JP2008184510A - Polyvinyl chloride resin composition particle production method - Google Patents
Polyvinyl chloride resin composition particle production method Download PDFInfo
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- JP2008184510A JP2008184510A JP2007017985A JP2007017985A JP2008184510A JP 2008184510 A JP2008184510 A JP 2008184510A JP 2007017985 A JP2007017985 A JP 2007017985A JP 2007017985 A JP2007017985 A JP 2007017985A JP 2008184510 A JP2008184510 A JP 2008184510A
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- polyvinyl chloride
- chloride resin
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- 229920000915 polyvinyl chloride Polymers 0.000 title claims abstract description 260
- 239000004800 polyvinyl chloride Substances 0.000 title claims abstract description 260
- 239000011342 resin composition Substances 0.000 title claims abstract description 197
- 239000002245 particle Substances 0.000 title claims abstract description 185
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 38
- 238000007873 sieving Methods 0.000 claims abstract description 36
- 239000004014 plasticizer Substances 0.000 claims abstract description 29
- 239000002699 waste material Substances 0.000 claims abstract description 26
- 238000001556 precipitation Methods 0.000 claims abstract description 20
- 239000000126 substance Substances 0.000 claims abstract description 14
- 239000011347 resin Substances 0.000 claims description 65
- 229920005989 resin Polymers 0.000 claims description 65
- 239000002904 solvent Substances 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 12
- 239000008187 granular material Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 7
- 229920002554 vinyl polymer Polymers 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 abstract description 12
- 230000001172 regenerating effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 37
- 238000001914 filtration Methods 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 15
- 239000002002 slurry Substances 0.000 description 9
- 150000002576 ketones Chemical class 0.000 description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- 239000000835 fiber Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- -1 earth Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000004576 sand Substances 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 230000001376 precipitating effect Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000007613 slurry method Methods 0.000 description 2
- 239000006057 Non-nutritive feed additive Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229910052570 clay Inorganic materials 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000007602 hot air drying Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Landscapes
- Combined Means For Separation Of Solids (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
【課題】ポリ塩化ビニル樹脂組成物を含む廃棄物を再生して可塑剤を含む顆粒状のポリ塩化ビニル樹脂組成物粒子を製造するポリ塩化ビニル樹脂組成物粒子製造方法において、品質の向上されたポリ塩化ビニル樹脂組成物粒子を効率よく製造し得るポリ塩化ビニル樹脂組成物粒子製造方法を提供することを課題としている。
【解決手段】前記課題を解決すべく、溶解工程、析出工程、乾燥工程を実施して顆粒状のポリ塩化ビニル樹脂組成物粒子を製造する方法であって、前記ポリ塩化ビニル樹脂組成物粒子に混在する粗大物を除去し得るように前記乾燥工程で乾燥されたポリ塩化ビニル樹脂組成物粒子を篩分けする篩分け工程をさらに実施し、しかも、前記ポリ塩化ビニル樹脂組成物粒子の温度が５５℃以下の状態で前記篩分け工程を実施することを特徴とするポリ塩化ビニル樹脂組成物粒子製造方法を提供する。
【選択図】 なしQuality of improvement in a polyvinyl chloride resin composition particle manufacturing method for producing granular polyvinyl chloride resin composition particles containing a plasticizer by regenerating a waste material including a polyvinyl chloride resin composition It is an object of the present invention to provide a method for producing polyvinyl chloride resin composition particles capable of efficiently producing polyvinyl chloride resin composition particles.
In order to solve the above problems, a method for producing granular polyvinyl chloride resin composition particles by performing a dissolution step, a precipitation step, and a drying step, wherein the polyvinyl chloride resin composition particles A sieving step of sieving the polyvinyl chloride resin composition particles dried in the drying step so as to remove mixed coarse substances is further performed, and the temperature of the polyvinyl chloride resin composition particles is 55. Provided is a method for producing polyvinyl chloride resin composition particles, wherein the sieving step is carried out at a temperature of not higher than ° C.
[Selection figure] None
Description
本発明は、ポリ塩化ビニル樹脂と可塑剤とを含むポリ塩化ビニル樹脂組成物が用いられた廃棄物を用いて可塑剤を含むポリ塩化ビニル樹脂組成物により顆粒状に形成されてなるポリ塩化ビニル樹脂組成物粒子を製造するポリ塩化ビニル樹脂組成物粒子製造方法に関する。 The present invention relates to a polyvinyl chloride formed into a granular shape by a polyvinyl chloride resin composition containing a plasticizer using a waste material in which the polyvinyl chloride resin composition containing a polyvinyl chloride resin and a plasticizer is used. The present invention relates to a method for producing polyvinyl chloride resin composition particles for producing resin composition particles.
従来、種々のポリマー製品が広範囲な用途に用いられている。中でも、ポリ塩化ビニル樹脂は、安価で加工性に優れ着色も容易で、耐候性や難燃性にも優れることから広く用いられている。
ところで、ポリ塩化ビニル樹脂は、単体では、硬度が高く溶融粘度も高いことから、通常、可塑剤などとともに使用される。すなわち、“塩ビレジン”などとよばれるポリ塩化ビニル樹脂単体で成形品が形成される場合に比べて、“塩ビコンパウンド”などとよばれる、ポリ塩化ビニル樹脂に可塑剤や安定剤、加工助剤などの各種配合薬剤が混合されたポリ塩化ビニル樹脂組成物が成形品の形成に用いられることが一般的である。
そして、通常、この“塩ビコンパウンド”は、コンパウンドメーカーで押し出し成形や、射出成形などのそれぞれの用途に適した状態に調整されて市販されており、例えば、粒径数ｍｍ程度のペレットや、粒径５００μｍ以下程度のグラニューラ（顆粒）など用途に応じた大きさに粒径が整えられて市販されている。
Conventionally, various polymer products are used in a wide range of applications. Among these, polyvinyl chloride resins are widely used because they are inexpensive, excellent in workability, easy to be colored, and excellent in weather resistance and flame retardancy.
By the way, a polyvinyl chloride resin is usually used together with a plasticizer because it has a high hardness and a high melt viscosity. In other words, compared to the case where a molded product is formed with a single polyvinyl chloride resin called “PVC resin”, plasticizer, stabilizer, and processing aid called “PVC compound” are used. In general, a polyvinyl chloride resin composition mixed with various compounding agents such as is used for forming a molded article.
In general, this “PVC compound” is commercially available after being adjusted to a state suitable for each application such as extrusion molding and injection molding by a compound maker. The particle size is adjusted to a size suitable for the application such as a granule (granule) having a diameter of about 500 μm or less and is commercially available.
この内、ペレットについては、通常、塩ビコンパウンドが押し出し機で押し出されてダイス部でホットカットされたり、ストランド状に押し出されたものが切断されたりして製造される。
一方グラニューラは、液体中にポリ塩化ビニル樹脂組成物で顆粒状の粒子を形成させるスラリー法などによって製造されている。
Of these, the pellets are usually manufactured by extruding a PVC compound with an extruder and hot-cutting at a die part, or cutting a strand-extruded one.
On the other hand, the granule is manufactured by a slurry method or the like in which granular particles are formed with a polyvinyl chloride resin composition in a liquid.
例えば、特許文献１には、このポリ塩化ビニル樹脂組成物を含む廃棄物を再生して再利用すべく、ポリ塩化ビニル樹脂を溶解可能なケトン類などの溶媒に廃棄物に含有されたポリ塩化ビニル樹脂組成物を溶解させてポリ塩化ビニル樹脂溶液を作製し、該ポリ塩化ビニル樹脂溶液と熱水とを接触させることにより、“ポリ塩化ビニル樹脂組成物粒子／水”のスラリーを形成させることが記載されており、このような方法によって、塊状のポリ塩化ビニル樹脂組成物が形成されることを抑制しつつ可塑剤を含有するポリ塩化ビニル樹脂組成物粒子を微細な状態で水中に大量析出させ得ることが記載されている。 For example, in Patent Document 1, in order to recycle and reuse the waste containing the polyvinyl chloride resin composition, the polyvinyl chloride contained in the waste in a solvent such as ketones that can dissolve the polyvinyl chloride resin. A polyvinyl chloride resin solution is prepared by dissolving a vinyl resin composition, and a slurry of “polyvinyl chloride resin composition particles / water” is formed by bringing the polyvinyl chloride resin solution into contact with hot water. By such a method, a large amount of polyvinyl chloride resin composition particles containing a plasticizer is precipitated in water in a fine state while suppressing the formation of a massive polyvinyl chloride resin composition. It is described that it can be made.
また、特許文献２においては、ポリ塩化ビニル樹脂を溶解可能なケトン類などの溶媒にポリ塩化ビニル樹脂組成物を溶解させてポリ塩化ビニル樹脂溶液を作製し、該ポリ塩化ビニル樹脂溶液にアルコールなどを蒸気状態で添加することにより、塊状のポリ塩化ビニル樹脂組成物が形成されることを抑制しつつ、可塑剤や溶剤の含有量が低減されたポリ塩化ビニル樹脂組成物粒子がアルコール中に顆粒状に形成されることが記載されている。 In Patent Document 2, a polyvinyl chloride resin composition is prepared by dissolving a polyvinyl chloride resin composition in a solvent such as ketones capable of dissolving the polyvinyl chloride resin, and alcohol or the like is added to the polyvinyl chloride resin solution. Is added in a vapor state to suppress the formation of a bulky polyvinyl chloride resin composition, and the polyvinyl chloride resin composition particles with reduced plasticizer and solvent content are granulated in alcohol. It is described that it is formed into a shape.
このようなスラリー法により形成されるポリ塩化ビニル樹脂組成物粒子は、通常、スラリーをろ過した後に、ポリ塩化ビニル樹脂組成物粒子に付着する貧溶媒を除去したり、ポリ塩化ビニル樹脂組成物粒子中に残留する溶媒を除去すべく、例えば、ケトン類や水の沸点以上の温度で加熱乾燥する乾燥工程が実施されたりしている。
また、このような場合のみならず、ポリ塩化ビニル樹脂組成物粒子を洗浄したり、湿式での比重分離を実施したりするような各種の工程後にもポリ塩化ビニル樹脂組成物粒子を加熱して乾燥させる乾燥工程が実施されたりしている。
The polyvinyl chloride resin composition particles formed by such a slurry method are usually used after removing the poor solvent adhering to the polyvinyl chloride resin composition particles after filtering the slurry, or the polyvinyl chloride resin composition particles In order to remove the solvent remaining therein, for example, a drying step in which heat drying is performed at a temperature equal to or higher than the boiling point of ketones or water is performed.
Further, not only in such a case, the polyvinyl chloride resin composition particles are also heated after various steps such as washing the polyvinyl chloride resin composition particles or performing specific gravity separation in a wet state. The drying process to dry is implemented.
このポリ塩化ビニル樹脂組成物粒子には、通常、その用途に応じた粒度に調整された質の整えられた状態とされることが求められており、粗大な塊状のポリ塩化ビニル樹脂組成物粒子の混在を抑制することが求められている。
また、ポリ塩化ビニル樹脂組成物を含む廃棄物を再生してポリ塩化ビニル樹脂組成物粒子を製造する場合においては、廃棄物に通常付着している砂や土などをポリ塩化ビニル樹脂組成物粒子に混在させるおそれを有し、これらの混在を抑制することが求められている。
さらに、廃棄物が壁紙やシート部材などの成形品の場合においては、これらに含まれている紙類、繊維質などをポリ塩化ビニル樹脂組成物粒子に混在させるおそれを有し、これらの混在を抑制することが求められている。
このことから、特に、ポリ塩化ビニル樹脂組成物を含む廃棄物を再生してポリ塩化ビニル樹脂組成物粒子を製造する場合には、粗大な塊状のポリ塩化ビニル樹脂組成物粒子の他に、これらの砂、土、紙類、繊維質などがポリ塩化ビニル樹脂組成物粒子へ混在することを防止して再生品の品質を高めることが強く求められている。
The polyvinyl chloride resin composition particles are usually required to be in a state of quality adjusted to a particle size according to the application, and are coarse and massive polyvinyl chloride resin composition particles. It is required to suppress the mixture of
In addition, in the case of producing polyvinyl chloride resin composition particles by recycling the waste containing the polyvinyl chloride resin composition, the polyvinyl chloride resin composition particles are removed from the sand or earth that is normally attached to the waste. Therefore, there is a need to suppress such mixing.
Furthermore, in the case where the waste is a molded product such as wallpaper or a sheet member, there is a possibility that papers, fibers, etc. contained therein may be mixed in the polyvinyl chloride resin composition particles. There is a need to suppress it.
Therefore, in particular, when the polyvinyl chloride resin composition particles are produced by recycling the waste containing the polyvinyl chloride resin composition, in addition to the coarse massive polyvinyl chloride resin composition particles, There is a strong demand to improve the quality of recycled products by preventing sand, earth, paper, fibers, and the like from being mixed into the polyvinyl chloride resin composition particles.
このことに対し塩化ビニル樹脂組成物粒子を作製した後に、粗大な塊状のポリ塩化ビニル樹脂組成物粒子や繊維などといった、粗大物を除去させることが考えられる。
その場合には、より短時間に、しかも、顆粒状のポリ塩化ビニル樹脂組成物粒子が粗大物とともに除去されたりして収率が低下することを防止しつつ粗大物を除去することが求められ、効率よく粗大物を除去することが求められる。
On the other hand, it is conceivable to remove coarse substances such as coarse massive polyvinyl chloride resin composition particles and fibers after producing the vinyl chloride resin composition particles.
In that case, it is required to remove the coarse product in a shorter time and while preventing the granular polyvinyl chloride resin composition particles from being removed together with the coarse product and reducing the yield. Therefore, it is required to remove coarse materials efficiently.
本発明の課題は、ポリ塩化ビニル樹脂組成物を含む廃棄物を再生して可塑剤を含む顆粒状のポリ塩化ビニル樹脂組成物粒子を製造するポリ塩化ビニル樹脂組成物粒子製造方法において、品質の向上されたポリ塩化ビニル樹脂組成物粒子を効率よく製造し得るポリ塩化ビニル樹脂組成物粒子製造方法を提供することにある。 An object of the present invention is to recycle waste containing a polyvinyl chloride resin composition to produce granular polyvinyl chloride resin composition particles containing a plasticizer. An object of the present invention is to provide a method for producing polyvinyl chloride resin composition particles, which can efficiently produce improved polyvinyl chloride resin composition particles.
本発明者は、乾燥工程が実施されるポリ塩化ビニル樹脂組成物粒子製造方法において、乾燥工程後の顆粒状のポリ塩化ビニル樹脂組成物粒子を所定温度以下とすることで篩の通過速度を向上させ得ることを見出し本発明の完成に到ったのである。 The present inventor improved the passing speed of the sieve by setting the granular polyvinyl chloride resin composition particles after the drying step to a predetermined temperature or less in the method for producing polyvinyl chloride resin composition particles in which the drying step is performed. As a result, the present invention has been completed.
すなわち、本発明は、前記課題を解決すべく、ポリ塩化ビニル樹脂と可塑剤とを含むポリ塩化ビニル樹脂組成物が用いられた廃棄物を用いて可塑剤を含むポリ塩化ビニル樹脂組成物により顆粒状に形成されてなるポリ塩化ビニル樹脂組成物粒子を製造すべく、ポリ塩化ビニル樹脂を溶解可能な溶媒に前記廃棄物中に含まれている前記ポリ塩化ビニル樹脂組成物を溶解させてポリ塩化ビニル樹脂溶液を作製する溶解工程と、ポリ塩化ビニル樹脂に対する貧溶媒と前記溶解工程により作製された前記ポリ塩化ビニル樹脂溶液とを混合することにより可塑剤を含むポリ塩化ビニル樹脂組成物で顆粒状に形成されてなるポリ塩化ビニル樹脂組成物粒子を前記貧溶媒中に析出させる析出工程と、前記析出工程で貧溶媒中に析出されたポリ塩化ビニル樹脂組成物粒子を温度が５５℃を超える状態となるように加熱して乾燥させる乾燥工程とを実施するポリ塩化ビニル樹脂組成物粒子製造方法であって、前記ポリ塩化ビニル樹脂組成物粒子に混在する粗大物を除去し得るように前記乾燥工程で乾燥されたポリ塩化ビニル樹脂組成物粒子を篩分けする篩分け工程をさらに実施し、しかも、前記ポリ塩化ビニル樹脂組成物粒子の温度が５５℃以下の状態で前記篩分け工程を実施することを特徴とするポリ塩化ビニル樹脂組成物粒子製造方法を提供する。 That is, in order to solve the above-mentioned problems, the present invention uses a waste product in which a polyvinyl chloride resin composition containing a polyvinyl chloride resin and a plasticizer is used to produce granules by using the polyvinyl chloride resin composition containing a plasticizer. In order to produce the polyvinyl chloride resin composition particles formed in a shape, the polyvinyl chloride resin composition contained in the waste is dissolved in a solvent capable of dissolving the polyvinyl chloride resin, A polyvinyl chloride resin composition containing a plasticizer by mixing a dissolving step for preparing a vinyl resin solution, a poor solvent for the polyvinyl chloride resin, and the polyvinyl chloride resin solution prepared by the dissolving step. A precipitation step of depositing the polyvinyl chloride resin composition particles formed in the poor solvent, and a polyvinyl chloride resin precipitated in the poor solvent in the precipitation step A method for producing a polyvinyl chloride resin composition particle, comprising a drying step of heating and drying the composition particle so that the temperature exceeds 55 ° C., and is mixed in the polyvinyl chloride resin composition particle A sieving step of sieving the polyvinyl chloride resin composition particles dried in the drying step so as to remove coarse substances is further performed, and the temperature of the polyvinyl chloride resin composition particles is 55 ° C. or less. The method for producing polyvinyl chloride resin composition particles is characterized in that the sieving step is carried out in the state described above.
なお、本明細書中における“顆粒状”との用語は、粒径が５００μｍ以下の粒状であることを意図して用いており、この“粒径５００μｍ以下”であるかどうかは、例えば、乾燥状態（含水率１％以下）で、湿度５０％、常温の条件下において、目開き３０メッシュの篩を通過するか否かにより判定することができる。
また、“粗大物”とは、例えば、前記条件で目開き１６メッシュの篩を通過させることが困難な形状を有するものを意図しており、例えば、大きさが１ｍｍを超える紙類、繊維質あるいはポリ塩化ビニル樹脂塩ビ以外の樹脂や、粒径１ｍｍを超える塊状のポリ塩化ビニル樹脂組成物粒子などを意図している。
Note that the term “granular” in this specification is intended to be a particle having a particle size of 500 μm or less, and whether or not the particle size is 500 μm or less is determined by, for example, drying. In the state (moisture content of 1% or less), it can be determined by whether or not it passes through a sieve having a mesh size of 30 mesh under conditions of humidity 50% and room temperature.
The “coarse” is intended to have a shape that is difficult to pass through a sieve having a mesh size of 16 mesh under the above-mentioned conditions. Or resin other than polyvinyl chloride resin polyvinyl chloride, the block-shaped polyvinyl chloride resin composition particle | grains exceeding a particle size of 1 mm, etc. are intended.
本発明によれば、前記ポリ塩化ビニル樹脂組成物粒子を篩分けする篩分け工程を実施することから、粗大物を除去することができポリ塩化ビニル樹脂組成物粒子の品質を向上させ得る。
しかも、篩分け工程をポリ塩化ビニル樹脂組成物粒子の温度が５５℃以下の状態で実施することから顆粒状のポリ塩化ビニル樹脂組成物粒子が篩を通過する速度を向上させ得る。
したがって、より短時間に粗大物を除去させ得る。
しかも、その際には、顆粒状のポリ塩化ビニル樹脂組成物粒子が粗大物に同伴されて除去されたりして収率が低下することをも抑制させ得る。
すなわち、粗大物の混在が抑制された顆粒状のポリ塩化ビニル樹脂組成物粒子を効率よく製造し得る。
According to the present invention, since the sieving step of sieving the polyvinyl chloride resin composition particles is performed, coarse substances can be removed and the quality of the polyvinyl chloride resin composition particles can be improved.
Moreover, since the sieving step is performed in a state where the temperature of the polyvinyl chloride resin composition particles is 55 ° C. or less, the speed at which the granular polyvinyl chloride resin composition particles pass through the sieve can be improved.
Accordingly, coarse materials can be removed in a shorter time.
In addition, in that case, it is possible to suppress the decrease in the yield due to the granular polyvinyl chloride resin composition particles being entrained by the coarse material and being removed.
That is, it is possible to efficiently produce granular polyvinyl chloride resin composition particles in which mixing of coarse products is suppressed.
以下に、本発明の好ましい実施の形態についてポリ塩化ビニル樹脂組成物が用いられた廃棄物から、顆粒状のポリ塩化ビニル樹脂組成物粒子を製造（再生）する場合を例に説明する。 In the following, a preferred embodiment of the present invention will be described by taking as an example the case where granular polyvinyl chloride resin composition particles are produced (regenerated) from waste in which the polyvinyl chloride resin composition is used.
本実施形態におけるポリ塩化ビニル樹脂組成物粒子製造方法においては、（１）ポリ塩化ビニル樹脂と可塑剤とを含むポリ塩化ビニル樹脂組成物により顆粒状に形成されてなるポリ塩化ビニル樹脂組成物粒子が液体中に含有されているスラリーを作製するスラリー作製工程、（２）このスラリーを濾過してポリ塩化ビニル樹脂組成物粒子と液体とをろ別するろ過工程（３）このろ過工程でろ別されたポリ塩化ビニル樹脂組成物粒子を乾燥させるべく加熱する乾燥工程、（４）前記乾燥工程後のポリ塩化ビニル樹脂組成物粒子に混在する粗大物を除去すべく前記ポリ塩化ビニル樹脂組成物粒子を篩分けする篩分け工程を実施する。 In the method for producing polyvinyl chloride resin composition particles in the present embodiment, (1) polyvinyl chloride resin composition particles formed into a granular shape from a polyvinyl chloride resin composition containing a polyvinyl chloride resin and a plasticizer. (2) Filtration step of filtering the slurry to separate the polyvinyl chloride resin composition particles from the liquid (3) Filtration separation in this filtration step A drying step in which the polyvinyl chloride resin composition particles are heated to dry; (4) the polyvinyl chloride resin composition particles in order to remove coarse substances mixed in the polyvinyl chloride resin composition particles after the drying step; A sieving step of sieving is performed.
（１）スラリー作製工程
前記スラリー作製工程においては、（１−ａ）前記廃棄物中に含まれているポリ塩化ビニル樹脂組成物を、ポリ塩化ビニル樹脂を溶解可能な溶媒に溶解させてポリ塩化ビニル樹脂溶液を作製する溶解工程、（１−ｂ）ポリ塩化ビニル樹脂に対する貧溶媒と前記溶解工程により作製された前記ポリ塩化ビニル樹脂溶液とを混合することにより可塑剤を含むポリ塩化ビニル樹脂組成物で顆粒状に形成されてなるポリ塩化ビニル樹脂組成物粒子を前記貧溶媒中に析出させる析出工程を実施して、顆粒状のポリ塩化ビニル樹脂組成物粒子がこの貧溶媒中に含有されているスラリーを作製する。
(1) Slurry preparation step In the slurry preparation step, (1-a) a polyvinyl chloride resin composition contained in the waste is dissolved in a solvent capable of dissolving the polyvinyl chloride resin to obtain a polychlorination. A dissolving step for producing a vinyl resin solution, (1-b) a polyvinyl chloride resin composition containing a plasticizer by mixing a poor solvent for the polyvinyl chloride resin and the polyvinyl chloride resin solution produced by the dissolving step A precipitation step of precipitating polyvinyl chloride resin composition particles formed into granules in a poor solvent, and the granular polyvinyl chloride resin composition particles are contained in the poor solvent. A slurry is prepared.
（１−ａ）溶解工程
前記溶解工程では、例えば、ポリ塩化ビニル樹脂を溶解することのできる溶媒と廃棄物とを攪拌装置が設けられた槽内などで攪拌しつつ混合することによりポリ塩化ビニル樹脂溶液を作製することができる。
このとき、砂、土あるいは金属片などの高比重物を槽底に沈殿させて除去させることができる。
また、ポリ塩化ビニル樹脂組成物に通常含有されている可塑剤は、ポリ塩化ビニル樹脂との高い相溶性を示すフタル酸エステルなどの物質が用いられていることから、ポリ塩化ビニル樹脂を溶解することのできる溶媒にも通常溶解される。
したがって、通常、この溶解工程における溶媒の種類や、ポリ塩化ビニル樹脂溶液の濃度などの条件を適宜選定することにより製造するポリ塩化ビニル樹脂組成物粒子中に含有させる前記可塑剤の量を調整させ得る。
(1-a) Dissolution Step In the dissolution step, for example, polyvinyl chloride is prepared by mixing a solvent capable of dissolving polyvinyl chloride resin and waste while stirring in a tank provided with a stirrer. A resin solution can be prepared.
At this time, high specific gravity such as sand, earth or metal pieces can be precipitated and removed from the bottom of the tank.
In addition, the plasticizer usually contained in the polyvinyl chloride resin composition dissolves the polyvinyl chloride resin because a substance such as a phthalate ester having high compatibility with the polyvinyl chloride resin is used. It is usually dissolved in the solvent that can be used.
Therefore, the amount of the plasticizer to be contained in the polyvinyl chloride resin composition particles to be produced is usually adjusted by appropriately selecting the conditions such as the type of solvent in this dissolution step and the concentration of the polyvinyl chloride resin solution. obtain.
なお、ポリ塩化ビニル樹脂組成物粒子に可塑剤量が５０重量％を超える量で含有されるとポリ塩化ビニル樹脂組成物粒子のタック性が上昇するおそれを有することから、乾燥工程後に篩分け工程で篩分けされるポリ塩化ビニル樹脂組成物粒子の可塑剤含有量を５０％以下とすべくこの溶解工程の条件を選定することで、篩分け工程におけるポリ塩化ビニル樹脂組成物粒子の篩通過速度をより確実に向上させ得るとともに収率の低下をより確実に抑制させ得る。 In addition, since the tackiness of the polyvinyl chloride resin composition particles may be increased if the amount of the plasticizer contained in the polyvinyl chloride resin composition particles exceeds 50% by weight, the sieving step after the drying step By selecting the conditions for this dissolution step so that the plasticizer content of the polyvinyl chloride resin composition particles sieved at 50% or less is selected, the passing speed of the polyvinyl chloride resin composition particles in the sieving step Can be improved more reliably, and a decrease in yield can be more reliably suppressed.
一方で、例えば、ポリ塩化ビニル樹脂組成物に炭酸カルシウム、クレー、水酸化アルミニウムなどの無機微粒子が含有されている場合には、溶媒には溶解されずにポリ塩化ビニル樹脂溶液に分散された状態となる。
これらは、ポリ塩化ビニル樹脂溶液を静置して沈殿させたり、遠心分離したりしてポリ塩化ビニル樹脂溶液から除去することが可能であり、また、一方でポリ塩化ビニル樹脂溶液を攪拌するなどしてこれら無機微粒子がポリ塩化ビニル樹脂溶液に分散されている状態を維持させることも可能である。
したがって、ポリ塩化ビニル樹脂溶液の状態を適宜調整して次段の析出工程に導入することにより析出工程で析出させるポリ塩化ビニル樹脂組成物粒子中に含有させるこれら無機微粒子の量を調整させ得る。
On the other hand, for example, when the polyvinyl chloride resin composition contains inorganic fine particles such as calcium carbonate, clay, and aluminum hydroxide, it is not dissolved in the solvent but is dispersed in the polyvinyl chloride resin solution. It becomes.
These can be removed from the polyvinyl chloride resin solution by allowing the polyvinyl chloride resin solution to settle and centrifuging, while stirring the polyvinyl chloride resin solution, etc. It is also possible to maintain the state in which these inorganic fine particles are dispersed in the polyvinyl chloride resin solution.
Therefore, the amount of the inorganic fine particles to be contained in the polyvinyl chloride resin composition particles precipitated in the precipitation step can be adjusted by appropriately adjusting the state of the polyvinyl chloride resin solution and introducing it into the subsequent precipitation step.
この溶解工程において用いる前記溶媒は、ポリ塩化ビニル樹脂を溶解し得るものであれば特に限定されるものではないが、廃棄物中に、例えば、ポリエチレンやポリプロピレンなどポリ塩化ビニル樹脂以外の樹脂が含有されている場合にこれらに対して溶解性が低いことが望ましく、極性溶媒、特にケトン類が好適である。
このケトン類としては、アセトン、メチルエチルケトン、ジエチルケトンなどが挙げられる。
The solvent used in this dissolving step is not particularly limited as long as it can dissolve the polyvinyl chloride resin, but the waste contains, for example, a resin other than the polyvinyl chloride resin such as polyethylene and polypropylene. When used, it is desirable to have low solubility in these, and polar solvents, particularly ketones are preferred.
Examples of the ketones include acetone, methyl ethyl ketone, and diethyl ketone.
なお、要すれば、この溶解工程においては、ポリ塩化ビニル樹脂組成物の溶解性を高めるべくポリ塩化ビニル樹脂組成物、溶剤あるいは両方を加温した状態で実施させることもできる。 If necessary, this dissolving step can be carried out in a state where the polyvinyl chloride resin composition, the solvent, or both are heated in order to increase the solubility of the polyvinyl chloride resin composition.
また、要すれば、溶解工程において作製したポリ塩化ビニル樹脂溶液をフィルターに通過させるなどしてろ過する溶液ろ過工程を実施することも可能である。
この溶解工程で用いたポリ塩化ビニル樹脂組成物が用いられた廃棄物には、通常、土や砂などが付着している。
また、この廃棄物中にポリ塩化ビニル樹脂組成物が用いられた壁紙やシート材が含まれている場合には、これらには、通常、紙類、繊維質が含有されている。
これら砂、土、紙類、繊維質がポリ塩化ビニル樹脂溶液に混入していたとしても、この溶液ろ過工程を実施することによりこれらの異物を除去することができ、最終的に得られるポリ塩化ビニル樹脂組成物粒子にこれらの異物が混在されるおそれをより確実に抑制させ得る。
Further, if necessary, a solution filtration step of filtering the polyvinyl chloride resin solution prepared in the dissolution step by passing it through a filter can be performed.
In general, soil, sand, or the like is attached to the waste in which the polyvinyl chloride resin composition used in the dissolution step is used.
In addition, when the waste contains a wallpaper or sheet material using the polyvinyl chloride resin composition, these usually contain papers and fibers.
Even if these sand, earth, paper, and fiber are mixed in the polyvinyl chloride resin solution, these foreign substances can be removed by carrying out this solution filtration step, and finally obtained polychlorinated The possibility that these foreign substances are mixed in the vinyl resin composition particles can be more reliably suppressed.
また、廃棄物中にケトン類など溶解工程において用いた溶媒に溶解され難いポリ塩化ビニル樹脂組成物以外の樹脂が混入されていたとしても、この溶液ろ過工程を実施することにより最終的に得られるポリ塩化ビニル樹脂組成物粒子にこれらの異物が混在されるおそれをより確実に抑制させ得る。 Further, even if a resin other than the polyvinyl chloride resin composition that is difficult to dissolve in the solvent used in the dissolution process, such as ketones, is mixed in the waste, it is finally obtained by carrying out this solution filtration process. The possibility that these foreign substances are mixed in the polyvinyl chloride resin composition particles can be more reliably suppressed.
なお、この溶液ろ過工程に用いるフィルターは、目開きが大きすぎると異物を充分に除去できず、また、目開きが小さいと目詰まりを起しやすくなり、処理効率が低下してしまうおそれがあるため目開き１００〜１３０μmのものを利用することが好ましい。 It should be noted that the filter used in this solution filtration step cannot sufficiently remove foreign matter if the opening is too large, and if the opening is small, clogging is likely to occur and processing efficiency may be reduced. Therefore, it is preferable to use a material having an opening of 100 to 130 μm.
（１−ｂ）析出工程
前記析出工程は、ポリ塩化ビニル樹脂に対する貧溶媒と前記溶解工程により作製された前記ポリ塩化ビニル樹脂溶液とを混合することにより前記ポリ塩化ビニル樹脂組成物で顆粒状に形成されてなるポリ塩化ビニル樹脂組成物粒子を前記貧溶媒中に析出させる工程であり、例えば、前記ポリ塩化ビニル樹脂溶液を攪拌装置が設けられた槽内に収容し、前記攪拌装置で槽内を攪拌しつつ、槽内に収容されているポリ塩化ビニル樹脂溶液中に加熱された熱水状態あるいはスチーム状態の水を注入するなどして実施することができる。
(1-b) Precipitation process The said precipitation process granulates with the said polyvinyl chloride resin composition by mixing the poor solvent with respect to a polyvinyl chloride resin, and the said polyvinyl chloride resin solution produced by the said melt | dissolution process. It is a step of precipitating the formed polyvinyl chloride resin composition particles in the poor solvent. For example, the polyvinyl chloride resin solution is contained in a tank provided with a stirrer, and the tank is filled with the stirrer. It can be carried out by injecting heated hot water or steam water into the polyvinyl chloride resin solution accommodated in the tank.
前記貧溶媒としては、上記のような水のほかにアルコール類など、例えば、常温、常圧の状態においてポリ塩化ビニル樹脂を溶解させたときに、溶液中のポリ塩化ビニル樹脂の濃度が１重量％以下、好ましくは、０．１重量％以下となるような液体から選定されることが望ましい。 Examples of the poor solvent include alcohols other than water as described above. For example, when the polyvinyl chloride resin is dissolved at normal temperature and pressure, the concentration of the polyvinyl chloride resin in the solution is 1 wt. It is desirable that the liquid be selected from such a ratio that it is not more than%, preferably not more than 0.1% by weight.
このように熱水やスチームを前記ポリ塩化ビニル樹脂溶液中に注入することにより、ポリ塩化ビニル樹脂溶液中に含まれている溶媒を揮発させて除去させることができる。
また、このとき溶媒の蒸発潜熱により注入した熱水やスチームは冷却されることとなる。したがって、熱水やスチームの注入を継続することにより、槽内には水が貯留された状態となるとともに、ポリ塩化ビニル樹脂溶液から溶媒が除去されてポリ塩化ビニル樹脂組成物が顆粒状に形成されたポリ塩化ビニル樹脂組成物粒子が水中に析出されることとなる。
Thus, by pouring hot water or steam into the polyvinyl chloride resin solution, the solvent contained in the polyvinyl chloride resin solution can be volatilized and removed.
At this time, the hot water or steam injected by the latent heat of vaporization of the solvent is cooled. Therefore, by continuing the injection of hot water or steam, water is stored in the tank, and the solvent is removed from the polyvinyl chloride resin solution to form a polyvinyl chloride resin composition in the form of granules. The resulting polyvinyl chloride resin composition particles are precipitated in water.
このとき熱水やスチームの温度や、注入量、さらには、槽内の温度条件や攪拌条件などを制御することにより、ポリ塩化ビニル樹脂組成物粒子の粒径を制御することができる。
なお、通常、この析出工程では、析出されたポリ塩化ビニル樹脂組成物粒子の内、より多くのポリ塩化ビニル樹脂組成物粒子を粒径５００μｍ以下の顆粒状に形成させることが好ましく、例えば、半数以上の粒子が５００μｍ以下の粒径に形成されるべくその条件を設定することが好ましい。
At this time, the particle size of the polyvinyl chloride resin composition particles can be controlled by controlling the temperature of hot water or steam, the injection amount, the temperature conditions in the tank, the stirring conditions, and the like.
Usually, in this precipitation step, it is preferable to form a larger number of polyvinyl chloride resin composition particles in the form of granules having a particle size of 500 μm or less among the precipitated polyvinyl chloride resin composition particles. The conditions are preferably set so that the above particles are formed to have a particle size of 500 μm or less.
（２）ろ過工程
前記溶解工程と前記析出工程とを実施することにより、ポリ塩化ビニル樹脂と可塑剤とを含むポリ塩化ビニル樹脂組成物により顆粒状に形成されてなるポリ塩化ビニル樹脂組成物粒子が水中に含まれているスラリーを作製するスラリー作製工程を実施した後は、ポリ塩化ビニル樹脂組成物粒子と水とをろ別する。
このろ過工程におけるポリ塩化ビニル樹脂組成物粒子と水とのろ別には、ろ過膜を用いるなどした一般的なろ過装置などを用いることができる。
このろ過工程を実施することにより、後段の乾燥工程におけるポリ塩化ビニル樹脂組成物粒子の乾燥に要する熱エネルギーを低減させ得る。
(2) Filtration step Polyvinyl chloride resin composition particles formed into a granular shape from a polyvinyl chloride resin composition containing a polyvinyl chloride resin and a plasticizer by performing the dissolution step and the precipitation step. After performing the slurry preparation process which produces the slurry contained in water, the polyvinyl chloride resin composition particles and water are separated by filtration.
For the filtration of the polyvinyl chloride resin composition particles and water in this filtration step, a general filtration device using a filtration membrane or the like can be used.
By carrying out this filtration step, the heat energy required for drying the polyvinyl chloride resin composition particles in the subsequent drying step can be reduced.
なおここでは詳述しないが、このろ過された水には、ろ過膜を通過した極微細なポリ塩化ビニル樹脂組成物粒子が含有されており、この水を加熱して析出工程でポリ塩化ビニル樹脂溶液中に注入する貧溶媒として用いることにより、このろ過膜を通過した極微細なポリ塩化ビニル樹脂組成物粒子が核となってポリ塩化ビニル樹脂組成物粒子が形成されやすくなり微細なポリ塩化ビニル樹脂組成物粒子を多数形成させやすくなるという効果を奏するとともにポリ塩化ビニル樹脂組成物の回収率が高められる。 Although not described in detail here, the filtered water contains very fine polyvinyl chloride resin composition particles that have passed through the filtration membrane, and this water is heated to deposit the polyvinyl chloride resin in the precipitation step. By using it as a poor solvent to be injected into the solution, the fine polyvinyl chloride resin composition particles that have passed through the filtration membrane are used as the core, and the polyvinyl chloride resin composition particles are easily formed. The effect of facilitating the formation of a large number of resin composition particles is achieved, and the recovery rate of the polyvinyl chloride resin composition is increased.
（３）乾燥工程
前記溶解工程と前記析出工程（スラリー作製工程）後にろ別されたポリ塩化ビニル樹脂組成物粒子には、水が付着していることから、この付着している水を除去すべく、ポリ塩化ビニル樹脂組成物粒子を５５℃を超える温度となるように加熱して乾燥させる乾燥工程を実施する。
この乾燥工程におけるポリ塩化ビニル樹脂組成物粒子の乾燥には、熱風乾燥炉などの一般的な乾燥装置を用いることができる。
この乾燥工程を実施するのは、後段の篩分け工程に導入させるポリ塩化ビニル樹脂組成物粒子を、乾燥状態とせずに水などが付着した状態とすると、ポリ塩化ビニル樹脂組成物粒子どうしが水を介して凝集してしまい速やかな篩分けを実施することが困難となるためである。
(3) Drying step Since the water adheres to the polyvinyl chloride resin composition particles filtered after the dissolution step and the precipitation step (slurry preparation step), the adhering water is removed. Therefore, the drying process which heats and drys the polyvinyl chloride resin composition particles to a temperature exceeding 55 ° C. is performed.
For drying the polyvinyl chloride resin composition particles in this drying step, a general drying device such as a hot air drying furnace can be used.
This drying step is carried out when the polyvinyl chloride resin composition particles to be introduced into the subsequent sieving step are not dried and water is attached to the polyvinyl chloride resin composition particles. This is because the agglomerates through the slag and it is difficult to carry out quick sieving.
上記に例示のように、析出工程において用いられる（ポリ塩化ビニル樹脂に対する）貧溶媒が水である場合、すなわち、この乾燥工程において除去する液体が水である場合には本実施形態のポリ塩化ビニル樹脂組成物粒子製造方法により製造されたポリ塩化ビニル樹脂組成物粒子を成形品の押し出し成形などに使用する際に、成形品中へのボイドなどの発生を抑制させ得る点から、水分量を測定した際にその値が１％以下となる状態までポリ塩化ビニル樹脂組成物粒子を乾燥させることが好ましく、さらには、２０００ｐｐｍ以下の水分量となるように乾燥工程を実施することが好ましい。 As exemplified above, when the poor solvent (relative to the polyvinyl chloride resin) used in the precipitation step is water, that is, when the liquid to be removed in this drying step is water, the polyvinyl chloride of this embodiment is used. When using polyvinyl chloride resin composition particles produced by the resin composition particle production method for extrusion molding of molded products, the moisture content is measured from the point that the generation of voids in the molded products can be suppressed. It is preferable to dry the polyvinyl chloride resin composition particles until the value becomes 1% or less, and it is preferable to carry out the drying step so that the water content is 2000 ppm or less.
また、この乾燥工程において除去する液体が水である場合には、ポリ塩化ビニル樹脂組成物粒子をすばやく且つ確実に乾燥させ得る点において７０℃以上に加熱された気体と接触させてポリ塩化ビニル樹脂組成物粒子を７０℃以上に加熱する乾燥工程を実施することが好ましい。
なお、乾燥温度が１００℃以上になると、塩化ビニル樹脂組成物の一部の成分が熱分解を起こすおそれがあるため、乾燥温度は７０℃以上１００℃以下とすることが好ましい。
Further, when the liquid to be removed in this drying step is water, the polyvinyl chloride resin composition particles are brought into contact with a gas heated to 70 ° C. or more in that the particles can be quickly and reliably dried. It is preferable to carry out a drying step in which the composition particles are heated to 70 ° C. or higher.
In addition, when a drying temperature will be 100 degreeC or more, since a part component of a vinyl chloride resin composition may raise | generate thermal decomposition, it is preferable that a drying temperature shall be 70 degreeC or more and 100 degrees C or less.
また、アセトンの沸点は、約５６℃であり、メチルエチルケトンの沸点は約８０℃であり、前記溶解工程に用いた溶媒が上記のようなケトン類である場合には、ポリ塩化ビニル樹脂組成物粒子に残留溶媒が生じることを抑制し得る点から、これらの沸点以上の温度でこの乾燥工程を実施することが好ましい。
なお、要すれば、この乾燥工程は、減圧環境下において実施するようにしてもよい。
Further, when the boiling point of acetone is about 56 ° C., the boiling point of methyl ethyl ketone is about 80 ° C., and the solvent used in the dissolving step is the above-mentioned ketones, polyvinyl chloride resin composition particles It is preferable to carry out this drying step at a temperature equal to or higher than these boiling points from the viewpoint of suppressing the generation of residual solvent.
If necessary, this drying step may be performed under a reduced pressure environment.
（４）篩分け工程
前記乾燥工程によって乾燥されたポリ塩化ビニル樹脂組成物粒子を、さらに、このポリ塩化ビニル樹脂組成物粒子に混在する粗大物を除去すべく篩分け工程を実施する。
このポリ塩化ビニル樹脂組成物粒子に混在する粗大物と顆粒状のポリ塩化ビニル樹脂組成物粒子との篩分けにおいては、振動篩など一般的な篩分け装置を用いることができる。
(4) Sieving step The sieving step is carried out to remove the polyvinyl chloride resin composition particles dried in the drying step, and to remove coarse substances mixed in the polyvinyl chloride resin composition particles.
In sieving coarse particles mixed with the polyvinyl chloride resin composition particles and granular polyvinyl chloride resin composition particles, a general sieving apparatus such as a vibration sieve can be used.
なお、このとき乾燥工程後のポリ塩化ビニル樹脂組成物粒子を、ポリ塩化ビニル樹脂組成物粒子の温度が５５℃以下となるまで冷却した後に篩分けを実施する。
このポリ塩化ビニル樹脂組成物粒子を冷却する方法については、特に限定されるものではないが冷風発生装置などの一般的な冷却装置を用いることができ、例えば、常温または冷却された気体の気流に同伴させて乾燥工程後のポリ塩化ビニル樹脂組成物粒子を篩分け装置まで搬送させるなどしてポリ塩化ビニル樹脂組成物粒子の搬送とともにポリ塩化ビニル樹脂組成物粒子の冷却を実施させるようにしてもよい。
この気流による搬送とともにポリ塩化ビニル樹脂組成物粒子の冷却を実施する場合には、ポリ塩化ビニル樹脂組成物粒子が気流中に分散された状態で搬送されることから、前記乾燥工程での乾燥が仮に不十分であったとしても、この気流搬送中にポリ塩化ビニル樹脂組成物粒子を乾燥させることができる。
At this time, the polyvinyl chloride resin composition particles after the drying step are cooled until the temperature of the polyvinyl chloride resin composition particles is 55 ° C. or less, and then sieving is performed.
A method for cooling the polyvinyl chloride resin composition particles is not particularly limited, but a general cooling device such as a cold air generator can be used, for example, at room temperature or in a cooled gas stream. In addition, the polyvinyl chloride resin composition particles after the drying step are transported to a sieving device, and the polyvinyl chloride resin composition particles are cooled together with the transportation of the polyvinyl chloride resin composition particles. Good.
When cooling the polyvinyl chloride resin composition particles together with the air flow, the polyvinyl chloride resin composition particles are conveyed in a state of being dispersed in the air flow. Even if insufficient, the polyvinyl chloride resin composition particles can be dried during the air flow.
この篩分け工程においては、例えば、目開き１ｍｍの篩を用いて、ポリ塩化ビニル樹脂組成物粒子を乾燥状態で篩分けして、篩を通過しない粗大物と篩を通過する顆粒状のポリ塩化ビニル樹脂組成物粒子とに篩分けする方法などを採用することができる。
この篩分け工程では、例えば、粒径が１ｍｍを超える粗大なポリ塩化ビニル樹脂組成物粒子や、ポリ塩化ビニル樹脂組成物とともに廃棄物中に混在していた繊維屑などが粗大物として除去される。
In this sieving step, for example, using a sieve having an opening of 1 mm, the polyvinyl chloride resin composition particles are sieved in a dry state, and a coarse product that does not pass through the sieve and a granular polychlorinated product that passes through the sieve. A method of sieving into vinyl resin composition particles can be employed.
In this sieving step, for example, coarse polyvinyl chloride resin composition particles having a particle diameter exceeding 1 mm, and fiber waste mixed in the waste together with the polyvinyl chloride resin composition are removed as coarse substances. .
この篩分け工程をポリ塩化ビニル樹脂組成物粒子の温度が５５℃以下で実施するのは、ポリ塩化ビニル樹脂組成物粒子には、可塑剤が含有されているため、その温度が５５℃を超える温度である場合には、ポリ塩化ビニル樹脂組成物粒子が軟化してタック性が出現して、顆粒状のポリ塩化ビニル樹脂組成物粒子どうしの凝集が生じて篩の目を通過させるのに時間を要したり、あるいは、顆粒状のポリ塩化ビニル樹脂組成物粒子が粗大物に付着して粗大物とともに除去されたりして顆粒状のポリ塩化ビニル樹脂組成物粒子の収率が低下して、粗大物の混在が抑制された顆粒状のポリ塩化ビニル樹脂組成物粒子を効率よく製造することができないためである。 This sieving step is carried out at a temperature of the polyvinyl chloride resin composition particles of 55 ° C. or lower because the polyvinyl chloride resin composition particles contain a plasticizer, and the temperature exceeds 55 ° C. When the temperature is high, the polyvinyl chloride resin composition particles soften and tackiness appears, and the granular polyvinyl chloride resin composition particles agglomerate and pass through the sieve eyes. Or the granular polyvinyl chloride resin composition particles adhere to the coarse product and are removed together with the coarse product, resulting in a decrease in the yield of the granular polyvinyl chloride resin composition particles, This is because it is impossible to efficiently produce granular polyvinyl chloride resin composition particles in which mixing of coarse substances is suppressed.
また、先に述べたように、顆粒状のポリ塩化ビニル樹脂組成物粒子が乾燥された状態で篩分け工程を実施するのは、水などの液体がポリ塩化ビニル樹脂組成物粒子に付着した状態でこの篩分け工程を実施するとポリ塩化ビニル樹脂組成物粒子どうしか水を介して凝集してしまい速やかな篩分けを実施することが困難となるためである。 In addition, as described above, the sieving step is performed in a state where the granular polyvinyl chloride resin composition particles are dried, in a state where a liquid such as water is attached to the polyvinyl chloride resin composition particles. When this sieving step is carried out, only the polyvinyl chloride resin composition particles are aggregated through water, making it difficult to carry out sieving quickly.
上記のような篩の通過速度をより高め得る点においてこの篩分け工程は、ポリ塩化ビニル樹脂組成物粒子の温度が５０℃以下で実施することが好ましい。
一方で、ポリ塩化ビニル樹脂組成物粒子の温度を必要以上に冷却しても、その冷却に見合う篩の通過速度の向上が期待できず、しかも、冷却にかかる時間やエネルギーを削減し得る点において、篩分け工程は、ポリ塩化ビニル樹脂組成物粒子の温度が４０℃以上で実施することが好ましい。
すなわち、篩分け工程を、前記ポリ塩化ビニル樹脂組成物粒子の温度が４０℃以上、５０℃以下の状態で実施することにより粗大物の混在が抑制され品質が向上された顆粒状のポリ塩化ビニル樹脂組成物粒子をよりいっそう効率よく製造することができる。
The sieving step is preferably performed at a temperature of the polyvinyl chloride resin composition particles of 50 ° C. or less in that the passage speed of the sieve can be further increased.
On the other hand, even if the temperature of the polyvinyl chloride resin composition particles is cooled more than necessary, an improvement in the passing speed of the sieve commensurate with the cooling cannot be expected, and the time and energy required for cooling can be reduced. The sieving step is preferably carried out at a temperature of the polyvinyl chloride resin composition particles of 40 ° C. or higher.
That is, by performing the sieving step in a state where the temperature of the polyvinyl chloride resin composition particles is 40 ° C. or more and 50 ° C. or less, the granular polyvinyl chloride in which the mixture of coarse substances is suppressed and the quality is improved. Resin composition particles can be produced more efficiently.
なお、本実施形態においては、上記のような方法を例にポリ塩化ビニル樹脂組成物粒子製造方法を説明したが、本発明においては、ポリ塩化ビニル樹脂組成物粒子製造方法を上記方法に限定するものではない。 In the present embodiment, the polyvinyl chloride resin composition particle production method has been described by taking the above method as an example. However, in the present invention, the polyvinyl chloride resin composition particle production method is limited to the above method. It is not a thing.
次に実施例を挙げて本発明をさらに詳しく説明するが、本発明はこれらに限定されるものではない。 EXAMPLES Next, although an Example is given and this invention is demonstrated in more detail, this invention is not limited to these.
（実施例１乃至４、比較例１乃至３）
廃棄物として回収された農業用ポリ塩化ビニルフィルムを溶媒に溶解させてポリ塩化ビニル樹脂溶液を作製する溶解工程と、該ポリ塩化ビニル樹脂溶液中にスチームを注入して水中に顆粒状のポリ塩化ビニル樹脂組成物粒子を析出させる析出工程を実施した。
この析出された顆粒状のポリ塩化ビニル樹脂組成物粒子を乾燥させてその性状を測定したところ平均粒径２７０μｍ、かさ密度０．４４ｇ／ｍｌ、可塑剤含有率２４％であった。
なお、これらは以下のようにして測定した。
（平均粒径）
電磁式篩い振とう機および目開き系の異なる９０、１２５、１８０、２５０、３５５、５００、７１０、１０００μｍの９種類のふるいを用いて篩い分けを行って粒度分布を求め、この粒度分布から平均粒径を求めた。
（かさ密度）
ＪＩＳ Ｋ６７２０−２に従って、かさ比重測定器Ａ型装置を用いて測定した。
（可塑剤含有量）
塩ビ再生物をテトラヒドロフランに溶解させた後、不溶解成分を遠心分離器により分離し、溶解成分をガスクロマトグラフィーで分析し、可塑剤含有量を定量分析した。
(Examples 1 to 4, Comparative Examples 1 to 3)
A dissolving process for producing a polyvinyl chloride resin solution by dissolving an agricultural polyvinyl chloride film collected as waste in a solvent, and injecting steam into the polyvinyl chloride resin solution to form granular polyvinyl chloride in water. A precipitation step for precipitating vinyl resin composition particles was performed.
The precipitated granular polyvinyl chloride resin composition particles were dried and measured for properties. The average particle size was 270 μm, the bulk density was 0.44 g / ml, and the plasticizer content was 24%.
These were measured as follows.
(Average particle size)
Nine types of sieves of 90, 125, 180, 250, 355, 500, 710, and 1000 μm with different sieve sieves and mesh systems are used to determine the particle size distribution, and the average is obtained from this particle size distribution. The particle size was determined.
(Bulk density)
According to JIS K6720-2, it measured using the bulk specific gravity measuring device A type apparatus.
(Plasticizer content)
After the recycled PVC product was dissolved in tetrahydrofuran, the insoluble component was separated by a centrifugal separator, the dissolved component was analyzed by gas chromatography, and the plasticizer content was quantitatively analyzed.
（振動篩通過速度の測定）
この乾燥後の顆粒状のポリ塩化ビニル樹脂組成物粒子１２０ｇを用いて、この顆粒状のポリ塩化ビニル樹脂組成物粒子が振動篩を通過する速度を測定した。
測定に際しては、顆粒状のポリ塩化ビニル樹脂組成物粒子の温度を３２℃（実施例１）、４０℃（実施例２）、５０℃（実施例３）、５５℃（実施例４）、６０℃（比較例１）、７０℃（比較例２）、８０℃（比較例３）の７通りで測定した。
なお、振動篩の篩は、２００ｍｍ×５０ｍｍの大きさで、目開き１ｍｍのものを用いた。
振動篩の振とう幅は、０．５ｍｍとし、加速度１Ｇで振とうさせた。
結果を表１に示す。
(Measurement of vibration sieve passing speed)
Using 120 g of the granular polyvinyl chloride resin composition particles after drying, the speed at which the granular polyvinyl chloride resin composition particles passed through the vibrating sieve was measured.
In the measurement, the temperature of the granular polyvinyl chloride resin composition particles was 32 ° C. (Example 1), 40 ° C. (Example 2), 50 ° C. (Example 3), 55 ° C. (Example 4), 60 The measurement was carried out in seven ways: ° C. (Comparative Example 1), 70 ° C. (Comparative Example 2), and 80 ° C. (Comparative Example 3).
Note that the vibrating sieve having a size of 200 mm × 50 mm and an opening of 1 mm was used.
The shaking width of the vibrating screen was 0.5 mm, and the vibrating sieve was shaken at an acceleration of 1G.
The results are shown in Table 1.
表１より、ポリ塩化ビニル樹脂組成物粒子の平均粒子径は篩いに対して充分に小さいにもかかわらず、温度が高い場合、ポリ塩化ビニル樹脂組成物粒子が残留することがわかる。 Table 1 shows that the polyvinyl chloride resin composition particles remain when the temperature is high, even though the average particle diameter of the polyvinyl chloride resin composition particles is sufficiently small with respect to the sieve.
（実施例５乃至８、比較例４乃至６）
実施例１乃至４、比較例１乃至３で用いられたものとは別に廃棄物として回収された農業用ポリ塩化ビニルフィルムを溶媒に溶解させてポリ塩化ビニル樹脂溶液を作製する溶解工程と、該ポリ塩化ビニル樹脂溶液中にスチームを注入して水中に顆粒状のポリ塩化ビニル樹脂組成物粒子を析出させる析出工程を実施した。
この析出された顆粒状のポリ塩化ビニル樹脂組成物粒子を乾燥させてその性状を実施例１乃至４、比較例１乃至３と同様に測定したところ平均粒径３６０μｍ、かさ密度０．５７ｇ／ｍｌ、可塑剤含有率２７％であった。
(Examples 5 to 8, Comparative Examples 4 to 6)
A dissolving step of preparing a polyvinyl chloride resin solution by dissolving an agricultural polyvinyl chloride film recovered as waste separately from those used in Examples 1 to 4 and Comparative Examples 1 to 3 in a solvent; A precipitation step was performed in which steam was injected into the polyvinyl chloride resin solution to precipitate granular polyvinyl chloride resin composition particles in water.
The precipitated granular polyvinyl chloride resin composition particles were dried and the properties thereof were measured in the same manner as in Examples 1 to 4 and Comparative Examples 1 to 3. The average particle size was 360 μm and the bulk density was 0.57 g / ml. The plasticizer content was 27%.
（振動篩通過速度の測定）
この平均粒径３６０μｍ、かさ密度０．５７ｇ／ｍｌのポリ塩化ビニル樹脂組成物粒子を用いて実施例１乃至４、比較例１乃至３と同じ条件で、１２０ｇのポリ塩化ビニル樹脂組成物粒子が振動篩を通過する速度を測定した。
結果を表２に示す。
(Measurement of vibration sieve passing speed)
Using the polyvinyl chloride resin composition particles having an average particle diameter of 360 μm and a bulk density of 0.57 g / ml, 120 g of the polyvinyl chloride resin composition particles were obtained under the same conditions as in Examples 1 to 4 and Comparative Examples 1 to 3. The speed through the vibrating sieve was measured.
The results are shown in Table 2.
（実施例９乃至１２、比較例７乃至９）
実施例１乃至８、比較例１乃至６で用いられたものとはさらに別に廃棄物として回収された農業用ポリ塩化ビニルフィルムを溶媒に溶解させてポリ塩化ビニル樹脂溶液を作製する溶解工程と、該ポリ塩化ビニル樹脂溶液中にスチームを注入して水中に顆粒状のポリ塩化ビニル樹脂組成物粒子を析出させる析出工程を実施した。
この析出された顆粒状のポリ塩化ビニル樹脂組成物粒子を乾燥させてその性状を実施例１乃至４、比較例１乃至３と同様に測定したところ平均粒径２７０μｍ、かさ密度０．６１ｇ／ｍｌ、可塑剤含有率２７％であった。
(Examples 9 to 12, Comparative Examples 7 to 9)
In addition to those used in Examples 1 to 8 and Comparative Examples 1 to 6, a dissolving step for preparing a polyvinyl chloride resin solution by dissolving an agricultural polyvinyl chloride film recovered as waste in a solvent; A precipitation step was performed in which steam was injected into the polyvinyl chloride resin solution to precipitate granular polyvinyl chloride resin composition particles in water.
The precipitated granular polyvinyl chloride resin composition particles were dried and their properties were measured in the same manner as in Examples 1 to 4 and Comparative Examples 1 to 3. The average particle size was 270 μm and the bulk density was 0.61 g / ml. The plasticizer content was 27%.
（振動篩通過速度の測定）
この平均粒径２７０μｍ、かさ密度０．６１ｇ／ｍｌのポリ塩化ビニル樹脂組成物粒子を用いて実施例１乃至８、比較例１乃至６と同じ条件で、１２０ｇのポリ塩化ビニル樹脂組成物粒子が振動篩を通過する速度を測定した。
結果を表３に示す。
(Measurement of vibration sieve passing speed)
Using the polyvinyl chloride resin composition particles having an average particle diameter of 270 μm and a bulk density of 0.61 g / ml, 120 g of the polyvinyl chloride resin composition particles were obtained under the same conditions as in Examples 1 to 8 and Comparative Examples 1 to 6. The speed through the vibrating sieve was measured.
The results are shown in Table 3.
（実施例１３乃至１６、比較例１０乃至１２）
廃棄物として回収され、ポリ塩化ビニル組成物が用いられた電線被覆材を溶媒に溶解させてポリ塩化ビニル樹脂溶液を作製する溶解工程と、該ポリ塩化ビニル樹脂溶液中にスチームを注入して水中に顆粒状のポリ塩化ビニル樹脂組成物粒子を析出させる析出工程を実施した。
この析出された顆粒状のポリ塩化ビニル樹脂組成物粒子を乾燥させてその性状を実施例１乃至４、比較例１乃至３と同様に測定したところ平均粒径３４０μｍ、かさ密度０．６８ｇ／ｍｌ、可塑剤含有率２６％であった。
(Examples 13 to 16, Comparative Examples 10 to 12)
A dissolution process for producing a polyvinyl chloride resin solution by dissolving the wire covering material collected as waste and using the polyvinyl chloride composition in a solvent; and pouring steam into the polyvinyl chloride resin solution A precipitation step was performed to precipitate granular polyvinyl chloride resin composition particles.
The precipitated granular polyvinyl chloride resin composition particles were dried and their properties were measured in the same manner as in Examples 1 to 4 and Comparative Examples 1 to 3. The average particle size was 340 μm and the bulk density was 0.68 g / ml. The plasticizer content was 26%.
（振動篩通過速度の測定）
この平均粒径３４０μｍ、かさ密度０．６８ｇ／ｍｌのポリ塩化ビニル樹脂組成物粒子を用いて実施例１乃至１２、比較例１乃至９と同じ条件で、１２０ｇのポリ塩化ビニル樹脂組成物粒子が振動篩を通過する速度を測定した。
結果を表４に示す。
(Measurement of vibration sieve passing speed)
Using the polyvinyl chloride resin composition particles having an average particle diameter of 340 μm and a bulk density of 0.68 g / ml, 120 g of the polyvinyl chloride resin composition particles were obtained under the same conditions as in Examples 1 to 12 and Comparative Examples 1 to 9. The speed through the vibrating sieve was measured.
The results are shown in Table 4.
以上のことからも、本発明によれば、粗大物の混在が抑制された顆粒状のポリ塩化ビニル樹脂組成物粒子を効率よく製造し得ることがわかる。 From the above, it can be seen that according to the present invention, granular polyvinyl chloride resin composition particles in which mixing of coarse products is suppressed can be efficiently produced.
Claims (4)
前記ポリ塩化ビニル樹脂組成物粒子に混在する粗大物を除去し得るように前記乾燥工程で乾燥されたポリ塩化ビニル樹脂組成物粒子を篩分けする篩分け工程をさらに実施し、しかも、前記ポリ塩化ビニル樹脂組成物粒子の温度が５５℃以下の状態で前記篩分け工程を実施することを特徴とするポリ塩化ビニル樹脂組成物粒子製造方法。 Polyvinyl chloride resin composition particles formed into granules from a polyvinyl chloride resin composition containing a plasticizer using a waste product in which the polyvinyl chloride resin composition containing a polyvinyl chloride resin and a plasticizer is used A dissolving step of preparing a polyvinyl chloride resin solution by dissolving the polyvinyl chloride resin composition contained in the waste in a solvent capable of dissolving the polyvinyl chloride resin, Polyvinyl chloride resin composition particles formed into a granular shape with a polyvinyl chloride resin composition containing a plasticizer by mixing a poor solvent for the resin and the polyvinyl chloride resin solution prepared by the dissolving step. Precipitation step for precipitation in the poor solvent, and the temperature of the polyvinyl chloride resin composition particles precipitated in the poor solvent in the precipitation step exceeds 55 ° C. A polyvinyl chloride resin composition particles manufacturing method for implementing a drying step of drying by Uni heating,
The method further includes a sieving step of sieving the polyvinyl chloride resin composition particles dried in the drying step so as to remove coarse substances mixed in the polyvinyl chloride resin composition particles, and the polyvinyl chloride The method for producing polyvinyl chloride resin composition particles, wherein the sieving step is performed in a state where the temperature of the vinyl resin composition particles is 55 ° C or lower.
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| EP4293067A1 (en) * | 2022-06-13 | 2023-12-20 | Brussels Recycling Metal (BR Met) SA | Micronized powder of recycled soft pvc and articles made therefrom |
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| EP4293067A1 (en) * | 2022-06-13 | 2023-12-20 | Brussels Recycling Metal (BR Met) SA | Micronized powder of recycled soft pvc and articles made therefrom |
| BE1030616B1 (en) * | 2022-06-13 | 2024-01-22 | Brussels Recycling Metal Br Met | Micronized powder in recycled soft PVC and articles made from this powder |
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