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WO2006008902A1 - Procédé servant à produire un polymère - Google Patents

Procédé servant à produire un polymère Download PDF

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Publication number
WO2006008902A1
WO2006008902A1 PCT/JP2005/011332 JP2005011332W WO2006008902A1 WO 2006008902 A1 WO2006008902 A1 WO 2006008902A1 JP 2005011332 W JP2005011332 W JP 2005011332W WO 2006008902 A1 WO2006008902 A1 WO 2006008902A1
Authority
WO
WIPO (PCT)
Prior art keywords
solvent
polymer
isobutylene
producing
block copolymer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2005/011332
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English (en)
Japanese (ja)
Inventor
Tomoyuki Yoshimi
Naoki Furukawa
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kaneka Corp
Original Assignee
Kaneka Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Kaneka Corp filed Critical Kaneka Corp
Priority to JP2006528535A priority Critical patent/JPWO2006008902A1/ja
Publication of WO2006008902A1 publication Critical patent/WO2006008902A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • C08F6/00—Post-polymerisation treatments
    • C08F6/06—Treatment of polymer solutions
    • C08F6/12—Separation of polymers from solutions
    • 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
    • C08F6/00—Post-polymerisation treatments
    • C08F6/001—Removal of residual monomers by physical means
    • C08F6/003—Removal of residual monomers by physical means from polymer solutions, suspensions, dispersions or emulsions without recovery of the polymer therefrom

Definitions

  • the present invention prepares a polymer, particularly an isobutylene block copolymer, as a powdered resin particle or a powdered resin pellet while efficiently removing the solvent contained in the product. Regarding the method.
  • Patent Document 1 discloses a method for producing an isobutylene block copolymer in a mixed solvent in which methyl chloride and methylcyclohexane are combined. It is disclosed.
  • Patent Document 2 discloses an isobutylene block copolymer having an isobutylene polymer block and a styrene polymer block force in a mixed solvent having methylene chloride and hexane power. A manufacturing method is disclosed.
  • a rubbery polymer recovery method employs a method of pelletizing by a submerged cut method after removing a solvent by a thin film evaporator or an extruder or a method of forming a granular material by steam stripping.
  • JP 2002-161109 A proposes a solvent removal method using a twin screw extruder for solvent evaporation of an isobutylene block copolymer.
  • Patent Document 1 US Pat. No. 4,946,899
  • Patent Document 2 Japanese Patent Publication No. 7-59601
  • Patent Document 3 JP-A-8-041123
  • Patent Document 4 Japanese Patent Laid-Open No. 2002-161109
  • the present invention provides a rosin powder granule or cocoon powder of a polymer, particularly an isobutylene block copolymer or cocoon of an isobutylene block copolymer that generates very little alcohol by steam stripping.
  • the object is to provide a method capable of stably producing fat pellets.
  • the present invention is a method for producing a coconut powder granule or a coconut pellet by removing the solvent of the polymer solution, and the solvent of the polymer solution is a primary having 3 to 8 carbon atoms and A mixed solvent of Z or secondary monohalogen ⁇ hydrocarbons and aliphatic and Z or aromatic hydrocarbons containing a polymer in which the catalyst is deactivated and removed from the solution after completion of polymerization.
  • grain In obtaining the body, a surfactant and water are added to the solution, and the liquid is liquid-dispersed by stirring, and the solvent is removed by heating in step (1).
  • the present invention relates to a method for producing a polymer, characterized by heating in the range represented
  • the present invention relates to a method for producing a polymer, wherein the polymer is an isobutylene block copolymer.
  • a preferred embodiment relates to a process for producing an isobutylene block copolymer, wherein the solvent removal temperature power in step (1) is 70 ° C or higher and lower than 130 ° C.
  • the internal temperature is 100 ° C or higher and lower than 160 ° C.
  • the present invention relates to a method for producing a characteristic isobutylene-based block copolymer.
  • isobutylene block copolymer force (A) polymer block mainly composed of isobutylene and (B) polymer block force mainly composed of an aromatic vinyl monomer It is related with the manufacturing method of the isobutylene type block copolymer characterized by the above-mentioned.
  • the present invention relates to a method for producing an isobutylene block copolymer, which is a solvent containing butyl butyl chloride and a solvent power of an isobutylene block copolymer solution.
  • a monohalogen carbonization in a stripping process is performed in order to obtain a polymer, in particular, an isobutylene block copolymer resin powder or resin pellet, while reducing the residual solvent in the product.
  • the decomposition of the hydrogen solvent can be suppressed. In other words, it is possible to suppress the production of alcohol associated with the decomposition of the monohalogen hydrocarbon solvent, and to make it possible to reuse the recovered solvent.
  • FIG. 1 is an explanatory diagram of an apparatus for performing solvent removal and steam stripping according to the present invention. Explanation of symbols
  • the polymer of the present invention is not particularly limited as long as it can be solution-polymerized, but an isobutylene polymer is particularly preferably used.
  • the isobutylene polymer of the present invention is not particularly limited as long as it is a polymer containing isobutylene, but (A) a polymer block mainly composed of isobutylene, and (B) an aromatic vinyl system.
  • the polymer block power isobutylene copolymer composed mainly of monomers is preferred. More specifically, monomers such as isoprene and aromatic vinyl monomers are added in the presence of a Lewis acid catalyst. Those obtained by cationic polymerization together with an initiator can be preferably used.
  • the polymer block composed mainly of isobutylene in (A) is usually a polymer block containing 60% by weight or more, preferably 80% by weight or more of isobutylene units.
  • the polymer block composed mainly of the aromatic bulle monomer (B) is usually a polymer containing 60% by weight or more, preferably 80% by weight or more of the aromatic bule monomer unit. It is a block.
  • the aromatic bur monomer is not particularly limited, and examples thereof include styrene, o-, m- or P-methylstyrene, a-methylstyrene, and indene. These may be used alone or in combination of two or more. Of these, styrene, p-methylstyrene, a- methylstyrene or a mixture thereof is particularly preferable from the viewpoint of cost.
  • the Lewis acid catalyst in the present invention is not particularly limited as long as it can be used for cationic polymerization, and examples thereof include metal halides such as TiCl, BC1, BF, A1C1, and SnCl. Of these, tetrasalt-titanium (TiCl 3) is preferable.
  • polymerization solvent used in the cationic polymerization a mixed solvent of primary and Z or secondary monohalogenated hydrocarbons having 3 to 8 carbon atoms and aliphatic and Z or aromatic hydrocarbons is used. it can.
  • the primary and Z or secondary monohalogenated hydrocarbons having 3 to 8 carbon atoms are not particularly limited, and include methyl chloride, methylene chloride, butyl chloride (1 chlorobutane), black benzene, and the like. Can be mentioned. Of these, butyl chloride is preferred in terms of the balance of the solubility of the isobutylene block copolymer, the ease of detoxification by decomposition, the cost, and the like.
  • the aliphatic and Z or aromatic hydrocarbons are not particularly limited, and examples thereof include pentane, hexane, heptane, octane, cyclohexane, methylcyclohexane, ethylcyclohexane, and toluene. Can be mentioned. One or more selected from the group consisting of methylcyclohexane, ethylcyclohexane and toluene power are particularly preferred.
  • X represents a halogen atom, an alkoxy group having 1 to 6 carbon atoms or an acyloxy group.
  • R 1 and R 2 are the same or different and each represents a monovalent hydrocarbon group hydrogen atom or 1 to 6 carbon atoms, R 1 and R 2 may be different even in the same.
  • R 3 represents a polyvalent aromatic hydrocarbon group or a polyvalent aliphatic hydrocarbon group.
  • n represents a natural number from 1 to 6.
  • Propyl) benzene is also called dicumulant mouth ride.
  • an electron donor component may be allowed to coexist if necessary.
  • examples of such compounds include pyridines, amines, amides, sulfoxides, esters, or metal compounds having an oxygen atom bonded to a metal atom.
  • the respective components are mixed under cooling, for example, at a temperature of 100 ° C or higher and lower than 0 ° C. Especially good for balancing energy costs and polymerization stability. Furthermore, the temperature range is 80 ° C to 1-30 ° C.
  • the number average molecular weight of the isobutylene block copolymer is not particularly limited, but the surface strength such as fluidity, calorific properties, physical properties, etc. is preferably 30000-500000. Especially preferred to be between 50000 and 40 0000! /.
  • the polymer solution containing the isobutylene block copolymer is brought into contact with water or alkali water to deactivate the catalyst to stop the reaction, and then washed with water to obtain a catalyst.
  • a refined dope can be obtained by extracting and removing residues and metal ions.
  • the temperature for deactivation and washing with water is not particularly limited, but is preferably in the range of room temperature to 100 ° C.
  • the amount of water used for deactivation and rinsing is not particularly limited, but the volume ratio of water to the polymer solution is preferably in the range of 1Z10-10.
  • the purified polymer solution obtained in this manner is subsequently subjected to the powder and granule step (1) (also referred to as a crumbization step).
  • the concentration of the resin in the polymer solution is preferably 10-60% by weight by adding the solvent used for polymerization as necessary.
  • the concentration can be adjusted to a desired concentration by using one or more evaporators such as flash evaporation, thin film evaporation, stirring tank, and wet wall type.
  • the polymer solution concentration is high, it can be adjusted to a desired concentration by diluting the solvent.
  • a surfactant and water are added to the purified polymer solution thus obtained, that is, the solution containing the isobutylene block copolymer from which the catalyst has been deactivated and removed, and the mixture is stirred.
  • the resin particles can be obtained by the step (1) in which the solvent is removed by heating while liquid-liquid dispersion.
  • the amount of water to be added is not particularly limited, but it is preferable that the liquid-liquid dispersion has a strength of 0.5 to 4 times that of the polymer solution.
  • the surfactant it is necessary to stably disperse the polymer solution at a high temperature of 70 ° C or higher, and to reduce foaming due to solvent volatilization. It is preferable to use the nonionic surfactant which has. Specific examples include glycerin fatty acid ester, sorbitan ester, propylene glycol fatty acid ester, sucrose fatty acid ester, citrate mono (di or tri) stearate ester, pentaerythritol fatty acid ester, trimethylolpropane fatty acid ester, polyglycerin fatty acid ester.
  • the amount of the nonionic surfactant to be added is not particularly limited, but is preferably 0.05 to 5 parts by weight with respect to the polymer.
  • the amount is less than 0.05 parts by weight, the properties as a surfactant cannot be sufficiently exhibited, and particles are not formed.
  • the amount exceeds 5 parts by weight, the physical properties of the weight body are deteriorated and the problem of foaming in the granular material becomes remarkable, which is not preferable.
  • the refined polymer solution and water are liquid-liquid dispersed in the presence of a nonionic surfactant, and then the solvent is removed by heating (1), whereby fine particles are formed.
  • a vessel equipped with a stirrer is preferably used as the device used for liquid-liquid dispersion by stirring and solvent removal.
  • Arbitrary blades such as screw blades, propeller blades, anchor blades, paddle blades, inclined paddle blades, turbine blades, and large lattice blades can be used. These can be used for the liquid-liquid dispersion operation and the solvent removal operation using the same stirring tank, or after the liquid-liquid dispersion operation is performed in advance to form the dispersion liquid, the solvent removal is subsequently performed in a plurality of stirring tanks. Can also be used.
  • the internal pressure is preferably less than 1.10 times and less than 1.04 times (saturated water vapor pressure calculated from the internal temperature). Since the water is in the can, it cannot be less than 1.000 times. 1. When it is 10 times or more, the mono- and logene ⁇ hydrocarbon solvent for the differential pressure with respect to the saturated water vapor pressure is steam stripping process (2) Disassembled by alcohol This is not preferable because a large amount of sulfite is generated.
  • the liquid temperature in the step (1) is not particularly limited, but is preferably equal to or higher than the azeotropic point of the solvent and water. However, even below the azeotropic point, the solvent can be easily removed by reducing the pressure in the container. Specifically, it is preferably 70 ° C or higher and lower than 130 ° C, more preferably 80 ° C or higher and less than 110 ° C. If it is less than 70 ° C, the solvent removal rate decreases, which is preferable in terms of production efficiency. If the temperature is 130 ° C or higher, the function of the nonionic surfactant is lost and a stable liquid-liquid dispersion system cannot be formed.
  • the aqueous solution containing the obtained rosin powder particles can be further removed by passing through step (2) by a steam stripping operation in which steam is continuously passed through.
  • the vessel used for steam stripping is preferably connected to a pipe for introducing steam, and the method of introducing steam into the stirring vessel is preferably used in the same manner as suspension and solvent removal operations. Further, the steam stripping operation can be carried out by venting steam in the same tank following the removal of the solvent, or can be continued by separately providing a stripping tank.
  • stripping can be performed by bringing steam and a resin slurry into contact with each other by a shelf method.
  • the liquid temperature in the step (2) is not particularly limited, but is preferably 100 ° C or higher and lower than 160 ° C, more preferably 120 ° C or higher and lower than 160 ° C. If it is less than 100 ° C, the solvent removal rate decreases, which is not preferable in terms of production efficiency. If the temperature is 160 ° C or higher, the fusion between the fats and oils is promoted, and a good granular material cannot be obtained.
  • the aqueous solution containing the rosin powder particles after the steam stripping is dehydrated and dried by the step (3) described below.
  • dehydration operations using various filters, centrifuges, and the like can be used.
  • the water content of the dehydrated fat particles after dehydration by this operation is not particularly limited, but it is effective to make it 10 to 50% by weight. is there.
  • the obtained hydrous greaves powder granule is a conductive heat transfer dryer such as a grooved agitator dryer.
  • the rice cake powder is dried by using a hot air heat receiving dryer such as a fluid dryer, etc. It can be a granule.
  • the moisture content in the product powder is not particularly limited, but less than 1% It is preferable to be full.
  • the above-described dehydrated water-containing greaves powder particles or dried product pulverulent particles can be commercialized as rosin pellets using an extruder having a devolatilization mechanism.
  • an extruder having a devolatilization mechanism a single-screw or twin-screw extruder having a vent mechanism can be used.
  • the twin-screw extruder is preferably used from the viewpoint of solvent removal and monomer removal efficiency.
  • the resin discharged from the extruder can be made into a final product by strand cutting, underwater cutting, hot cutting, etc.
  • Molecular weight GPC system manufactured by Waters (column: Shodex K-804 (polystyrene gel) manufactured by Showa Denko KK, mobile phase: black mouth form). The number average molecular weight is expressed in terms of polystyrene.
  • the obtained polymer solution was poured into a large amount of water to stop the reaction. After the reaction was stopped, the polymer solution phase and the aqueous phase were separated with a separating funnel. After the polymer solution phase was washed twice with the same method, it was confirmed that the aqueous layer was neutral, and the polymer solution phase was discharged with a sufficient force to obtain a polymer solution.
  • a pressure-resistant stirrer with a tank volume of 50 liters and an inner diameter of 30 cm is charged with 12.5 liters of pure water and 12.5 liters of the polymer solution obtained in the production example, and 5 parts of nonionic surfactant (polyethylene glycol monostearate) is added. Add lg and seal.
  • the stirrer blade was heated by a jacket while stirring at 400 rpm using a two-stage tilted four-paddle paddle with a blade diameter of 15 cm.
  • Example 2 The same procedure as in Example 1 was performed except that the stripping condition was changed to 160 ° C in the step (2).

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

Abstract

On produit des particules de résine ou des granules de résine d'un polymère, en particulier d'un copolymère en blocs de l'isobutylène, tout en parvenant à réduire la quantité de solvant résiduel dans le produit. Dans le procédé, on empêche un solvant de type hydrocarbure monohalogéné de se décomposer au cours d'une étape de stripping et de produire ainsi un alcool pour pouvoir recycler le solvant devant être récupéré au cours de ce stripping. Le solvant d'une solution de polymère est un solvant mélangé comprenant un hydrocarbure monohalogéné en C3-8 primaire et/ou secondaire et un hydrocarbure aliphatique et/ou aromatique. Avant de produire les particules de résine à partir de la solution contenant un copolymère en blocs de l'isobutylène et obtenue après la polymérisation et après désactivation/séparation du catalyseur, on ajoute un tensioactif et de l'eau à la solution et on chauffe ce mélange pour enlever le solvant tout en agitant pour avoir une dispersion liquide-liquide. Dans cette étape (1), on régule la pression effective de la partie en phase gazeuse dans la cuve pour qu'elle soit dans un intervalle précis.
PCT/JP2005/011332 2004-07-16 2005-06-21 Procédé servant à produire un polymère Ceased WO2006008902A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2006528535A JPWO2006008902A1 (ja) 2004-07-16 2005-06-21 重合体の製造方法

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JP2004-209434 2004-07-16
JP2004209434 2004-07-16

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WO2006008902A1 true WO2006008902A1 (fr) 2006-01-26

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1712569A4 (fr) * 2004-01-29 2008-11-12 Kaneka Corp Procede pour fabriquer la poudre de resine d isobutylene
JP2009249463A (ja) * 2008-04-03 2009-10-29 Kaneka Corp 自動車内装用表皮成形用粉体の製造方法
WO2016136908A1 (fr) * 2015-02-26 2016-09-01 旭硝子株式会社 Procédé de production d'un liquide aqueux contenant un polymère de vinyle et procédé de production d'un agent résistant à l'eau et résistant à l'huile
EP3246341A4 (fr) * 2015-01-16 2018-08-01 C&Cpel Co., Ltd. Appareil de séparation d'un solvant issu d'une étape de polymérisation d'une série de polyoléfines dans une solution à base de catalyseur métallocène, et procédé associé
WO2020203811A1 (fr) * 2019-04-04 2020-10-08 日本ゼオン株式会社 Procédé de désolvatation de solution de polymère
KR20220012156A (ko) * 2020-07-22 2022-02-03 주식회사 엘지화학 용매의 회수 방법 및 회수 장치
EP3971221A4 (fr) * 2020-07-22 2022-09-07 Lg Chem, Ltd. Procédé et appareillage de récupération d'un solvant

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5725309A (en) * 1980-07-23 1982-02-10 Sumitomo Chem Co Ltd Recovery of rubbery polymer from polymer solution
JP2002030192A (ja) * 2000-02-09 2002-01-31 Sekisui Chem Co Ltd トナー用樹脂組成物の製造方法
JP2004155880A (ja) * 2002-11-06 2004-06-03 Kanegafuchi Chem Ind Co Ltd イソブチレン系熱可塑性エラストマー樹脂の製造方法
JP2004269711A (ja) * 2003-03-10 2004-09-30 Kanegafuchi Chem Ind Co Ltd 樹脂粉粒体の製造方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5725309A (en) * 1980-07-23 1982-02-10 Sumitomo Chem Co Ltd Recovery of rubbery polymer from polymer solution
JP2002030192A (ja) * 2000-02-09 2002-01-31 Sekisui Chem Co Ltd トナー用樹脂組成物の製造方法
JP2004155880A (ja) * 2002-11-06 2004-06-03 Kanegafuchi Chem Ind Co Ltd イソブチレン系熱可塑性エラストマー樹脂の製造方法
JP2004269711A (ja) * 2003-03-10 2004-09-30 Kanegafuchi Chem Ind Co Ltd 樹脂粉粒体の製造方法

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1712569A4 (fr) * 2004-01-29 2008-11-12 Kaneka Corp Procede pour fabriquer la poudre de resine d isobutylene
JP2009249463A (ja) * 2008-04-03 2009-10-29 Kaneka Corp 自動車内装用表皮成形用粉体の製造方法
EP3246341A4 (fr) * 2015-01-16 2018-08-01 C&Cpel Co., Ltd. Appareil de séparation d'un solvant issu d'une étape de polymérisation d'une série de polyoléfines dans une solution à base de catalyseur métallocène, et procédé associé
WO2016136908A1 (fr) * 2015-02-26 2016-09-01 旭硝子株式会社 Procédé de production d'un liquide aqueux contenant un polymère de vinyle et procédé de production d'un agent résistant à l'eau et résistant à l'huile
CN107406533A (zh) * 2015-02-26 2017-11-28 旭硝子株式会社 含乙烯基聚合物的水性液体的制造方法及耐水耐油剂的制造方法
JPWO2016136908A1 (ja) * 2015-02-26 2017-12-07 旭硝子株式会社 ビニルポリマー含有水性液の製造方法および耐水耐油剤の製造方法
US10246604B2 (en) 2015-02-26 2019-04-02 AGC Inc. Method for producing vinyl polymer-containing aqueous liquid and method for producing water/oil resistant agent
WO2020203811A1 (fr) * 2019-04-04 2020-10-08 日本ゼオン株式会社 Procédé de désolvatation de solution de polymère
KR20220012156A (ko) * 2020-07-22 2022-02-03 주식회사 엘지화학 용매의 회수 방법 및 회수 장치
EP3971221A4 (fr) * 2020-07-22 2022-09-07 Lg Chem, Ltd. Procédé et appareillage de récupération d'un solvant
KR102535166B1 (ko) 2020-07-22 2023-05-22 주식회사 엘지화학 용매의 회수 방법 및 회수 장치
US11970558B2 (en) 2020-07-22 2024-04-30 Lg Chem, Ltd. Method of recovering solvent and solvent recovery apparatus

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