaction pressure is 8 atm.
Respectively detecting an alpha olefin monomer, a fluorostyrene monomer and an alpha olefin-fluorostyrene polymer before and after operation to obtain: the conversion rate of the alpha olefin monomer is 99.1%, the conversion rate of the fluorostyrene monomer is 98.9%, and the purity of the alpha olefin-fluorostyrene polymer is 99.1%.
EXAMPLE six
Use the system and process of the utility model to carry out the preparation of alpha olefin-fluoro styrene polymer, wherein:
the alpha olefin monomer is a mixture of ethylene, propylene and butylene, the fluorostyrene monomer is a mixture of difluorostyrene and trifluorostyrene, the solvent in the first reaction kettle is deionized water, the solvent in the second reaction kettle is saturated saline, the emulsifier is a mixture of sodium dodecyl sulfate, sodium dodecyl sulfate and sodium dodecyl sulfate, and the initiator is hydrogen peroxide solution.
During pre-emulsification, the stirring speed of the first reaction kettle is 300 r/min; during emulsification, the stirring speed of the first reaction kettle is 500r/min, and the reaction temperature is 60 ℃; when demulsifying, the stirring speed of the second reaction kettle is 1000r/min, and the reaction pressure is 10 atm.
Respectively detecting an alpha olefin monomer, a fluorostyrene monomer and an alpha olefin-fluorostyrene polymer before and after operation to obtain: the conversion rate of the alpha olefin monomer is 99.3%, the conversion rate of the fluorostyrene monomer is 99.4%, and the purity of the alpha olefin-fluorostyrene polymer is 99.3%.
Comparative example No. three
The preparation of the α -olefin-fluorostyrene polymer was carried out using the prior art and process, wherein the α -olefin monomer, the fluorostyrene monomer, the solvents in the reaction vessels and the operating parameters of the equipments during the system operation, which were selected in this comparative example, were the same as in example six above.
Respectively detecting an alpha olefin monomer, a fluorostyrene monomer and an alpha olefin-fluorostyrene polymer before and after operation to obtain: the conversion rate of the alpha olefin monomer was 97.8%, the conversion rate of the fluorostyrene monomer was 97.6%, and the purity of the alpha olefin-fluorostyrene polymer was 98.2%.
Therefore, use the utility model discloses can effectively improve alpha alkene-fluorine styrene polymer's conversion rate after system and the technology, and can effectively improve alpha alkene monomer and fluorine styrene monomer's conversion rate.
So far, the technical solution of the present invention has been described with reference to 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. Without departing from the principle of the present invention, a person skilled in the art can make equivalent changes or substitutions to the related technical features, and the technical solutions after these changes or substitutions will fall within the protection scope of the present 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 changes may occur 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 system for producing an α -olefin-fluorostyrene polymer, comprising:
a monomer storage tank for storing a monomer to be polymerized;
the reaction unit is connected with the monomer storage tank and is used for respectively receiving materials, a solvent and an additive;
the micro-interface generator is arranged in the reaction unit and is used for crushing the alpha olefin monomer to form micron-sized bubbles with the diameter being more than or equal to 1 mu m and less than 1 mm;
the filter is connected with the discharge port of the reaction unit and is used for filtering the mixed material output by the reaction unit;
the washing unit is connected with the solid phase outlet of the filter and is used for washing the solid phase material output by the filter;
the drying box is connected with the discharge port of the washing unit and is used for drying the washed materials;
and the heat exchangers are respectively arranged at the designated positions in the system and are used for exchanging heat for the materials.
2. The system for preparing an α -olefin-fluorostyrene polymer according to claim 1, wherein said monomer tank comprises:
an alpha olefin storage tank for storing an alpha olefin monomer;
the fluorostyrene storage tank is used for storing fluorostyrene monomers.
3. The system for preparing an α -olefin-fluorostyrene polymer according to claim 2, wherein said reaction unit comprises:
the first reaction kettle is a stirring kettle and is respectively connected with the alpha olefin storage tank and the fluorostyrene storage tank and used for respectively receiving an alpha olefin monomer and a fluorostyrene monomer;
and the second reaction kettle is a stirring kettle and is respectively connected with the alpha olefin storage tank and used for conveying the alpha olefin monomer to the interior of the second reaction kettle.
4. The system for preparing an α -olefin-fluorostyrene polymer according to claim 3, wherein said first reaction vessel has an additive feeding pipe for feeding deionized water, an initiator and an emulsifier into the first reaction vessel.
5. The system for preparing α -olefin-fluoro styrene polymer according to claim 3, wherein the second reaction vessel has a material feeding pipe and a brine feeding pipe on a sidewall thereof, wherein the material feeding pipe is connected to the discharge port of the first reaction vessel for feeding the material discharged from the first reaction vessel to the interior of the second reaction vessel, and the brine feeding pipe is used for feeding the saturated brine to the interior of the second reaction vessel.
6. The system for preparing an α -olefin-fluorostyrene polymer according to claim 3, wherein said micro-interface generator comprises:
the first micro-interface generator is arranged at the bottom end in the first reaction kettle, is connected with the alpha olefin storage tank and is used for crushing alpha olefin monomers into micron-sized bubbles;
and the second micro-interface generator is arranged at the bottom end in the second reaction kettle, is connected with the alpha olefin storage tank and is used for crushing the alpha olefin monomer into micron-sized bubbles.
7. The system for preparing an α -olefin-fluorostyrene polymer according to claim 5, wherein said heat exchangers are respectively disposed at the discharge port of said first reaction vessel and the discharge port of said second reaction vessel, for exchanging heat between the materials output from said first reaction vessel and said second reaction vessel.
8. The system for preparing an α -olefin-fluorostyrene polymer according to claim 1, wherein said washing unit comprises:
a first scrubber connected to the filter for washing the alpha olefin-fluorostyrene polymer filtered by the filter;
and a second scrubber connected to the first scrubber for performing a secondary scrubbing of the alpha olefin-fluorostyrene polymer output from the first scrubber.
9. The system as claimed in claim 8, wherein the top of the first scrubber is provided with a feed nozzle for spraying boiling water onto the surface of the α -olefin-fluorostyrene polymer.
10. The system as claimed in claim 8, wherein the second scrubber is provided at a top thereof with a feed nozzle for spraying ethanol onto the surface of the α -olefin-fluorostyrene polymer.
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