JP2023177538A - Recycled oil and production method thereof - Google Patents
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 55
- 239000002699 waste material Substances 0.000 claims abstract description 47
- 239000002244 precipitate Substances 0.000 claims abstract description 41
- 239000010913 used oil Substances 0.000 claims abstract description 31
- 238000004064 recycling Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims description 135
- 239000000203 mixture Substances 0.000 claims description 103
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 96
- 238000003756 stirring Methods 0.000 claims description 83
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 44
- 238000001816 cooling Methods 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 30
- 239000002904 solvent Substances 0.000 claims description 23
- 235000011187 glycerol Nutrition 0.000 claims description 22
- 239000002243 precursor Substances 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 238000001914 filtration Methods 0.000 claims description 15
- 239000003513 alkali Substances 0.000 claims description 14
- 239000003518 caustics Substances 0.000 claims description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 9
- 235000011118 potassium hydroxide Nutrition 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 239000003921 oil Substances 0.000 description 313
- 235000019198 oils Nutrition 0.000 description 310
- 238000006243 chemical reaction Methods 0.000 description 15
- 238000011282 treatment Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 239000008162 cooking oil Substances 0.000 description 12
- 239000007788 liquid Substances 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 8
- 235000013311 vegetables Nutrition 0.000 description 8
- 229910052801 chlorine Inorganic materials 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- 229910052698 phosphorus Inorganic materials 0.000 description 7
- 229910052717 sulfur Inorganic materials 0.000 description 7
- 235000020679 tap water Nutrition 0.000 description 7
- 239000008399 tap water Substances 0.000 description 7
- 239000008157 edible vegetable oil Substances 0.000 description 6
- 235000019482 Palm oil Nutrition 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000000446 fuel Substances 0.000 description 5
- 239000002540 palm oil Substances 0.000 description 5
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 4
- 239000000295 fuel oil Substances 0.000 description 4
- 229910052740 iodine Inorganic materials 0.000 description 4
- 239000011630 iodine Substances 0.000 description 4
- 239000010699 lard oil Substances 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000011574 phosphorus Substances 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- 235000015112 vegetable and seed oil Nutrition 0.000 description 4
- 239000008158 vegetable oil Substances 0.000 description 4
- 125000001309 chloro group Chemical group Cl* 0.000 description 3
- 239000010730 cutting oil Substances 0.000 description 3
- 239000010687 lubricating oil Substances 0.000 description 3
- 125000004433 nitrogen atom Chemical group N* 0.000 description 3
- 125000004437 phosphorous atom Chemical group 0.000 description 3
- 230000001954 sterilising effect Effects 0.000 description 3
- 238000004659 sterilization and disinfection Methods 0.000 description 3
- 125000004434 sulfur atom Chemical group 0.000 description 3
- 235000019737 Animal fat Nutrition 0.000 description 2
- 239000010720 hydraulic oil Substances 0.000 description 2
- 230000007257 malfunction Effects 0.000 description 2
- 239000002480 mineral oil Substances 0.000 description 2
- 235000010446 mineral oil Nutrition 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 1
- 239000003225 biodiesel Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 239000010710 diesel engine oil Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 235000019387 fatty acid methyl ester Nutrition 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 229910001867 inorganic solvent Inorganic materials 0.000 description 1
- 239000003049 inorganic solvent Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- -1 methanol Chemical compound 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005809 transesterification reaction Methods 0.000 description 1
- 239000002349 well water Substances 0.000 description 1
- 235000020681 well water Nutrition 0.000 description 1
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Abstract
Description
本発明は、使用済み油又は廃油を再資源化した再生油及びその製造方法に関する。 The present invention relates to recycled oil obtained by recycling used oil or waste oil, and a method for producing the same.
工場、飲食店、スーパー、コンビニエンスストアー、学校及び一般家庭等において揚げ物等で使用した廃食用油が生じ、これをそのまま下水道等に放出すると環境問題を引き起こす恐れがあり、廃食用油を環境に優しくなるように、再資源化処理したり、再生油を分離回収したりすることが検討されている。 Waste cooking oil used for frying is generated in factories, restaurants, supermarkets, convenience stores, schools, and ordinary households.If this is discharged directly into sewers, etc., it may cause environmental problems. In order to make this possible, consideration is being given to recycling the oil and separating and recovering the recycled oil.
特許文献１には、色相の悪い廃食用油をアルコール等で処理後、活性白土等の吸着剤で精製する方法が開示され、脱色精製処理後の廃食用油を植物インキ用原料やバイオディーゼル用燃料等に利用することが開示されている。 Patent Document 1 discloses a method of treating waste cooking oil with a poor hue with alcohol or the like and then refining it with an adsorbent such as activated clay. It has been disclosed that it can be used for fuel, etc.
また、特許文献２には、廃食用油を濾過して遺物を除去しクリーン廃食用油とし、これにメタノール及び苛性アルカリを加えてエステル化し、そのエステル化油を水洗後層分離し、上層部分を吸着処理する廃食用油の再生方法が開示され、得られた再生油を切削油やディーゼルエンジン油等に用いることが開示されている。 Furthermore, Patent Document 2 discloses that waste cooking oil is filtered to remove artifacts to obtain clean waste cooking oil, which is esterified by adding methanol and caustic alkali, and the esterified oil is washed with water, separated into layers, and the upper layer is separated. A method for regenerating waste cooking oil by adsorption treatment is disclosed, and the use of the obtained regenerated oil as cutting oil, diesel engine oil, etc. is disclosed.
しかしながら、上記のような再生油は、例えば、バイオディーゼル用燃料等において燃費が低い、エンジン停止が発生する等の問題があり、燃料、潤滑油、添加剤等の種々の用途において安定して使用できる高品質の再生油が望まれていた。また、再生油の分離回収効率が悪く、粘度の高い廃食用油は、前処理で粘度を、例えば２０ｍＰａ・ｓ程度かそれ以下まで低くしなければ分離回収ができない等の問題があり、さらにその場合には、分離回収効率が悪くなる等の問題もあり、効率よく高品質の再生油が得られるような方策が待ち望まれていた。 However, the above-mentioned recycled oil has problems such as low fuel consumption and engine stoppage when used as fuel for biodiesel, etc., and cannot be stably used in various applications such as fuel, lubricating oil, and additives. There was a desire for high-quality recycled oil. In addition, the efficiency of separation and recovery of recycled oil is poor, and waste cooking oil with high viscosity cannot be separated and recovered unless the viscosity is lowered to, for example, 20 mPa・s or less through pretreatment. In some cases, there are problems such as poor separation and recovery efficiency, and there has been a long-awaited measure to efficiently obtain high-quality recycled oil.
本発明は、使用済み油又は廃油を再資源化して得られる高品質の再生油と、このような再生油を効率よく製造することが可能な製造方法を提供することを課題とする。 An object of the present invention is to provide high-quality recycled oil obtained by recycling used oil or waste oil, and a production method that can efficiently produce such recycled oil.
上記課題を解決するための請求項１に記載の発明は、使用済み油又は廃油を再資源化した再生油であって、再生油全量基準で水分含有量が５００質量ｐｐｍ以下の範囲であり、１０℃以下の温度において析出する成分の含有量が再生油全量基準で１質量％以下の範囲であることを特徴とする。 The invention according to claim 1 for solving the above problem is a recycled oil obtained by recycling used oil or waste oil, and the water content is in the range of 500 mass ppm or less based on the total amount of recycled oil, It is characterized in that the content of components that precipitate at a temperature of 10° C. or lower is in the range of 1% by mass or less based on the total amount of recycled oil.
また、請求項３に記載の発明は、使用済み油又は廃油を再資源化して再生油を製造する方法であって、再生油Ａと該再生油Ａの動粘度よりも低い動粘度を具備する再生油Ｂを製造し、前記再生油Ａと前記再生油Ｂを混合比（体積比）１：０～０：１の範囲で適宜混合して、所望の動粘度を具備する再生油とし、
前記再生油Ａの製造では、２０℃における粘度が４８ｍＰａ・ｓを超え、かつ引火点が３００℃を超える前記使用済み油又は廃油に、混合するための溶媒として２０℃における粘度が４８ｍＰａ・ｓ以下であり、かつ引火点が３００℃以下である溶媒および水の少なくとも１種を１５体積％～２５体積％の範囲で加えて混合することにより、２０℃における粘度が４０ｍＰａ・ｓ～４８ｍＰａ・ｓであり、かつ引火点が２５０℃～３００℃である油含有組成物を得る混合工程と、前記油含有組成物に含まれる水分を除去する水分除去工程と、水分を除去した前記油含有組成物を冷却する冷却工程と、前記冷却工程によって前記油含有組成物に生じた析出物を除去する析出物除去工程と、を有し、前記混合工程では、下記条件により撹拌を行い、
・撹拌方法 ： ミキサー式撹拌
・撹拌速度 ： １８００r.p.m.以上
・撹拌時間 ： ３０分以上
前記再生油Ｂの製造では、２０℃における粘度が４８ｍＰａ・ｓを超え、かつ引火点が３００℃を超える前記使用済み油又は廃油に、アルコール、苛性アルカリを加えて混合することにより、２０℃における粘度が４０ｍＰａ・ｓ～４８ｍＰａ・ｓであり、かつ引火点が１７０℃～１８０℃である第１油含有組成物を得る第１混合工程と、前記第１油含有組成物に含まれるグリセリンを除去するグリセリン除去工程と、グリセリンを除去した前記第１油含有組成物に５体積％未満の範囲で水を加えて混合することにより油含有前駆組成物を得る第２混合前段工程と、前記油含有前駆組成物に含まれる水分を除去する水分除去前段工程と、水分を除去した前記油含有前駆組成物に１０体積％以上の範囲で水を加えて混合することにより第２油含有組成物を得る第２混合後段工程と、前記第２油含有組成物に含まれる水分を除去する水分除去後段工程と、水分を除去した前記第２油含有組成物を冷却する冷却工程と、前記冷却工程によって前記第２油含有組成物に生じた析出物を除去する析出物除去工程と、を有し、第１混合工程、前記第２混合前段工程および前記第２混合後段工程では下記条件により撹拌を行うことを特徴とする。
・撹拌方法 ： ミキサー式撹拌
・撹拌速度 ： １８００r.p.m.以上
・撹拌時間 ： ３０分以上
Further, the invention according to claim 3 is a method for producing recycled oil by recycling used oil or waste oil, comprising a recycled oil A and a kinematic viscosity lower than the kinematic viscosity of the recycled oil A. Producing recycled oil B, mixing the recycled oil A and the recycled oil B appropriately at a mixing ratio (volume ratio) in the range of 1:0 to 0:1 to obtain a recycled oil having a desired kinematic viscosity;
In the production of the recycled oil A, a solvent with a viscosity of 48 mPa·s or less at 20°C and a flash point of 300°C or less is used as a solvent for mixing By adding and mixing at least one of a solvent and water having a flash point of 300°C or less in a range of 15% to 25% by volume, the viscosity at 20°C is 40mPa・s to 48mPa・s. a mixing step for obtaining an oil-containing composition with a flash point of 250° C. to 300° C.; a water removing step for removing water contained in the oil-containing composition; and a water removing step for removing water from the oil-containing composition. It has a cooling step of cooling, and a precipitate removal step of removing precipitates generated in the oil-containing composition by the cooling step, and in the mixing step, stirring is performed under the following conditions,
・Stirring method: Mixer type stirring ・Stirring speed: 1800 rpm or more ・Stirring time: 30 minutes or more In the production of the recycled oil B, the above-mentioned oil with a viscosity of more than 48 mPa・s at 20°C and a flash point of more than 300°C is used. A first oil-containing composition having a viscosity of 40 mPa·s to 48 mPa·s at 20°C and a flash point of 170°C to 180°C is obtained by adding and mixing alcohol and caustic alkali to used oil or waste oil. a first mixing step for obtaining a product, a glycerin removal step for removing glycerin contained in the first oil-containing composition, and adding water in an amount of less than 5% by volume to the first oil-containing composition from which glycerin has been removed. a second pre-mixing step for obtaining an oil-containing precursor composition by mixing the oil-containing precursor composition; a pre-moisture removal step for removing water contained in the oil-containing precursor composition; a second post-mixing step for obtaining a second oil-containing composition by adding and mixing water in a range of % by volume or more; a post-moisture removal step for removing water contained in the second oil-containing composition; a cooling step of cooling the second oil-containing composition from which has been removed, and a precipitate removal step of removing precipitates generated in the second oil-containing composition by the cooling step, the first mixing step In the second pre-mixing step and the second post-mixing step, stirring is performed under the following conditions.
・Stirring method: Mixer type stirring ・Stirring speed: 1800r.pm or more ・Stirring time: 30 minutes or more
本発明は上記のとおりであって、本発明に係る再生油は高品質であり、種々の用途において安定して使用できるという効果があり、本発明に係る再生油の製造方法によれば、高品質の再生油を効率よく製造可能であるという効果がある。 The present invention is as described above, and the recycled oil according to the present invention has the effect of being of high quality and can be stably used in various applications. This has the effect of being able to efficiently produce high quality recycled oil.
＜再生油＞
本発明に係る再生油は、使用済み油又は廃油を再資源化した再生油であって、再生油全量基準で水分含有量が５００質量ｐｐｍ以下の範囲であり、１０℃以下の温度において析出する成分の含有量が再生油全量基準で１質量％以下の範囲であることを特徴とするものである。
<Recycled oil>
The recycled oil according to the present invention is a recycled oil obtained by recycling used oil or waste oil, has a water content of 500 mass ppm or less based on the total amount of recycled oil, and precipitates at a temperature of 10°C or lower. It is characterized in that the content of the components is in a range of 1% by mass or less based on the total amount of recycled oil.
本発明の再生油において、水分含有量が５００質量ｐｐｍを超えると、本発明の効果が奏され難いことがあり好ましくない。本発明では、水分含有量は
ＪＩＳ Ｋ ２２７５に準拠して測定されるものとする。
In the recycled oil of the present invention, if the water content exceeds 500 mass ppm, it may be difficult to achieve the effects of the present invention, which is not preferable. In the present invention, the water content is measured in accordance with JIS K 2275.
本発明の再生油において、１０℃以下の温度において析出する成分の含有量が再生油全量基準で１質量％を超えると、気温が１０℃を下回るような環境での再生油の使用において、例えば、ラード、パーム油等の低温特性が劣る成分によってポンプの詰まりや、シリンダー内のピストンの摺動不良等の不具合を生じることがあり好ましくない。本発明では、１０℃以下の温度において析出する成分の含有量はフィルターをかけることにより除去した量により測定されるものとする。 In the recycled oil of the present invention, if the content of components that precipitate at a temperature of 10°C or lower exceeds 1% by mass based on the total amount of recycled oil, when the recycled oil is used in an environment where the temperature is below 10°C, for example, , lard, palm oil, and other components with poor low-temperature properties are undesirable because they can cause problems such as clogging of the pump and poor sliding of the piston in the cylinder. In the present invention, the content of components that precipitate at a temperature of 10° C. or lower is measured by the amount removed by filtering.
また、本発明に係る再生油は、再生油全量基準で、例えば、硫黄分含有量（硫黄原子換算値）、窒素分含有量（窒素原子換算値）、塩素分含有量（塩素原子換算値）、リン分含有量（リン原子換算値）、残留炭素含有量、１０％残留炭素含有量、灰分含有量、金属成分含有量を所定の範囲とすることができる。また、再生油のヨウ素価を所定の範囲とすることができる。 In addition, the recycled oil according to the present invention has, for example, sulfur content (sulfur atom equivalent value), nitrogen content (nitrogen atom equivalent value), and chlorine content (chlorine atom equivalent value) based on the total amount of recycled oil. , phosphorus content (phosphorus atom equivalent value), residual carbon content, 10% residual carbon content, ash content, and metal component content can be set within predetermined ranges. Furthermore, the iodine value of the recycled oil can be within a predetermined range.
本発明の再生油における硫黄分含有量はＪＩＳ Ｋ２５４１－６に準拠して測定され、窒素分含有量はＪＩＳ Ｋ２６０９に準拠して測定され、塩素分含有量はＪＰＩ－５Ｓ－６４－２００２に準拠して測定され、リン分含有量はＪＩＳ Ｋ０１１６に準拠して測定され、残留炭素含有量はＪＩＳ Ｋ２２７０に準拠して測定され、１０％残留炭素含有量は、予め試料を蒸留し、残った１０質量％の試料を用いてＪＩＳ Ｋ２２７０に準拠して測定され、灰分含有量はＪＩＳ Ｋ２２７２に準拠して測定され、金属成分含有量はＪＩＳ Ｋ８０８３（ICPより一括分析） に準拠して測定されるものとする。また、本発明の再生油において、ヨウ素価はＪＩＳ Ｋ００７０に準拠して測定されるものとする。 The sulfur content in the recycled oil of the present invention is measured in accordance with JIS K2541-6, the nitrogen content is measured in accordance with JIS K2609, and the chlorine content is measured in accordance with JPI-5S-64-2002. The phosphorus content was measured in accordance with JIS K0116, the residual carbon content was measured in accordance with JIS K2270, and the 10% residual carbon content was determined by distilling the sample in advance and using the remaining 10 The ash content is measured in accordance with JIS K2270 using a mass% sample, the ash content is measured in accordance with JIS K2272, and the metal content is measured in accordance with JIS K8083 (batch analysis from ICP). shall be. Further, in the recycled oil of the present invention, the iodine value shall be measured in accordance with JIS K0070.
本発明の再生油は、２０℃における動粘度が４ｃｍ２／ｓ～５１ｃｍ２／ｓ、好ましくは５ｃｍ２／ｓ～４０ｃｍ２／ｓの範囲であってよい。なお、本発明において、動粘度は、ＪＩＳ Ｋ２２８３：２０００に準拠して測定されるものとする。 The recycled oil of the present invention may have a kinematic viscosity at 20° C. ranging from 4 cm 2 /s to 51 cm 2 /s, preferably from 5 cm 2 /s to 40 cm 2 /s. In addition, in this invention, kinematic viscosity shall be measured based on JISK2283:2000.
本発明の再生油は、ディーゼルエンジン等の燃料、潤滑油、各種添加剤等の用途に応じて動粘度を調整することが好ましい。この場合、動粘度が異なる２種以上の再生油を混合して動粘度を調整してもよい。例えば、２０℃における動粘度が３５ｃｍ２／ｓ～４２ｃｍ２／ｓ程度の再生油と、２０℃における動粘度が３ｃｍ２／ｓ～６ｃｍ２／ｓ程度の再生油を所望の比率（混合比（体積比）１：０～０：１）で混合することにより、所望の動粘度を具備する再生油としてもよい。 It is preferable that the kinematic viscosity of the recycled oil of the present invention is adjusted depending on the use as fuel for diesel engines, lubricating oil, various additives, etc. In this case, the kinematic viscosity may be adjusted by mixing two or more types of recycled oils having different kinematic viscosities. For example, a desired ratio ( mixing ratio ( By mixing at a volume ratio of 1:0 to 0:1), recycled oil having a desired kinematic viscosity may be obtained.
このような本発明に係る再生油は、使用済み油又は廃油を再資源化して得られるものでありながら高品質であり、種々の用途、例えば、エンジン、ボイラー等燃料油、潤滑油、添加剤、工業油等の用途において安定して使用することができる。 Although the recycled oil according to the present invention is obtained by recycling used oil or waste oil, it is of high quality and can be used for various purposes, such as fuel oil for engines and boilers, lubricating oil, and additives. It can be stably used in applications such as , industrial oil, etc.
＜再生油の製造方法＞
本発明に係る再生油の製造方法は、使用済み油又は廃油を再資源化して再生油を製造する方法であって、再生油Ａと該再生油Ａの動粘度よりも低い動粘度を具備する再生油Ｂを製造し、前記再生油Ａと前記再生油Ｂを混合比（体積比）１：０～０：１の範囲で適宜混合して、所望の動粘度を具備する再生油とし、
前記再生油Ａの製造では、２０℃における粘度が４８ｍＰａ・ｓを超え、かつ引火点が３００℃を超える前記使用済み油又は廃油に、混合するための溶媒として２０℃における粘度が４８ｍＰａ・ｓ以下であり、かつ引火点が３００℃以下である溶媒および水の少なくとも１種を加えて混合することにより、２０℃における粘度が４０ｍＰａ・ｓ～４８ｍＰａ・ｓであり、かつ引火点が２５０℃～３００℃である油含有組成物を得る混合工程と、前記油含有組成物に含まれる水分を除去する水分除去工程と、水分を除去した前記油含有組成物を冷却する冷却工程と、前記冷却工程によって前記油含有組成物に生じた析出物を除去する析出物除去工程と、を有し、前記混合工程では、下記条件により撹拌を行い、
・撹拌方法 ： ミキサー式撹拌
・撹拌速度 ： １８００r.p.m.以上
・撹拌時間 ： ３０分以上
前記再生油Ｂの製造では、２０℃における粘度が４８ｍＰａ・ｓを超え、かつ引火点が３００℃を超える前記使用済み油又は廃油に、アルコール、苛性アルカリを加えて混合することにより、２０℃における粘度が４０ｍＰａ・ｓ～４８ｍＰａ・ｓであり、かつ引火点が１７０℃～１８０℃である第１油含有組成物を得る第１混合工程と、前記第１油含有組成物に含まれるグリセリンを除去するグリセリン除去工程と、グリセリンを除去した前記第１油含有組成物に５体積％未満の範囲で水を加えて混合することにより油含有前駆組成物を得る第２混合前段工程と、前記油含有前駆組成物に含まれる水分を除去する水分除去前段工程と、水分を除去した前記油含有前駆組成物に１０体積％以上の範囲で水を加えて混合することにより第２油含有組成物を得る第２混合後段工程と、前記第２油含有組成物に含まれる水分を除去する水分除去後段工程と、水分を除去した前記第２油含有組成物を冷却する冷却工程と、前記冷却工程によって前記第２油含有組成物に生じた析出物を除去する析出物除去工程と、を有し、第１混合工程、前記第２混合前段工程および前記第２混合後段工程では下記条件により撹拌を行うことを特徴とする。
・撹拌方法 ： ミキサー式撹拌
・撹拌速度 ： １８００r.p.m.以上
・撹拌時間 ： ３０分以上
<Production method of recycled oil>
The method for producing recycled oil according to the present invention is a method for producing recycled oil by recycling used oil or waste oil, which comprises recycled oil A and a kinematic viscosity lower than the kinematic viscosity of the recycled oil A. Producing recycled oil B, mixing the recycled oil A and the recycled oil B appropriately at a mixing ratio (volume ratio) in the range of 1:0 to 0:1 to obtain a recycled oil having a desired kinematic viscosity;
In the production of the recycled oil A, a solvent with a viscosity of 48 mPa·s or less at 20°C and a flash point of 300°C or less is used as a solvent for mixing By adding and mixing at least one of a solvent and water having a flash point of 300°C or less, the viscosity at 20°C is 40 mPa·s to 48 mPa·s and the flash point is 250°C to 300°C. a mixing step to obtain an oil-containing composition at a temperature of a precipitate removal step of removing precipitates generated in the oil-containing composition, and in the mixing step, stirring is performed under the following conditions,
・Stirring method: Mixer type stirring ・Stirring speed: 1800 rpm or more ・Stirring time: 30 minutes or more In the production of the recycled oil B, the above-mentioned oil with a viscosity of more than 48 mPa・s at 20°C and a flash point of more than 300°C is used. A first oil-containing composition having a viscosity of 40 mPa·s to 48 mPa·s at 20°C and a flash point of 170°C to 180°C is obtained by adding and mixing alcohol and caustic alkali to used oil or waste oil. a first mixing step for obtaining a product, a glycerin removal step for removing glycerin contained in the first oil-containing composition, and adding water in an amount of less than 5% by volume to the first oil-containing composition from which glycerin has been removed. a second pre-mixing step for obtaining an oil-containing precursor composition by mixing the oil-containing precursor composition; a pre-moisture removal step for removing water contained in the oil-containing precursor composition; a second post-mixing step for obtaining a second oil-containing composition by adding and mixing water in a range of % by volume or more; a post-moisture removal step for removing water contained in the second oil-containing composition; a cooling step of cooling the second oil-containing composition from which has been removed, and a precipitate removal step of removing precipitates generated in the second oil-containing composition by the cooling step, the first mixing step In the second pre-mixing step and the second post-mixing step, stirring is performed under the following conditions.
・Stirring method: Mixer type stirring ・Stirring speed: 1800r.pm or more ・Stirring time: 30 minutes or more
なお、本発明において、粘度は、ＪＩＳ Ｚ ８８０３に規定する粘度計を用いて測定されるものであり、液体内部に生じる流れに抵抗する性質で、せん断応力とせん断速度との比をいう。また、動粘度は、ＪＩＳ Ｋ２２８３：２０００に準拠して測定されるものとする。また、引火点は、ＪＩＳ Ｋ ２２６５－２に規定する迅速平衡密閉法に準拠して測定されるものである。 In the present invention, viscosity is measured using a viscometer specified in JIS Z 8803, and refers to the property of resisting flow generated inside a liquid, and refers to the ratio of shear stress to shear rate. Furthermore, the kinematic viscosity shall be measured in accordance with JIS K2283:2000. Further, the flash point is measured in accordance with the rapid equilibrium sealing method specified in JIS K 2265-2.
本発明の再生油の製造方法において用いる使用済み油は、２０℃における粘度が４８ｍＰａ・ｓを超え、かつ引火点が３００℃を超える使用済み油であれば特に限定されず、公知の使用済み油であってよい。使用済み油としては、例えば、使用済みの燃料油、工業用油、家庭用油、鉱物油、植物油、動物油脂等を挙げることができる。このような使用済み油は、油成分以外にも水分等の他の成分が含まれていてもよい。また、本発明の再生油の製造方法において用いる廃油は、２０℃における粘度が４８ｍＰａ・ｓを超え、かつ引火点が３００℃を超える廃油であれば特に限定されず、公知の廃油であってよい。廃油としては、例えば、廃食用油、廃棄物の燃料油、食用油、鉱物油、植物油、動物油脂等を挙げることができる。このような廃油は、油成分以外にも水分等の他の成分が含まれていてもよい。 The used oil used in the method for producing recycled oil of the present invention is not particularly limited as long as it has a viscosity of more than 48 mPa・s at 20°C and a flash point of more than 300°C, and can be any known used oil. It may be. Examples of the used oil include used fuel oil, industrial oil, household oil, mineral oil, vegetable oil, animal fat, and the like. Such used oil may contain other components such as water in addition to oil components. Furthermore, the waste oil used in the method for producing recycled oil of the present invention is not particularly limited as long as it has a viscosity of more than 48 mPa·s at 20°C and a flash point of more than 300°C, and may be any known waste oil. . Examples of the waste oil include waste cooking oil, waste fuel oil, edible oil, mineral oil, vegetable oil, animal fat, and the like. Such waste oil may contain other components such as water in addition to oil components.
なお、本発明では、使用済み油又は廃油の１種、例えば、植物性廃食用油のみを用いてもよく、また、使用済み油又は廃油の２種以上の組み合わせ、例えば、植物性廃食用油とバージン食用油の組み合わせを用いてもよい。バージン食用油を用いる場合、再生油の製造コストを考慮して、使用済み油又は廃油に対して１０質量％以下とすることが好ましい。 In addition, in the present invention, only one kind of used oil or waste oil, for example, vegetable waste cooking oil, may be used, or a combination of two or more kinds of used oil or waste oil, for example, vegetable waste cooking oil. A combination of and virgin edible oil may also be used. When using virgin edible oil, it is preferable to use 10% by mass or less based on used oil or waste oil in consideration of the production cost of recycled oil.
（再生油Ａの製造）
再生油Ａの製造の混合工程において、使用済み油又は廃油に混合するための溶媒は、２０℃における粘度が４８ｍＰａ・ｓ以下であり、かつ引火点が３００℃以下である溶媒および水の少なくとも１種である。２０℃における粘度が４８ｍＰａ・ｓ以下であり、かつ引火点が３００℃以下である溶媒は、特に限定されず、公知の溶媒であってよい。このような混合するための溶媒としては、例えば、無機溶媒、有機溶媒等が挙げられるが、本発明においては、混合するための溶媒が水、アルコール又は苛性アルカリであることが好ましく、水又は低級アルコールであることがより好ましく、水であることが最も好ましい。なお、混合するための溶媒は、加熱して用いられてもよく、例えば、水を５０℃～７０℃の温度にて用いることが好ましい。なお、水としては特に限定されず、水道水、工業用水、川水、地下水、井戸水、蒸留水、イオン交換水、純水等が挙げられる。
(Manufacture of recycled oil A)
In the mixing process for producing recycled oil A, the solvent to be mixed with used oil or waste oil is at least one of a solvent having a viscosity at 20°C of 48 mPa·s or less and a flash point of 300°C or less, and water. It is a seed. The solvent having a viscosity of 48 mPa·s or less at 20°C and a flash point of 300°C or less is not particularly limited, and may be any known solvent. Examples of the solvent for such mixing include inorganic solvents and organic solvents, but in the present invention, the solvent for mixing is preferably water, alcohol, or caustic alkali, and water or lower Alcohol is more preferred, and water is most preferred. Note that the solvent for mixing may be used while being heated; for example, it is preferable to use water at a temperature of 50°C to 70°C. Note that water is not particularly limited, and includes tap water, industrial water, river water, ground water, well water, distilled water, ion exchange water, pure water, and the like.
再生油Ａの製造の混合工程において、使用済み油又は廃油に対する混合するための溶媒の混合割合は、１５体積％～２５体積％、好ましくは１８体積％～２２体積％の範囲である。 In the mixing step for producing recycled oil A, the mixing ratio of the solvent for mixing with the used oil or waste oil is in the range of 15% to 25% by volume, preferably 18% to 22% by volume.
再生油Ａの製造の混合工程において、使用済み油又は廃油に混合するための溶媒を加えた後の混合は、下記の撹拌条件にて行うことができる。
・撹拌方法 ： ミキサー式撹拌
・撹拌速度 ： １８００r.p.m.以上
・撹拌時間 ： ３０分以上
In the mixing step for producing recycled oil A, mixing after adding a solvent to used oil or waste oil can be performed under the following stirring conditions.
・Stirring method: Mixer type stirring ・Stirring speed: 1800r.pm or more ・Stirring time: 30 minutes or more
撹拌方法が上記と異なる場合、例えば、撹拌速度が１８００r.p.m.未満、あるいは、撹拌時間が３０分未満であるような撹拌方法では、製造後の再生油粒子が微細化されておらず性能を発揮できない恐れがあり好ましくない。 If the stirring method is different from the above, for example, if the stirring speed is less than 1800 r.p.m. or the stirring time is less than 30 minutes, the recycled oil particles after production will not be finely divided and will not perform well. This is not desirable as it may not be possible.
また、撹拌速度が１８００r.p.m.未満、あるいは、撹拌時間が３０分未満であると、製造後の再生油の腐敗を生じるおそれがあり好ましくない。 Furthermore, if the stirring speed is less than 1800 r.p.m. or the stirring time is less than 30 minutes, there is a risk that the recycled oil after production will spoil, which is not preferable.
上記のような撹拌条件による混合は、例えば、佐竹マルチミクス(株)製 ポータブルミキサーのような撹拌装置を使用することが好適である。 For mixing under the above stirring conditions, it is preferable to use a stirring device such as a portable mixer manufactured by Satake Multimix Co., Ltd., for example.
本発明では、混合工程にて、使用済み油又は廃油に溶媒を加えた後に上記のような撹拌条件で混合を行うので、再生油の腐敗を抑制することができ好適である。 In the present invention, in the mixing step, after adding a solvent to used oil or waste oil, mixing is performed under the above-mentioned stirring conditions, which is preferable because spoilage of the recycled oil can be suppressed.
再生油Ａの製造の混合工程において得られる油含有組成物は、２０℃における粘度が４０ｍＰａ・ｓ～４８ｍＰａ・ｓであり、かつ引火点が２５０℃～３００℃であれば特に限定されず、状態は液状、ゾル状、ゲル状のいずれであってもよい。本発明においては、油含有組成物が使用済み油又は廃油を主成分として含有することが好ましい。ここで、主成分とは全体量に対して５０質量％以上含む成分をいう。 The oil-containing composition obtained in the mixing step of producing recycled oil A is not particularly limited as long as it has a viscosity at 20°C of 40 mPa·s to 48 mPa·s and a flash point of 250°C to 300°C. may be in liquid, sol, or gel form. In the present invention, it is preferable that the oil-containing composition contains used oil or waste oil as a main component. Here, the main component refers to a component containing 50% by mass or more based on the total amount.
再生油Ａの製造における水分除去工程での水分除去処理は、油含有組成物に含まれる水分を除去できる処理であれば特に限定されず、完全に水分を除去する必要はなく、一部の水分が除去できるものであればよい。本発明においては、水分除去を、水層と油層との層分離及び／又は乾燥にて行うことが好ましい。例えば、混合工程において溶媒として水を用いた場合、混合工程において得られる油含有組成物には、水層と油層との層分離が生じるので、水層を取り除くことにより水分除去を行うことができる。また、乾燥による水分除去も、水分の全部又は一部が除去できればよく、乾燥手段は、例えば天日干し等でよく、高温にて乾燥させる必要はない。さらに、水分を除去した油含有組成物を加熱、例えば１２０℃に加熱して乾燥、殺菌処理を同時に行ってもよい。 The water removal treatment in the water removal step in the production of recycled oil A is not particularly limited as long as it is a process that can remove water contained in the oil-containing composition, and it is not necessary to completely remove water, but some water may be removed. It is acceptable as long as it can be removed. In the present invention, it is preferable to remove water by separating a water layer and an oil layer and/or by drying. For example, when water is used as a solvent in the mixing step, the oil-containing composition obtained in the mixing step will have a layer separation between a water layer and an oil layer, so water can be removed by removing the water layer. . Further, moisture removal by drying only needs to remove all or part of the moisture, and the drying means may be, for example, sun drying, and there is no need to dry at high temperatures. Furthermore, the oil-containing composition from which water has been removed may be heated, for example to 120° C., to simultaneously perform drying and sterilization treatments.
再生油Ａの製造における冷却工程での冷却手段は、水分を除去した油含有組成物を冷却できればよく特に限定されず、公知の冷却手段であってよい。本発明においては、油含有組成物が冷却されることにより低温特性が劣る成分、例えば、ラード、パーム油等が析出するので、析出物が生じるまで冷却することが好ましい。このような冷却工程では、１０℃以下、好ましくは５℃以下、より好ましくは－５℃以下の温度にて冷却することが好適である。 The cooling means in the cooling step in the production of recycled oil A is not particularly limited as long as it can cool the oil-containing composition from which water has been removed, and may be any known cooling means. In the present invention, components with poor low-temperature properties, such as lard and palm oil, precipitate when the oil-containing composition is cooled, so it is preferable to cool the composition until precipitates form. In such a cooling step, it is suitable to cool at a temperature of 10°C or lower, preferably 5°C or lower, more preferably -5°C or lower.
再生油Ａの製造では、析出物除去工程にて、上記の冷却工程によって油含有組成物に生じた析出物を除去することにより、高品質の再生油を容易、かつ効率的に得ることができる。例えば、ラード、パーム油等の低温特性が劣る成分を除去することができるので、気温が１０℃を下回るような環境での再生油の使用段階において、ポンプの詰まりや、シリンダー内のピストンの摺動不良等の不具合を防止することができる。 In the production of recycled oil A, high-quality recycled oil can be easily and efficiently obtained by removing the precipitates generated in the oil-containing composition in the cooling step in the precipitate removal step. . For example, since it is possible to remove components with poor low-temperature properties such as lard and palm oil, it is possible to prevent clogging of pumps and sliding of pistons in cylinders when using recycled oil in environments where the temperature is below 10℃. Problems such as malfunction can be prevented.
再生油Ａの製造の析出物除去工程における油含有組成物からの析出物除去は、濾過フィルターを用いて油含有組成物を濾過することにより行うことが好ましい。使用する濾過フィルターは、本発明の目的を阻害しない限り特に限定されず、公知の濾過フィルターであってよい。濾過フィルターとしては、例えば、１００メッシュ及び目開き１４９μｍ～２００メッシュ及び目開き７４μｍのフィルターであることが好ましい。 The removal of precipitates from the oil-containing composition in the precipitate removal step of producing recycled oil A is preferably performed by filtering the oil-containing composition using a filtration filter. The filter used is not particularly limited as long as it does not impede the purpose of the present invention, and may be any known filter. As the filtration filter, for example, a filter having a mesh size of 100 mesh, an opening of 149 μm to 200 mesh, and an opening of 74 μm is preferable.
本発明では、再生油Ａの製造の混合工程における使用済み油又は廃油に対する混合するための溶媒の混合割合、混合するための溶媒の温度、撹拌条件を調整すること、上記の水分除去処理の条件を調整すること、上記の冷却工程における冷却温度を調整することにより、得られる再生油Ａにおける成分含有量を調整することができる。例えば、硫黄分含有量（硫黄原子換算値）、窒素分含有量（窒素原子換算値）、塩素分含有量（塩素原子換算値）、リン分含有量（リン原子換算値）、残留炭素含有量、１０％残留炭素含有量、灰分含有量、金属成分含有量、水分含有量、１０℃以下の温度において析出する成分の含有量を所定の範囲とすることができる。また、再生油のヨウ素価を所定の範囲とすることができる。 In the present invention, the mixing ratio of the solvent for mixing with used oil or waste oil in the mixing process of producing recycled oil A, the temperature of the solvent for mixing, and the stirring conditions are adjusted, and the conditions of the water removal treatment described above are adjusted. By adjusting the cooling temperature in the cooling step described above, the component content in the obtained recycled oil A can be adjusted. For example, sulfur content (sulfur atom equivalent value), nitrogen content (nitrogen atom equivalent value), chlorine content (chlorine atom equivalent value), phosphorus content (phosphorus atom equivalent value), residual carbon content , 10% residual carbon content, ash content, metal component content, moisture content, and content of components that precipitate at a temperature of 10° C. or lower can be set within predetermined ranges. Furthermore, the iodine value of the recycled oil can be within a predetermined range.
（再生油Ｂの製造）
再生油Ｂは、再生油Ａの動粘度よりも低い動粘度を具備するものである。この再生油Ｂの製造の第１混合工程において、使用済み油又は廃油に混合するアルコール、苛性アルカリは、予め混合、撹拌して使用することが好ましい。また、アルコールと苛性アルカリの混合割合は、例えば、混合液における苛性アルカリ濃度を８質量％～１０質量％の範囲とすることができる。使用するアルコールとしては低級アルコール、特にメタノールが好ましく、苛性アルカリとしては苛性カリが好ましく使用できる。なお、混合するアルコール、苛性アルカリは、加熱して用いられてもよく、例えば、７０℃以下の温度にて用いることができる。加熱により７０℃を超えると、アルコールのみが揮発してしまい、第１混合工程にて未成熟もしくは未反応の状態が生じ、得られる再生油Ｂの品質が低下することがあり好ましくない。
(Production of recycled oil B)
The recycled oil B has a kinematic viscosity lower than that of the recycled oil A. In the first mixing step of producing the recycled oil B, the alcohol and caustic alkali to be mixed with the used oil or waste oil are preferably mixed and stirred in advance before use. Further, the mixing ratio of alcohol and caustic alkali can be such that the concentration of caustic alkali in the mixed liquid is in the range of 8% by mass to 10% by mass. The alcohol used is preferably a lower alcohol, particularly methanol, and the caustic alkali is preferably caustic potash. Note that the alcohol and caustic alkali to be mixed may be heated and used, for example, at a temperature of 70° C. or lower. If the temperature exceeds 70° C. due to heating, only the alcohol will volatilize, resulting in an immature or unreacted state in the first mixing step, which may deteriorate the quality of the obtained recycled oil B, which is not preferable.
再生油Ｂの製造の第１混合工程において、使用済み油又は廃油に対する混合するアルコールと苛性アルカリの総量の混合割合は、本発明の目的を阻害しなければ特に限定されないが、好ましくは１０体積％～２５体積％、より好ましくは２０体積％～２５体積％の範囲である。 In the first mixing step of producing recycled oil B, the mixing ratio of the total amount of alcohol and caustic alkali to the used oil or waste oil is not particularly limited as long as it does not impede the object of the present invention, but is preferably 10% by volume. The range is from 25% by volume, more preferably from 20% to 25% by volume.
再生油Ｂの製造の第１混合工程において、使用済み油又は廃油にアルコール、苛性アルカリを加えた後の混合では、下記条件により撹拌を行う。
・撹拌方法 ： ミキサー式撹拌
・撹拌速度 ： １８００r.p.m.以上
・撹拌時間 ： ３０分以上
In the first mixing step of producing recycled oil B, after alcohol and caustic alkali are added to used oil or waste oil, stirring is performed under the following conditions.
・Stirring method: Mixer type stirring ・Stirring speed: 1800r.pm or more ・Stirring time: 30 minutes or more
上記のような撹拌条件による混合は、例えば、佐竹マルチミクス(株)製 ポータブルミキサーのような撹拌装置を使用することが好適である。 For mixing under the above stirring conditions, it is preferable to use a stirring device such as a portable mixer manufactured by Satake Multimix Co., Ltd., for example.
再生油Ｂの製造の第１混合工程において得られる第１油含有組成物は、エステル交換反応により生成されたエステル、例えば脂肪酸メチルエステルと、副産物のグリセリンを含有しており、２０℃における粘度が４０ｍＰａ・ｓ～４８ｍＰａ・ｓであり、かつ引火点が１７０℃～１８０℃であれば特に限定されず、状態は液状とする。 The first oil-containing composition obtained in the first mixing step of producing recycled oil B contains esters produced by transesterification, such as fatty acid methyl ester, and glycerin as a by-product, and has a viscosity at 20°C. There is no particular limitation as long as the temperature is 40 mPa·s to 48 mPa·s and the flash point is 170°C to 180°C, and the state is liquid.
再生油Ｂの製造におけるグリセリン除去工程でのグリセリン除去処理は、第１油含有組成物に含まれるグリセリンを除去できる処理であれば特に限定されない。例えば、グリセリン除去を、グリセリン層と油層との層分離にて行うことが好ましい。 The glycerin removal treatment in the glycerin removal step in the production of recycled oil B is not particularly limited as long as it is a treatment that can remove glycerin contained in the first oil-containing composition. For example, it is preferable to remove glycerin by separating a glycerin layer and an oil layer.
再生油Ｂの製造では、第２混合前段工程にて、上記のグリセリン除去工程でグリセリンを除去した第１油含有組成物に５体積％未満の範囲で水を加えて混合することにより油含有前駆組成物を得て、この油含有前駆組成物に含まれる水分を水分除去前段工程にて除去する。その後、第２混合後段工程にて、水分を除去した油含有前駆組成物に１０体積％以上、好ましくは１５体積％～２５体積％の範囲で水を加えて混合することにより第２油含有組成物を得て、この第２油含有組成物に含まれる水分を水分除去後段工程にて除去する。このように、第２混合前段工程における水の添加量を第１油含有組成物の５体積％未満とするのは、第２混合前段工程での水洗いにて、第１油含有組成物（粗製品）が鹸化されて洗剤となることを防止するためである。このような第２混合前段工程と水分除去前段工程が終了すれば、第１油含有組成物（粗製品）に含有される鹸化成分が取り除かれ、第２混合後段工程では水の添加量を多くして混合洗浄することができる。 In the production of recycled oil B, in the second pre-mixing step, water is added to the first oil-containing composition from which glycerin has been removed in the above-mentioned glycerin removal step and mixed in an amount of less than 5% by volume to form an oil-containing precursor. A composition is obtained, and the water contained in this oil-containing precursor composition is removed in a pre-moisture removal step. Thereafter, in a second mixing latter step, water is added to the oil-containing precursor composition from which water has been removed in an amount of 10% by volume or more, preferably in the range of 15% to 25% by volume, and mixed to form a second oil-containing composition. The water contained in this second oil-containing composition is removed in a subsequent water removal step. In this way, the reason why the amount of water added in the second pre-mixing step is less than 5% by volume of the first oil-containing composition is that the first oil-containing composition (crude) is This is to prevent the product from becoming saponified and becoming a detergent. When the second pre-mixing step and the water removal pre-step are completed, the saponification components contained in the first oil-containing composition (crude product) are removed, and the amount of water added is increased in the second post-mixing step. It can be mixed and washed.
本発明では、第２混合後段工程と、その後の水分除去後段工程からなる操作を２回以上、例えば、２回～４回の範囲で設定することができる。 In the present invention, the operation consisting of the second post-mixing step and the subsequent post-moisture removal step can be performed two or more times, for example, in the range of two to four times.
再生油Ｂの製造の第２混合前段工程、第２混合後段工程の混合では、下記条件により撹拌を行う。
・撹拌方法 ： ミキサー式撹拌
・撹拌速度 ： １８００r.p.m.以上
・撹拌時間 ： ３０分以上
In the mixing in the first stage of the second mixing step and the second stage of the second mixing stage in the production of recycled oil B, stirring is performed under the following conditions.
・Stirring method: Mixer type stirring ・Stirring speed: 1800r.pm or more ・Stirring time: 30 minutes or more
再生油Ｂの製造における水分除去前段工程、水分除去後段工程での水分除去処理は、上記の第２混合前段工程で得られた油含有前駆組成物に含まれる水分、第２混合後段工程で得られた第２油含有組成物含まれる水分を除去できる処理であれば特に限定されず、完全に水分を除去する必要はなく、一部の水分が除去できるものであればよい。本発明においては、水分除去を、水層と油層との層分離及び／又は乾燥にて行うことが好ましい。例えば、第２混合前段工程で得られる油含有前駆組成物や、第２混合後段工程で得られる第２油含有組成物には、水層と油層との層分離が生じるので、水層を取り除くことにより水分除去を行うことができる。また、乾燥による水分除去も、水分の全部又は一部が除去できればよく、乾燥手段は、例えば天日干し等でよく、高温にて乾燥させる必要はない。さらに、水分を除去した第２油含有組成物を加熱、例えば１２０℃に加熱して乾燥、殺菌処理を同時に行ってもよい。 In the production of recycled oil B, the water removal treatment in the first stage water removal step and the second stage water removal step removes the water contained in the oil-containing precursor composition obtained in the second first stage mixing step and the water obtained in the second second stage mixing step. The treatment is not particularly limited as long as it can remove the moisture contained in the second oil-containing composition, and it is not necessary to completely remove the moisture, but any treatment that can remove a portion of the moisture is sufficient. In the present invention, it is preferable to remove water by separating the water layer and the oil layer and/or by drying. For example, in the oil-containing precursor composition obtained in the pre-second mixing step and the second oil-containing composition obtained in the post-second mixing step, a water layer and an oil layer separate, so the water layer is removed. Moisture can be removed by this. Further, moisture removal by drying only needs to remove all or part of the moisture, and the drying means may be, for example, sun drying, and there is no need to dry at high temperatures. Furthermore, the second oil-containing composition from which water has been removed may be heated, for example to 120° C., to simultaneously perform drying and sterilization treatment.
再生油Ｂの製造における冷却工程での冷却手段は、水分を除去した第２油含有組成物を冷却できればよく特に限定されず、公知の冷却手段であってよい。本発明においては、第２油含有組成物が冷却されることにより低温特性が劣る成分、例えば、ラード、パーム油等が析出するので、析出物が生じるまで冷却することが好ましい。このような冷却工程では、１０℃以下、好ましくは５℃以下、より好ましくは－５℃以下の温度にて冷却することが好適である。 The cooling means in the cooling step in the production of recycled oil B is not particularly limited as long as it can cool the second oil-containing composition from which water has been removed, and may be any known cooling means. In the present invention, components with poor low-temperature properties, such as lard and palm oil, precipitate when the second oil-containing composition is cooled, so it is preferable to cool the second oil-containing composition until precipitates form. In such a cooling step, it is suitable to cool at a temperature of 10°C or lower, preferably 5°C or lower, more preferably -5°C or lower.
再生油Ｂの製造では、析出物除去工程にて、上記の冷却工程によって第２油含有組成物に生じた析出物を除去することにより、高品質の再生油を容易、かつ効率的に得ることができる。例えば、ラード、パーム油等の低温特性が劣る成分を除去することができるので、気温が１０℃を下回るような環境での再生油の使用段階において、ポンプの詰まりや、シリンダー内のピストンの摺動不良等の不具合を防止することができる。 In the production of recycled oil B, high quality recycled oil can be easily and efficiently obtained by removing the precipitates generated in the second oil-containing composition in the above cooling step in the precipitate removal step. Can be done. For example, since it is possible to remove components with poor low-temperature properties such as lard and palm oil, it is possible to prevent clogging of pumps and sliding of pistons in cylinders when using recycled oil in environments where the temperature is below 10℃. Problems such as malfunction can be prevented.
再生油Ｂの製造の析出物除去工程における第２油含有組成物からの析出物除去は、濾過フィルターを用いて油含有組成物を濾過することにより行うことが好ましい。使用する濾過フィルターは、本発明の目的を阻害しない限り特に限定されず、公知の濾過フィルターであってよい。濾過フィルターとしては、例えば、１００メッシュ及び目開き１４９μｍ～２００メッシュ及び目開き７４μｍのフィルターであることが好ましい。 Precipitates are preferably removed from the second oil-containing composition in the precipitate removal step of producing recycled oil B by filtering the oil-containing composition using a filtration filter. The filter used is not particularly limited as long as it does not impede the purpose of the present invention, and may be any known filter. As the filtration filter, for example, a filter having a mesh size of 100 mesh, an opening of 149 μm to 200 mesh, and an opening of 74 μm is preferable.
本発明では、再生油Ｂの製造の第１混合工程における使用済み油又は廃油に対するアルコール、苛性アルカリの混合割合、混合時の温度、撹拌条件、第２混合前段工程における第１油含有組成物に対する水の混合割合、第２混合後段工程における油含有前駆組成物に対する水の混合割合、混合時の温度、撹拌条件を調整すること、水分除去処理の条件を調整すること、冷却工程における冷却温度を調整することにより、得られる再生油Ｂにおける成分含有量を調整することができる。例えば、硫黄分含有量（硫黄原子換算値）、窒素分含有量（窒素原子換算値）、塩素分含有量（塩素原子換算値）、リン分含有量（リン原子換算値）、残留炭素含有量、１０％残留炭素含有量、灰分含有量、金属成分含有量、水分含有量、１０℃以下の温度において析出する成分の含有量を所定の範囲とすることができる。また、再生油のヨウ素価を所定の範囲とすることができる。 In the present invention, the mixing ratio of alcohol and caustic alkali to used oil or waste oil in the first mixing step of producing recycled oil B, the temperature at the time of mixing, stirring conditions, and the ratio of alcohol to the first oil-containing composition in the second pre-mixing step. Adjusting the mixing ratio of water, the mixing ratio of water to the oil-containing precursor composition in the second post-mixing step, the temperature during mixing, the stirring conditions, adjusting the conditions of water removal treatment, and the cooling temperature in the cooling step. By adjusting, the component content in the obtained recycled oil B can be adjusted. For example, sulfur content (sulfur atom equivalent value), nitrogen content (nitrogen atom equivalent value), chlorine content (chlorine atom equivalent value), phosphorus content (phosphorus atom equivalent value), residual carbon content , 10% residual carbon content, ash content, metal component content, moisture content, and content of components that precipitate at a temperature of 10° C. or lower can be set within predetermined ranges. Furthermore, the iodine value of the recycled oil can be within a predetermined range.
（再生油の調製）
本発明では、上記のように製造した再生油Ａと、上記のように製造した再生油Ｂを混合比（体積比）１：０～０：１の範囲で適宜混合して、所望の動粘度を具備する再生油とする。再生油Ｂは、再生油Ａの動粘度よりも低い動粘度を具備するものである。例えば、再生油Ａの動粘度をｖａ、再生油Ｂの動粘度をｖｂ、ｖａ＞ｖｂとし、所望の動粘度がｖである場合、再生油Ａと再生油Ｂの混合比（体積比ａ：ｂ）は、下記の式から設定することができる。
ｖ＝（ｖａ・ａ＋ｖｂ・ｂ）／（ａ＋ｂ）
(Preparation of recycled oil)
In the present invention, the recycled oil A produced as described above and the recycled oil B produced as described above are appropriately mixed at a mixing ratio (volume ratio) of 1:0 to 0:1 to obtain a desired kinematic viscosity. The recycled oil has the following properties. The recycled oil B has a kinematic viscosity lower than that of the recycled oil A. For example, if the kinematic viscosity of reclaimed oil A is v a and the kinematic viscosity of reclaimed oil B is v b , and the desired kinematic viscosity is v , then the mixing ratio of reclaimed oil A and reclaimed oil B ( The volume ratio a:b) can be set from the following formula.
v=(v a・a+v b・b)/(a+b)
再生油Ａの動粘度ｖａ、再生油Ｂの動粘度ｖｂは、製造ロットにより多少変動するので、製造ロットごとに再生油Ａ、再生油Ｂの動粘度を測定し、再生油の用途に応じた動粘度を具備するように、再生油Ａと再生油Ｂの混合比（体積比）を設定することができる。例えば、２０℃における動粘度ｖａが３５ｃｍ２／ｓ～４２ｃｍ２／ｓの範囲内で特定された再生油Ａと、２０℃における動粘度ｖｂが３ｃｍ２／ｓ～６ｃｍ２／ｓの範囲内で特定された再生油Ｂを、所望の比率（混合比（体積比）１：０～０：１）で混合することにより、所望の動粘度ｖを具備する再生油とすることができる。 Since the kinematic viscosity v a of recycled oil A and the kinematic viscosity v b of recycled oil B vary somewhat depending on the production lot, the kinematic viscosity of recycled oil A and recycled oil B is measured for each production lot, and the kinematic viscosity of recycled oil A and recycled oil B is measured for each production lot. The mixing ratio (volume ratio) of recycled oil A and recycled oil B can be set so as to have a corresponding kinematic viscosity. For example, a recycled oil A whose kinematic viscosity v a at 20°C is in the range of 35 cm 2 /s to 42 cm 2 /s and a kinematic viscosity v b at 20°C in the range of 3 cm 2 /s to 6 cm 2 /s By mixing the recycled oil B specified in the above in a desired ratio (mixing ratio (volume ratio) 1:0 to 0:1), a recycled oil having a desired kinematic viscosity v can be obtained.
本発明の製造方法で得られた再生油は、低温特性に優れた高品質な油であるので、必要に応じてさらに公知の添加剤や処理が施され、燃料油、工業油等の各種油として種々の用途に用いることができる。 Since the recycled oil obtained by the production method of the present invention is a high-quality oil with excellent low-temperature properties, it may be further subjected to known additives and treatments as necessary, and used in various oils such as fuel oil and industrial oil. It can be used for various purposes.
以下に、実施例によって本発明を更に詳細に説明するが、本発明はこれによって何ら限定されるものではない。 EXAMPLES The present invention will be explained in more detail below with reference to Examples, but the present invention is not limited thereto.
［実施例１］
（再生油Ａの製造）
植物性廃食用油（色：ＡＳＴＭカラー８．０のこげ茶、匂い：異臭あり、２０℃における粘度４８．２０ｍＰａ・ｓ、引火点３０６℃）５００Ｌを反応容器に入れ、植物性廃食用油に対する混合割合が２０体積％となるように水道水（１６℃）を反応容器に入れた。その後、撹拌装置を稼働させると同時に反応容器を加熱して液温を７０℃に維持しながら撹拌した。（混合工程）
[Example 1]
(Manufacture of recycled oil A)
Put 500 L of vegetable waste cooking oil (color: ASTM color 8.0 dark brown, odor: off-odor, viscosity at 20°C 48.20 mPa・s, flash point 306°C) into a reaction container, Tap water (16° C.) was put into the reaction container so that the mixing ratio was 20% by volume. Thereafter, the reaction vessel was heated at the same time as the stirring device was operated, and the mixture was stirred while maintaining the liquid temperature at 70°C. (Mixing process)
上記の混合工程では、反応容器における植物性廃食用油と水道水の撹拌は、撹拌装置として、佐竹マルチミクス(株)製 ポータブルミキサーを用いて、下記の条件で行った。
・撹拌方法 ： ミキサー式撹拌
・撹拌速度 ： １８００r.p.m.
・撹拌時間 ： ３０分
In the above mixing step, the vegetable waste edible oil and tap water in the reaction vessel were stirred using a portable mixer manufactured by Satake Multimix Co., Ltd. as a stirring device under the following conditions.
・Stirring method: Mixer type stirring ・Stirring speed: 1800r.pm
・Stirring time: 30 minutes
上記の混合工程により、２０℃における粘度が４０．５ｍＰａ・ｓであり、引火点が２５０℃の油含有組成物（色：ＡＳＴＭカラー６．０の茶色、匂い：植物油臭）を得た。 Through the above mixing step, an oil-containing composition having a viscosity at 20° C. of 40.5 mPa·s and a flash point of 250° C. (color: ASTM color 6.0 brown, odor: vegetable oil odor) was obtained.
上記の混合工程で得られた油含有組成物を静置することにより水層と油層との層分離を生じさせ、水層を取り除いた後、油含有組成物を１２０℃まで加熱して乾燥、殺菌処理を同時に行った。（水分除去工程） By allowing the oil-containing composition obtained in the above mixing step to stand still, a layer separation between a water layer and an oil layer is caused, and after removing the water layer, the oil-containing composition is heated to 120 ° C. and dried. Sterilization treatment was performed at the same time. (Moisture removal process)
次いで、油含有組成物を反応容器ごと冷蔵室に入れ、油含有組成物が－５℃の温度となるまで冷却した。これにより、油含有組成物において低温特性が劣る成分の析出が見られた。（冷却工程） Next, the oil-containing composition was placed in a refrigerator along with the reaction container, and cooled until the oil-containing composition reached a temperature of -5°C. As a result, precipitation of components with poor low-temperature properties was observed in the oil-containing composition. (cooling process)
次に、上記の冷蔵室内にて、濾過フィルター（１００メッシュ、目開き１４９μｍ）を用いて油含有組成物を濾過することにより、再生油Ａを得た。（析出物除去工程） Next, recycled oil A was obtained by filtering the oil-containing composition using a filtration filter (100 mesh, opening 149 μm) in the above-mentioned refrigerator room. (Precipitate removal process)
この再生油Ａの２０℃における動粘度を測定した結果、３７ｃｍ２／ｓであった。なお、動粘度は、ＪＩＳ Ｋ２２８３：２０００に準拠して測定した。 The kinematic viscosity of this recycled oil A at 20° C. was measured and found to be 37 cm 2 /s. Note that the kinematic viscosity was measured in accordance with JIS K2283:2000.
（再生油Ｂの製造）
上記と同じ植物性廃食用油５００Ｌを反応容器に入れ、反応容器を加熱して液温を７０℃に維持しながら撹拌した。その後、容積比で９０．６：９．４（苛性カリの濃度を９．４％と設定する）で混合したメタノールと苛性カリの混合液を、植物性廃食用油に対する混合割合が２０体積％となるように反応容器に投入し、液温を７０℃に維持しながら撹拌した。（第１混合工程）
(Production of recycled oil B)
500 L of the same vegetable waste cooking oil as above was placed in a reaction vessel, and the reaction vessel was heated and stirred while maintaining the liquid temperature at 70°C. After that, a mixed solution of methanol and caustic potash mixed at a volume ratio of 90.6:9.4 (the concentration of caustic potash is set at 9.4%) is mixed at a mixing ratio of 20% by volume with respect to the vegetable waste cooking oil. The mixture was poured into a reaction vessel and stirred while maintaining the liquid temperature at 70°C. (First mixing step)
上記の第１混合工程では、撹拌装置として、佐竹マルチミクス(株)製 ポータブルミキサーを用いて、下記の条件で行った。
・撹拌方法 ： ミキサー式撹拌
・撹拌速度 ： １８００r.p.m.
・撹拌時間 ： ３０分
The first mixing step was carried out under the following conditions using a portable mixer manufactured by Satake Multimix Co., Ltd. as a stirring device.
・Stirring method: Mixer type stirring ・Stirring speed: 1800r.pm
・Stirring time: 30 minutes
上記の第１混合工程により、２０℃における粘度が４４ｍＰａ・ｓであり、引火点が１７６℃の第１油含有組成物（色：ＡＳＴＭカラー１．０の黄色、匂い：植物油臭）を得た。 Through the above first mixing step, a first oil-containing composition (color: ASTM color 1.0 yellow, odor: vegetable oil odor) having a viscosity of 44 mPa·s at 20°C and a flash point of 176°C was obtained. .
上記の第１混合工程で得られた第１油含有組成物を静置することによりグリセリン層と油層との層分離を生じさせ、グリセリン層を取り除いた。（グリセリン除去工程） The first oil-containing composition obtained in the first mixing step was allowed to stand to cause separation between the glycerin layer and the oil layer, and the glycerin layer was removed. (Glycerin removal process)
グリセリンを除去した第１油含有組成物４８０Ｌを反応容器に入れ、第１油含有組成物に対する混合割合が４体積％となるように水道水（１６℃）を反応容器に入れた。その後、撹拌装置を稼働させると同時に反応容器を加熱して液温を７０℃に維持しながら撹拌した。（第２混合前段工程） 480 L of the first oil-containing composition from which glycerin had been removed was placed in a reaction vessel, and tap water (16°C) was placed in the reaction vessel so that the mixing ratio to the first oil-containing composition was 4% by volume. Thereafter, the reaction vessel was heated at the same time as the stirring device was operated, and the mixture was stirred while maintaining the liquid temperature at 70°C. (Second mixing preliminary step)
この第２混合前段工程では、撹拌装置として、佐竹マルチミクス(株)製 ポータブルミキサーを用いて、下記の条件で行った。
・撹拌方法 ： ミキサー式撹拌
・撹拌速度 ： １８００r.p.m.
・撹拌時間 ： ３０分
This second pre-mixing step was carried out under the following conditions using a portable mixer manufactured by Satake Multimix Co., Ltd. as a stirring device.
・Stirring method: Mixer type stirring ・Stirring speed: 1800r.pm
・Stirring time: 30 minutes
第２混合前段工程で得られた油含有前駆組成物を静置することにより水層と油層との層分離を生じさせ、水層を取り除いた。（水分除去前段工程） The oil-containing precursor composition obtained in the second pre-mixing step was allowed to stand to cause separation between the water layer and the oil layer, and the water layer was removed. (Pre-moisture removal step)
次に、水分を除去した油含有前駆組成物４８０Ｌを反応容器に入れ、油含有前駆組成物に対する混合割合が２０体積％となるように水道水（１６℃）を反応容器に入れた。その後、第２混合前段工程と同様の条件で撹拌装置を稼働させると同時に反応容器を加熱して液温を７０℃に維持しながら撹拌した。（第２混合後段工程） Next, 480 L of the oil-containing precursor composition from which water had been removed was placed in a reaction container, and tap water (16° C.) was added to the reaction container so that the mixing ratio to the oil-containing precursor composition was 20% by volume. Thereafter, the stirring device was operated under the same conditions as in the second pre-mixing step, and at the same time, the reaction vessel was heated to maintain the liquid temperature at 70° C. while stirring. (Second mixing latter step)
第２混合後段工程で得られた第２油含有組成物を静置することにより水層と油層との層分離を生じさせ、水層を取り除いた後、第２油含有組成物を１２０℃まで加熱して乾燥、殺菌処理を同時に行った。（水分除去後段工程） The second oil-containing composition obtained in the latter stage of the second mixing step is allowed to stand to cause layer separation between the water layer and the oil layer, and after removing the water layer, the second oil-containing composition is heated to 120°C. It was heated, dried, and sterilized at the same time. (Water removal stage process)
次いで、第２油含有組成物を反応容器ごと冷蔵室に入れ、油含有組成物が－５℃の温度となるまで冷却した。これにより、第２油含有組成物において低温特性が劣る成分の析出が見られた。（冷却工程） Next, the second oil-containing composition was placed in a refrigerator along with the reaction container, and cooled until the oil-containing composition reached a temperature of -5°C. As a result, precipitation of components with poor low-temperature properties was observed in the second oil-containing composition. (cooling process)
次に、上記の冷蔵室内にて、濾過フィルター（１００メッシュ、目開き１４９μｍ）を用いて第２油含有組成物を濾過することにより、再生油Ｂを得た。（析出物除去工程） Next, the second oil-containing composition was filtered using a filtration filter (100 mesh, opening 149 μm) in the above-mentioned refrigerator room to obtain recycled oil B. (Precipitate removal process)
この再生油Ｂの２０℃における動粘度を測定した結果、５ｃｍ２／ｓであった。なお、動粘度は、ＪＩＳ Ｋ２２８３：２０００に準拠して測定した。 The kinematic viscosity of this recycled oil B at 20° C. was measured and found to be 5 cm 2 /s. Note that the kinematic viscosity was measured in accordance with JIS K2283:2000.
（再生油の調製）
上記の再生油Ａと再生油Ｂを混合比（体積比）５．５：１で混合して再生油（試料Ｉ）を得た。この再生油（試料Ｉ）の動粘度を測定した結果、３２ｃｍ２／ｓであった。また、再生油（試料Ｉ）の水分含有量は再生油全量基準で３２０質量ｐｐｍであり、１０℃以下の温度において析出する成分の含有量は再生油全量基準で１質量％であった。
(Preparation of recycled oil)
The above recycled oil A and recycled oil B were mixed at a mixing ratio (volume ratio) of 5.5:1 to obtain a recycled oil (sample I). The kinematic viscosity of this recycled oil (Sample I) was measured and found to be 32 cm 2 /s. In addition, the water content of the recycled oil (sample I) was 320 mass ppm based on the total amount of recycled oil, and the content of components that precipitated at a temperature of 10° C. or lower was 1% by mass based on the total amount of recycled oil.
また、上記の再生油Ａと再生油Ｂを混合比（体積比）３．５：３で混合して再生油（試料II）を得た。この再生油（試料II）の動粘度を測定した結果、２２ｃｍ２／ｓであり、再生油（試料II）の水分含有量は再生油全量基準で３２０質量ｐｐｍであり、１０℃以下の温度において析出する成分の含有量は再生油全量基準で１質量％であった。 In addition, recycled oil (sample II) was obtained by mixing the recycled oil A and recycled oil B at a mixing ratio (volume ratio) of 3.5:3. As a result of measuring the kinematic viscosity of this recycled oil (sample II), it was 22 cm 2 /s, and the water content of the recycled oil (sample II) was 320 mass ppm based on the total amount of recycled oil, and at a temperature of 10°C or less. The content of the precipitated components was 1% by mass based on the total amount of recycled oil.
また、上記の再生油Ａと再生油Ｂを混合比（体積比）２．１：４．４で混合して再生油（試料III）を得た。この再生油（試料III）の動粘度を測定した結果、１５ｃｍ２／ｓであり、再生油（試料III）の水分含有量は再生油全量基準で３２０質量ｐｐｍであり、１０℃以下の温度において析出する成分の含有量は再生油全量基準で１質量％であった。 In addition, recycled oil (sample III) was obtained by mixing the recycled oil A and recycled oil B at a mixing ratio (volume ratio) of 2.1:4.4. As a result of measuring the kinematic viscosity of this recycled oil (sample III), it was 15 cm 2 /s, and the water content of the recycled oil (sample III) was 320 mass ppm based on the total amount of recycled oil, and at a temperature of 10°C or less. The content of the precipitated components was 1% by mass based on the total amount of recycled oil.
さらに、上記の再生油Ａと再生油Ｂを混合比（体積比）０．４６：６．０４で混合して再生油（試料IV）を得た。この再生油（試料IV）の動粘度を測定した結果、７ｃｍ２／ｓであり、再生油（試料IV）の水分含有量は再生油全量基準で３２０質量ｐｐｍであり、１０℃以下の温度において析出する成分の含有量は再生油全量基準で1質量％であった。 Furthermore, the above recycled oil A and recycled oil B were mixed at a mixing ratio (volume ratio) of 0.46:6.04 to obtain a recycled oil (sample IV). As a result of measuring the kinematic viscosity of this recycled oil (sample IV), it was 7 cm 2 /s, and the water content of the recycled oil (sample IV) was 320 mass ppm based on the total amount of recycled oil, and at a temperature of 10°C or less. The content of the precipitated components was 1% by mass based on the total amount of recycled oil.
尚、再生油の水分含有量はＪＩＳ Ｋ ２２７５に準拠して測定し、１０℃以下の温度において析出する成分の含有量はフィルターをかけることにより除去した量により測定した。 The water content of the recycled oil was measured in accordance with JIS K 2275, and the content of components that precipitate at temperatures below 10°C was measured by the amount removed by filtering.
上記の４種の再生油（試料Ｉ～IV）の中で、動粘度が２２ｃｍ２／ｓである再生油（試料II）を作動油及び切削油として０℃の環境下で使用したが、支障は生じなかった。 Among the four types of recycled oils (Samples I to IV) mentioned above, the recycled oil (Sample II) with a kinematic viscosity of 22 cm 2 /s was used as a hydraulic oil and cutting oil in an environment of 0°C, but there were no problems. did not occur.
[比較例１]
再生油Ａの製造の混合工程における植物性廃食用油に対する水道水の混合割合を５体積％とし、また、植物性廃食用油と水道水の撹拌を、撹拌装置として、佐竹マルチミクス(株)製 ポータブルミキサーを用いて、下記の条件で行った他は、実施例１の再生油Ａの製造と同様にして、再生Ａ′油を得た。この再生Ａ′油の２０℃における動粘度を測定した結果、３７ｃｍ２／ｓであった。
・撹拌方法 ： ミキサー式撹拌
・撹拌速度 ： １８００r.p.m.
・撹拌時間 ： ３０分
[Comparative example 1]
In the mixing process of producing recycled oil A, the mixing ratio of tap water to vegetable waste edible oil was 5% by volume, and the stirring device used to stir the vegetable waste edible oil and tap water was manufactured by Satake Multimix Co., Ltd. Regenerated oil A' was obtained in the same manner as in Example 1, except that a portable mixer was used and the following conditions were used. The kinematic viscosity of this recycled A' oil at 20° C. was measured and found to be 37 cm 2 /s.
・Stirring method: Mixer type stirring ・Stirring speed: 1800r.pm
・Stirring time: 30 minutes
上記の再生Ａ′油と再生油Ｂを混合比（体積比）３．５：３で混合して再生油（比較試料Ｉ）を得た。この再生油（比較試料Ｉ）の動粘度を測定した結果、２２ｃｍ２／ｓであった。また、再生油（比較試料Ｉ）の水分含有量は再生油全量基準で３２０質量ｐｐｍであり、１０℃以下の温度において析出する成分の含有量は再生油全量基準で１質量％であった。しかし、再生油（試料II）と再生油（比較試料Ｉ）を４０℃の環境下で９０日間静置すると、再生油（比較試料Ｉ）では腐敗が生じた。 The above recycled oil A' and recycled oil B were mixed at a mixing ratio (volume ratio) of 3.5:3 to obtain a recycled oil (comparative sample I). The kinematic viscosity of this recycled oil (comparative sample I) was measured and found to be 22 cm 2 /s. In addition, the water content of the recycled oil (comparative sample I) was 320 mass ppm based on the total amount of recycled oil, and the content of components that precipitated at a temperature of 10° C. or lower was 1% by mass based on the total amount of recycled oil. However, when the recycled oil (Sample II) and the recycled oil (Comparative Sample I) were allowed to stand for 90 days in a 40°C environment, the recycled oil (Comparative Sample I) suffered from spoilage.
[比較例２]
再生油Ｂの製造の第１混合工程と、グリセリン除去工程を実施しない他は、実施例１の再生油Ｂの製造と同様にして、再生Ｂ′油を得た。
[Comparative example 2]
Regenerated oil B' was obtained in the same manner as in the production of recycled oil B in Example 1, except that the first mixing step and the glycerin removal step in the production of recycled oil B were not performed.
この再生Ｂ′油の２０℃における動粘度を測定した結果、３７ｃｍ２／ｓと高いものであり、実施例１の再生油Ａとの混合により動粘度を調整した再生油の調製は難しいものであった。 As a result of measuring the kinematic viscosity of this recycled oil B' at 20°C, it was as high as 37 cm 2 /s, and it was difficult to prepare a recycled oil whose kinematic viscosity was adjusted by mixing it with the recycled oil A of Example 1. there were.
[比較例３]
再生油Ａの製造の冷却工程を実施しなかった他は、実施例１と同様にして、再生Ａ″油を得た。この再生Ａ″油の２０℃における動粘度を測定した結果、４０ｃｍ２／ｓであった。
[Comparative example 3]
Recycled oil A'' was obtained in the same manner as in Example 1, except that the cooling step for producing recycled oil A was not performed.The kinematic viscosity of this recycled oil A'' at 20°C was measured, and the result was 40 cm 2 /s.
上記の再生Ａ″油と再生油Ｂ（動粘度は５ｃｍ２／ｓ）を混合比（体積比）３．２：３．３で混合して再生油（比較試料II）を得た。この再生油（比較試料II）の動粘度を測定した結果、２２ｃｍ２／ｓであった。また、再生油（比較試料II）の水分含有量は再生油全量基準で３２０質量ｐｐｍであったが、１０℃以下の温度において析出する成分の含有量は再生油全量基準で１質量％を超えるものであった。 The above recycled oil A'' and recycled oil B (kinematic viscosity: 5 cm 2 /s) were mixed at a mixing ratio (volume ratio) of 3.2:3.3 to obtain recycled oil (comparative sample II). The kinematic viscosity of the oil (comparative sample II) was measured and found to be 22 cm 2 /s.Also, the water content of the recycled oil (comparative sample II) was 320 mass ppm based on the total amount of recycled oil, but it was 10 cm 2 /s. The content of components that precipitate at temperatures below 0.degree. C. exceeded 1% by mass based on the total amount of recycled oil.
この再生油（比較試料II）を作動油及び切削油として０℃の環境下で使用したところ、析出物が発生しポンプの詰まりや、シリンダー内のピストンの摺動不良等の不具合が生じた。 When this recycled oil (Comparative Sample II) was used as a hydraulic oil and cutting oil in an environment of 0°C, precipitates were generated and problems such as clogging of the pump and poor sliding of the piston in the cylinder occurred.
本発明は上記のとおりであって、本発明の再生油によれば、高品質であり、種々の用途において安定して使用できるという効果があり、本発明の再生油の製造方法によれば、高品質の再生油を効率よく製造可能であるという効果があるので、その産業上の利用可能性は大である。 The present invention is as described above, and the recycled oil of the present invention is of high quality and can be stably used in various applications, and the method for producing recycled oil of the present invention has the following effects: Since it has the effect of being able to efficiently produce high-quality recycled oil, its industrial applicability is great.
Claims (15)
再生油全量基準で水分含有量が５００質量ｐｐｍ以下の範囲であり、
１０℃以下の温度において析出する成分の含有量が再生油全量基準で１質量％以下の範囲であることを特徴とする再生油。 In recycled oil that is recycled from used oil or waste oil,
The water content is in the range of 500 mass ppm or less based on the total amount of recycled oil,
A recycled oil characterized in that the content of components that precipitate at a temperature of 10° C. or lower is 1% by mass or less based on the total amount of recycled oil.
再生油Ａと該再生油Ａの動粘度よりも低い動粘度を具備する再生油Ｂを製造し、前記再生油Ａと前記再生油Ｂを混合比（体積比）１：０～０：１の範囲で混合して、所望の動粘度を具備する再生油とし、
前記再生油Ａの製造では、２０℃における粘度が４８ｍＰａ・ｓを超え、かつ引火点が３００℃を超える前記使用済み油又は廃油に、混合するための溶媒として２０℃における粘度が４８ｍＰａ・ｓ以下であり、かつ引火点が３００℃以下である溶媒および水の少なくとも１種を１５体積％～２５体積％の範囲で加えて混合することにより、２０℃における粘度が４０ｍＰａ・ｓ～４８ｍＰａ・ｓであり、かつ引火点が２５０℃～３００℃である油含有組成物を得る混合工程と、前記油含有組成物に含まれる水分を除去する水分除去工程と、水分を除去した前記油含有組成物を冷却する冷却工程と、前記冷却工程によって前記油含有組成物に生じた析出物を除去する析出物除去工程と、を有し、前記混合工程では、下記条件により撹拌を行い、
・撹拌方法 ： ミキサー式撹拌
・撹拌速度 ： １８００r.p.m.以上
・撹拌時間 ： ３０分以上
前記再生油Ｂの製造では、２０℃における粘度が４８ｍＰａ・ｓを超え、かつ引火点が３００℃を超える前記使用済み油又は廃油に、アルコール、苛性アルカリを加えて混合することにより、２０℃における粘度が４０ｍＰａ・ｓ～４８ｍＰａ・ｓであり、かつ引火点が１７０℃～１８０℃である第１油含有組成物を得る第１混合工程と、前記第１油含有組成物に含まれるグリセリンを除去するグリセリン除去工程と、グリセリンを除去した前記第１油含有組成物に５体積％未満の範囲で水を加えて混合することにより油含有前駆組成物を得る第２混合前段工程と、前記油含有前駆組成物に含まれる水分を除去する水分除去前段工程と、水分を除去した前記油含有前駆組成物に１０体積％以上の範囲で水を加えて混合することにより第２油含有組成物を得る第２混合後段工程と、前記第２油含有組成物に含まれる水分を除去する水分除去後段工程と、水分を除去した前記第２油含有組成物を冷却する冷却工程と、前記冷却工程によって前記第２油含有組成物に生じた析出物を除去する析出物除去工程と、を有し、第１混合工程、前記第２混合前段工程および前記第２混合後段工程では下記条件により撹拌を行うことを特徴とする再生油の製造方法。
・撹拌方法 ： ミキサー式撹拌
・撹拌速度 ： １８００r.p.m.以上
・撹拌時間 ： ３０分以上 In a method for producing recycled oil by recycling used oil or waste oil,
A recycled oil A and a recycled oil B having a kinematic viscosity lower than that of the recycled oil A are produced, and the recycled oil A and the recycled oil B are mixed at a mixing ratio (volume ratio) of 1:0 to 0:1. mixed within a range to obtain recycled oil having a desired kinematic viscosity;
In the production of the recycled oil A, a solvent with a viscosity of 48 mPa·s or less at 20°C and a flash point of 300°C or less is used as a solvent for mixing By adding and mixing at least one of a solvent and water having a flash point of 300°C or less in a range of 15% to 25% by volume, the viscosity at 20°C is 40mPa・s to 48mPa・s. a mixing step for obtaining an oil-containing composition with a flash point of 250° C. to 300° C.; a water removing step for removing water contained in the oil-containing composition; and a water removing step for removing water from the oil-containing composition. It has a cooling step of cooling, and a precipitate removal step of removing precipitates generated in the oil-containing composition by the cooling step, and in the mixing step, stirring is performed under the following conditions,
・Stirring method: Mixer type stirring ・Stirring speed: 1800 rpm or more ・Stirring time: 30 minutes or more In the production of the recycled oil B, the above-mentioned oil with a viscosity of more than 48 mPa・s at 20°C and a flash point of more than 300°C is used. A first oil-containing composition having a viscosity of 40 mPa·s to 48 mPa·s at 20°C and a flash point of 170°C to 180°C is obtained by adding and mixing alcohol and caustic alkali to used oil or waste oil. a first mixing step for obtaining a product, a glycerin removal step for removing glycerin contained in the first oil-containing composition, and adding water in an amount of less than 5% by volume to the first oil-containing composition from which glycerin has been removed. a second pre-mixing step for obtaining an oil-containing precursor composition by mixing the oil-containing precursor composition; a pre-moisture removal step for removing water contained in the oil-containing precursor composition; a second post-mixing step for obtaining a second oil-containing composition by adding and mixing water in a range of % by volume or more; a post-moisture removal step for removing water contained in the second oil-containing composition; a cooling step of cooling the second oil-containing composition from which has been removed, and a precipitate removal step of removing precipitates generated in the second oil-containing composition by the cooling step, the first mixing step A method for producing recycled oil, characterized in that in the second pre-mixing step and the second post-mixing step, stirring is performed under the following conditions.
・Stirring method: Mixer type stirring ・Stirring speed: 1800r.pm or more ・Stirring time: 30 minutes or more
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| JP2022090265A JP2023177538A (en) | 2022-06-02 | 2022-06-02 | Recycled oil and production method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| JP2022090265A JP2023177538A (en) | 2022-06-02 | 2022-06-02 | Recycled oil and production method thereof |
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| JP2023177538A true JP2023177538A (en) | 2023-12-14 |
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| JP2022090265A Pending JP2023177538A (en) | 2022-06-02 | 2022-06-02 | Recycled oil and production method thereof |
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