JP4257186B2 - Recycle additive composition for asphalt pavement waste - Google Patents

Recycle additive composition for asphalt pavement waste Download PDF

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JP4257186B2
JP4257186B2 JP2003390794A JP2003390794A JP4257186B2 JP 4257186 B2 JP4257186 B2 JP 4257186B2 JP 2003390794 A JP2003390794 A JP 2003390794A JP 2003390794 A JP2003390794 A JP 2003390794A JP 4257186 B2 JP4257186 B2 JP 4257186B2
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asphalt
mass
additive composition
oil
fat
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JP2005154464A (en
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大作 立石
好和 中村
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Eneos Corp
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Nippon Oil Corp
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Description

本発明は舗装用アスファルトの再生添加剤に関する。詳しくは環境および人体に対する安全性に優れ、かつ舗装廃材中に含まれる劣化を受け硬化したアスファルトを初期の軟らかさまで回復させる、すなわち低下した針入度、伸度を回復させる能力に優れたアスファルト再生添加剤組成物に関する。   The present invention relates to a paving asphalt regeneration additive. Specifically, asphalt regeneration is excellent in safety to the environment and the human body, and has the ability to recover the hardened asphalt contained in pavement waste materials to the initial softness, that is, the ability to restore reduced penetration and elongation. It relates to an additive composition.

舗装廃材の再生には、舗装廃材、新規骨材、新規アスファルトの3者をアスファルト合材工場のミキサーにて混合し、舗装廃材中に含まれる劣化を受け硬化したアスファルトの針入度、伸度を初期の軟らかさまで回復させるため、アスファルト再生添加剤を添加して劣化アスファルトを再生する方法が行われている。このアスファルト再生添加剤は、劣化により失われたアスファルト中の芳香族成分を補う目的から、芳香族性の高い鉱油、例えば石油精製の溶剤抽出工程から得られるエキストラクト油などが利用されているのが現状である(例えば、特許文献1、2参照)。   To recycle pavement waste, mix pavement waste, new aggregate, and new asphalt with a mixer in the asphalt mixture factory, and the penetration and elongation of the asphalt hardened by the deterioration contained in the pavement waste. In order to restore the initial softness, a method for regenerating degraded asphalt by adding an asphalt regeneration additive has been performed. This asphalt regeneration additive uses mineral oil with high aromaticity, for example, extract oil obtained from the solvent extraction process of petroleum refining, for the purpose of supplementing aromatic components in asphalt lost due to deterioration. Is the current situation (see, for example, Patent Documents 1 and 2).

このような芳香族性の高い鉱油は、劣化したアスファルト中の芳香族成分を補うため、劣化により大きく低下した針入度、伸度を回復させる能力が高い。特に伸度を大きく回復させるためには、添加する鉱油には高い芳香族性が要求される。ところが、芳香族性の高い鉱油には多量の多環芳香族(PCA)が含まれるため、環境、人体に対する負荷が大きく、現在、環境および人体に対する安全性が高いアスファルト再生添加剤の開発に対する要望が高くなっている。
特開平02−091303号 特開平08−333515号
Such mineral oil with high aromaticity compensates for the aromatic component in the deteriorated asphalt, and therefore has a high ability to recover the penetration and elongation greatly reduced due to deterioration. In particular, in order to greatly recover the elongation, the added mineral oil is required to have high aromaticity. However, since mineral oils with high aromaticity contain a large amount of polycyclic aromatics (PCA), there is a heavy burden on the environment and the human body, and there is a demand for the development of an asphalt regeneration additive that is currently highly safe for the environment and the human body. Is high.
Japanese Patent Laid-Open No. 02-091303 JP 08-333515 A

環境および人体に対する安全性に優れ、かつ舗装廃材中に含まれる劣化を受け硬化したアスファルトを初期の軟らかさまで繰り返し回復させる、すなわち低下した針入度、伸度を繰り返し大きく回復するアスファルト再生添加剤が求められている。   An asphalt regeneration additive that is highly safe for the environment and the human body, and that repeatedly recovers the asphalt that has deteriorated and hardened in the pavement waste to its initial softness, that is, it repeatedly recovers greatly reduced penetration and elongation. It has been demanded.

本発明者らは、前記課題について鋭意研究を重ねた結果、油脂に劣化したアスファルトの針入度、伸度を大きく回復する能力があることを確認し、環境および人体に対する安全性が高く、かつ舗装廃材中の劣化アスファルトの針入度、伸度を繰り返し大きく回復することができる高性能なアスファルト再生添加剤組成物が得られることを見出し、本発明を完成するに至ったものである。   As a result of intensive studies on the above problems, the present inventors have confirmed that oil and fat have the ability to greatly recover the penetration and elongation of asphalt that has deteriorated, and are highly safe for the environment and the human body, and The present inventors have found that a high-performance asphalt regeneration additive composition capable of repeatedly recovering the penetration and elongation of deteriorated asphalt in paving waste materials can be obtained, and have completed the present invention.

すなわち、本発明の第1は40℃における動粘度が300〜900mm/s、多環芳香族分(PCA)が3質量%未満である鉱油と油脂を配合して得られる組成物であって、40℃における動粘度が40〜400mm/s、多環芳香族分(PCA)が3質量%未満、引火点が220℃以上であることを特徴としたアスファルト再生添加剤組成物に関する。 That is, the first of the present invention is a composition obtained by blending mineral oil and fat with a kinematic viscosity at 40 ° C. of 300 to 900 mm 2 / s and a polycyclic aromatic content (PCA) of less than 3% by mass. And an asphalt regeneration additive composition having a kinematic viscosity at 40 ° C. of 40 to 400 mm 2 / s, a polycyclic aromatic content (PCA) of less than 3% by mass, and a flash point of 220 ° C. or more.

本発明の第2は、本発明の第1のアスファルト再生添加剤組成において、鉱油と油脂の配合割合が、鉱油10〜90質量%、油脂90〜10質量%(合計100質量%)であることを特徴とするものである。   2nd of this invention WHEREIN: In the 1st asphalt reproduction | regeneration additive composition of this invention, the mixture ratio of mineral oil and fats and oils is 10-90 mass% of mineral oils, and 90-10 mass% of fats and oils (100 mass% in total). It is characterized by.

本発明の第3は、本発明の第1または2のアスファルト再生添加剤組成物において、油脂の脂肪酸部分が炭素数3から18である飽和脂肪酸、不飽和脂肪酸、又はこれらの混合物であることを特徴とするものである。   The third aspect of the present invention is that in the first or second asphalt regeneration additive composition of the present invention, the fatty acid part of the fat is a saturated fatty acid having 3 to 18 carbon atoms, an unsaturated fatty acid, or a mixture thereof. It is a feature.

本発明の第4は、本発明の第1〜3のいずれか1のアスファルト再生添加剤組成物において、油脂が動物油脂又は植物油脂であることを特徴とするものである。 A fourth aspect of the present invention is the asphalt regeneration additive composition according to any one of the first to third aspects of the present invention, wherein the fat is an animal fat or a vegetable fat.

本発明の第5は、本発明の第1〜3のいずれか1のアスファルト再生添加剤組成物において、油脂が動物油脂又は植物油脂の廃油を原料とすることを特徴とするものである。 According to a fifth aspect of the present invention, in the asphalt regeneration additive composition according to any one of the first to third aspects of the present invention, the fat is made from a waste oil of animal fat or vegetable fat.

本発明のアスファルト再生添加剤組成物は、環境および人体に対する安全性に優れ、かつ、舗装廃材中に含まれる劣化を受け硬化したアスファルトを再生する能力が高いため、針入度、伸度を大きく回復させることができる。   The asphalt regeneration additive composition of the present invention is excellent in safety to the environment and the human body, and has a high ability to regenerate the asphalt that has been hardened due to deterioration contained in pavement waste, so that the penetration and elongation are large. Can be recovered.

以下、本発明について詳述する。
(鉱油の動粘度)
本発明にかかる鉱油の40℃における動粘度は、300〜900mm/sであることが必要である。40℃における動粘度が300mm/sより低い場合は、軽質留分を多くむため、アスファルト舗装混合物を作製するときに高温の骨材と接触すると白煙が生じ好ましくない。一方、40℃における動粘度が900mm/sを超える場合は、流動性が低下してハンドリング性が悪くなるとともに、針入度、伸度を回復させるために多量の鉱油が必要となることから好ましくない。かかる理由から、40℃における動粘度の下限は350mm/s以上が好ましく、400mm/s以上がより好ましい。また、上限は800mm/s以下が好ましく、700mm/s以下がより好ましい。
なお、ここでいう40℃における動粘度とは、JIS K2283「原油及び石油製品−動粘度試験方法及び粘度指数算出方法」により測定される動粘度(mm/s)を意味する。
Hereinafter, the present invention will be described in detail.
(Kinematic viscosity of mineral oil)
The kinematic viscosity at 40 ° C. of the mineral oil according to the present invention needs to be 300 to 900 mm 2 / s. When the kinematic viscosity at 40 ° C. is lower than 300 mm 2 / s, the light fraction is increased. Therefore, when making an asphalt pavement mixture, white smoke is undesirably generated when it comes into contact with high-temperature aggregate. On the other hand, when the kinematic viscosity at 40 ° C. exceeds 900 mm 2 / s, the fluidity is lowered and handling properties are deteriorated, and a large amount of mineral oil is required to recover the penetration and elongation. It is not preferable. For this reason, the lower limit of the kinematic viscosity at 40 ° C. is preferably 350 mm 2 / s or more, and more preferably 400 mm 2 / s or more. The upper limit is preferably 800 mm 2 / s or less, more preferably 700 mm 2 / s.
Here, the kinematic viscosity at 40 ° C. means a kinematic viscosity (mm 2 / s) measured by JIS K2283 “Crude oil and petroleum products—Kinematic viscosity test method and viscosity index calculation method”.

(鉱油の多環芳香族の含有量)
本発明にかかる鉱油中の多環芳香族分(PCA)は、3質量%未満であることが必要である。鉱油中のPCAが3質量%以上であると、環境及び人体に対する負荷が高まる恐れがあるため好ましくない。かかる理由からPCAは、2.8質量%未満が好ましく、2質量%未満がより好ましい、さらに1質量%未満が好ましい。さらに言うなら0.3質量%未満が特に好ましい。
なお、ここでいう多環芳香族分(PCA)とは、”The Institute of Petroleum”のIP346/92 ”Determination of polycyclic aromatics in unused lubricating base oils and asphaltene free petroleum fractions - Dimethyl sulphoxide extraction refractive index method”の方法に準拠して得られる多環芳香族炭化水素化合物の含有量(質量%)のことを意味する。
(Polycyclic aromatic content of mineral oil)
The polycyclic aromatic content (PCA) in the mineral oil according to the present invention needs to be less than 3% by mass. If the PCA in the mineral oil is 3% by mass or more, the load on the environment and the human body may increase, such being undesirable. For this reason, PCA is preferably less than 2.8% by mass, more preferably less than 2% by mass, and even more preferably less than 1% by mass. If it says further, less than 0.3 mass% is especially preferable.
The polycyclic aromatics (PCA) here refers to “The Institute of Petroleum” IP346 / 92 “Determination of polycyclic aromatics in unused lubricant base oils and asphaltene free petroleum fractions-Dimethyl sulphoxide extraction refractive index method”. It means the content (% by mass) of the polycyclic aromatic hydrocarbon compound obtained according to the method.

(鉱油の引火点)
本発明にかかる鉱油の引火点は220℃以上であることが好ましい。鉱油の引火点が
220℃未満の場合は、アスファルト舗装混合物の製造時の安全性が低下するため好ましくない。かかる理由から引火点は、230℃以上がより好ましく、250℃以上がさらに好ましい。なお、ここでいう引火点とはJIS K2265「原油及び石油製品−引火点試験方法」のクリーブランド開放式引火点試験方法により測定される引火点(℃)を意味する。
(The flash point of mineral oil)
The flash point of the mineral oil according to the present invention is preferably 220 ° C. or higher. When the flash point of mineral oil is less than 220 ° C., the safety during production of the asphalt pavement mixture decreases, which is not preferable. For this reason, the flash point is more preferably 230 ° C. or higher, and further preferably 250 ° C. or higher. The flash point here means the flash point (° C.) measured by the Cleveland open-type flash point test method of JIS K2265 “Crude oil and petroleum products—Flash point test method”.

(鉱油の密度)
本発明にかかる鉱油の15℃における密度は0.88〜0.95/cmであることが好ましい。鉱油の15℃における密度が0.88g/cm未満だと、軽質成分を多く含むため、舗装廃材の再生時に白煙が生じやすくなり好ましくない。よって、密度の下限は0.90g/cm以上がより好ましい。一方、密度の上限は0.95g/cmを超えると芳香族成分の割合が高く、PCAが3質量%以上になる恐れが生じ、環境、人体への負荷が大きくなるため好ましくない。かかる理由から0.94g/cm以下がより好ましい。
なお、ここでいう密度とはJIS K2249「原油及び石油製品−密度試験方法」により測定される15℃における密度(g/cm)を意味する。
(Mineral oil density)
The density of the mineral oil according to the present invention at 15 ° C. is preferably 0.88 to 0.95 / cm 3 . If the density of the mineral oil at 15 ° C. is less than 0.88 g / cm 3 , since it contains a lot of light components, white smoke is likely to be generated during the regeneration of the paving waste, which is not preferable. Therefore, the lower limit of the density is more preferably 0.90 g / cm 3 or more. On the other hand, if the upper limit of the density exceeds 0.95 g / cm 3 , the ratio of the aromatic component is high, PCA may be 3% by mass or more, and the load on the environment and the human body increases. For this reason, 0.94 g / cm 3 or less is more preferable.
In addition, the density here means the density (g / cm 3 ) at 15 ° C. measured by JIS K2249 “Crude oil and petroleum products—density test method”.

(鉱油の%CA)
本発明にかかる鉱油の%CAは20%未満であることが好ましい。%CAが20%以上であるとPCAが3質量%以上になる恐れがあり、環境、人体への負荷が大きくなるため好ましくない。かかる理由から18%以下であることがより好ましく、15%以下であることがさらに好ましい。
なお、ここでいう%CAとは、ASTM D3238“Standard Test Method for Calculation of Carbon Distribution and Structural Group Analysis of Petroleum Oils by the n-d-M Method”により測定される全炭素数に対する芳香族環炭素数の百分率(%)を意味する。
(% CA of mineral oil)
The% CA of the mineral oil according to the present invention is preferably less than 20%. If% CA is 20% or more, PCA may be 3% by mass or more, which increases the load on the environment and the human body. For this reason, it is more preferably 18% or less, and further preferably 15% or less.
In addition,% CA here refers to the percentage of the number of aromatic ring carbons to the total number of carbons measured by ASTM D3238 “Standard Test Method for Calculation of Carbon Distribution and Structural Group Analysis of Petroleum Oils by the ndM Method” (% ).

(鉱油のアニリン点)
本発明にかかる鉱油のアニリン点は70℃以上であることが好ましい。アニリン点が
70℃未満であるとPCAが3質量%以上になる恐れがあり、環境、人体への負荷が大きくなるため好ましくない。かかる理由から80℃以上がより好ましく、85℃以上がさらに好ましい。
なお、ここでいうアニリン点とはJIS K2256「石油製品アニリン点及び混合アニリン点試験方法」により測定されるアニリン点(℃)を意味する。
(Aniline point of mineral oil)
The aniline point of the mineral oil according to the present invention is preferably 70 ° C. or higher. If the aniline point is less than 70 ° C., the PCA may be 3% by mass or more, which increases the load on the environment and the human body. For this reason, 80 ° C. or higher is more preferable, and 85 ° C. or higher is more preferable.
Here, the aniline point means an aniline point (° C.) measured by JIS K2256 “Petroleum product aniline point and mixed aniline point test method”.

(鉱油の薄膜加熱質量変化率)
本発明にかかる鉱油の薄膜加熱質量変化率は−3.0質量%以下(薄膜加熱減量が3.0質量%以下)であることが好ましい。薄膜加熱質量変化率が−3.0質量%を超える(薄膜加熱減量が3.0質量%を超える)場合、軽質成分を多く含むため、舗装廃材の再生時に白煙が生じやすくなり好ましくない。かかる理由から−2.0質量%以下(薄膜加熱減量が2.0質量%以下)がより好ましく、−1.0質量%以下(薄膜加熱減量が1.0質量%以下)がさらに好ましい。さらに言うなら、−0.5質量%以下(薄膜加熱減量が0.5質量%以下)がより好ましい。
なお、ここでいう薄膜加熱質量変化率とは、JIS K2207「石油アスファルト−薄膜加熱試験法」により測定される薄膜加熱質量変化率(質量%)を指し、負の値は質量の減量を意味する。
(Change rate of heating mass of mineral oil)
The thin film heating mass change rate of the mineral oil according to the present invention is preferably −3.0 mass% or less (thin film heating loss is 3.0 mass% or less). When the thin film heating mass change rate exceeds −3.0 mass% (thin film heating loss exceeds 3.0 mass%), since it contains a large amount of light components, white smoke is likely to be generated during the regeneration of paving waste, which is not preferable. For this reason, −2.0 mass% or less (thin film heating loss is 2.0 mass% or less) is more preferable, and −1.0 mass% or less (thin film heating loss is 1.0 mass% or less) is more preferable. If it says further, -0.5 mass% or less (a thin film heating loss will be 0.5 mass% or less) is more preferable.
The thin film heating mass change rate here refers to the thin film heating mass change rate (mass%) measured by JIS K2207 “Petroleum Asphalt—Thin Film Heating Test Method”, and a negative value means a weight loss. .

(鉱油)
本発明の鉱油を製造する際に用いる原油は特に限定されるものではないが、例えば、ペンシルベニヤ原油、ミナス原油、大慶原油等のパラフィン基原油、カリフォルニア原油、テキサス原油、ベネズエラ原油等のナフテン基原油、ミッドコンチネント原油、アラビア原油、ガッチサラン原油、カフジ原油、マヤ原油、ニュートラルゾーンスペシャル原油、フート原油、クェート原油、ラタウェー原油、アルライアン原油、エオシン原油、ソリューシュ原油等の混合基原油等が好ましい。この中でも好ましくは、混合基原油、ナフテン基原油である。
(Mineral oil)
The crude oil used in producing the mineral oil of the present invention is not particularly limited. Preferred are crude crude oil, mid-continuous crude oil, Arabic crude oil, Gucci Saran crude oil, Kafuji crude oil, Maya crude oil, neutral zone special crude oil, Foot crude oil, Kuwait crude oil, Rataway crude oil, Allian crude oil, Eosin crude oil, Solish crude oil and the like. Of these, mixed base crude oil and naphthene base crude oil are preferable.

本発明の鉱油は40℃の動粘度、PCAの含有量、が上述の範囲であり、これと油脂を配合して得られるアスファルト再生添加剤組成物が所定の性状を満たしていれば、特に限定されるものではないが、溶剤脱れき、溶剤抽出、水素化分解溶剤脱ろう、接触脱ろう、水素化精製、硫酸洗浄、白土処理等を適宜組み合わせて精製した留分を使用できる。特に原油を減圧蒸留して得られる潤滑油留分を、フルフラールを用いて潤滑油留分中の芳香族化合物やレジン分をとり除くフルフラール抽出などの溶剤抽出、減圧蒸留残渣油から液体プロパンを用いて潤滑油留分を抽出し、アスファルト分や樹脂分を分離するプロパン脱れきなどの溶剤脱れき、MEK等の溶剤を用いてろう分を除去するMEK脱ろうなどの溶剤脱ろう、及び水素化精製を組み合わせて得られる高粘度高級潤滑油成分(ブライトストック)などが好適に用いられる。好ましくは、混合基原油およびナフテン基原油を処理し得られた高粘度高級潤滑油成分(ブライトストック)である。   The mineral oil of the present invention has a kinematic viscosity of 40 ° C. and a PCA content within the above-mentioned ranges, and is particularly limited if the asphalt regeneration additive composition obtained by blending this with oils and fats satisfies predetermined properties. However, it is possible to use a fraction that has been purified by a suitable combination of solvent removal, solvent extraction, hydrocracking solvent dewaxing, catalytic dewaxing, hydrorefining, sulfuric acid washing, clay treatment, and the like. In particular, the oil fraction obtained by distilling crude oil under reduced pressure is extracted with a solvent extraction such as furfural extraction using a furfural to remove aromatics and resin in the oil fraction, and liquid propane is used from the oil obtained by distillation under reduced pressure. Solvent dewaxing, such as MEK dewaxing, which removes wax using a solvent such as MEK, and hydrorefining A high-viscosity high-grade lubricating oil component (bright stock) or the like obtained by combining these is preferably used. Preferably, it is a high viscosity high-grade lubricating oil component (bright stock) obtained by processing mixed base crude oil and naphthene base crude oil.

(油脂)
本発明の油脂は動物油脂又は植物油脂が好ましい。より好ましくは植物油脂である。動物油脂の原料としては、牛脂、牛乳脂質(バター)、豚脂、羊脂、鯨油、魚油、肝油等の動物油脂が挙げられる、植物油脂としては、ココヤシ、パームヤシ、オリーブ、べにばな、菜種(菜の花)、米ぬか、ひまわり、綿実、とうもろこし、大豆、ごま等の種子部及びその他の部分等から得られる植物油脂が挙げられる。また、本発明においては、これらの動物油脂、植物油脂を民生用、産業用、食用等で使用した廃油脂も雑物等の除去工程を加えた後に原料とすることができる。
(Oil)
The oil of the present invention is preferably animal oil or vegetable oil. More preferred is vegetable oil. Animal fats and oils include animal fats such as beef tallow, milk fat (butter), pork tallow, sheep fat, whale oil, fish oil, liver oil, etc. Examples of vegetable oils are coconut palm, palm palm, olive, Examples include vegetable oils and fats obtained from rapeseed (rapeseed), rice bran, sunflower, cottonseed, corn, soybean, sesame seeds and other parts. Moreover, in this invention, the waste fats and oils which used these animal fats and vegetable fats and oils for consumer use, industrial use, food use, etc. can also be used as a raw material after adding the removal process of miscellaneous matters.

これらの油脂を構成するグリセライドの脂肪酸部分が炭素数3〜18である飽和脂肪酸、不飽和結合を1つ若しくは複数有する不飽和脂肪酸、又はこれらの混合物であることが好ましい。またこれら油脂の凝固点は20℃以下であることが望ましく、0℃以下であればより望ましい。また−10℃以下であればさらにより好ましい。またこれら油脂の凝固点が低いほど、得られるアスファルト再生添加剤組成物の凝固点も低くなる傾向にあり、低温下でのハンドリング性が優れたものとなる。ただし、凝固点が20℃を超える油脂を配合する場合であっても、凝固点以上に加温することにより容易に液状化できるため、本アスファルト再生添加剤組成物に用いる油脂として使用することができる。   It is preferable that the fatty acid part of the glyceride constituting these fats and oils is a saturated fatty acid having 3 to 18 carbon atoms, an unsaturated fatty acid having one or more unsaturated bonds, or a mixture thereof. Further, the freezing point of these fats and oils is desirably 20 ° C. or less, and more desirably 0 ° C. or less. Moreover, it is still more preferable if it is -10 degrees C or less. Further, the lower the freezing point of these fats and oils, the lower the freezing point of the resulting asphalt regeneration additive composition, and the better the handling properties at low temperatures. However, even when fats and oils having a freezing point exceeding 20 ° C. are blended, they can be easily liquefied by heating above the freezing point, so that they can be used as fats and oils used in the present asphalt regeneration additive composition.

炭素数3〜18の飽和脂肪酸の例としては、酪酸(CCOOH)、カプロン酸(C11COOH)、カプリル酸(C15COOH)、カプリン酸(C19COOH)、ラウリン酸(C1123COOH)、ミリスチン酸(C1327COOH)、パルミチン酸(C1531COOH)、ステアリン酸(C1735COOH)等が挙げられる。また、炭素数3〜18の不飽和脂肪酸の例としてはオレイン酸(C1733COOH)、リノール酸(C1731COOH)、リノレン酸(C1729COOH)、リシノレン酸(C1732(OH)COOH)等が挙げられる。自然界の物質におけるこれら脂肪酸の炭化水素部は一般に直鎖であることが多いが、本発明においては側鎖を有する構造、すなわち異性体であっても使用することができる。また、不飽和脂肪酸における分子中の不飽和結合の位置も、本発明においては自然界で一般に存在確認されているものだけでなく、化学合成によって任意の位置に設定されたものも使用することができる。
上述の油脂(動物油、植物油)はこれらの脂肪酸基を1種または複数種有しており、油脂の種類によってその有する脂肪酸類は異なっている。例えば、ココヤシ油はラウリン酸、ミリスチン酸等の飽和脂肪酸を比較的多く有しているが、菜種油、大豆油はオレイン酸、リノール酸等の不飽和脂肪酸を多く有している。
Examples of saturated fatty acids having 3 to 18 carbon atoms include butyric acid (C 3 H 7 COOH), caproic acid (C 5 H 11 COOH), caprylic acid (C 7 H 15 COOH), capric acid (C 9 H 19 COOH) ), Lauric acid (C 11 H 23 COOH), myristic acid (C 13 H 27 COOH), palmitic acid (C 15 H 31 COOH), stearic acid (C 17 H 35 COOH), and the like. Examples of unsaturated fatty acids having 3 to 18 carbon atoms include oleic acid (C 17 H 33 COOH), linoleic acid (C 17 H 31 COOH), linolenic acid (C 17 H 29 COOH), and ricinolenic acid (C 17 H 32 (OH) COOH) and the like. In general, the hydrocarbon portion of these fatty acids in natural substances is generally linear, but in the present invention, even a structure having a side chain, that is, an isomer can be used. Moreover, the position of the unsaturated bond in the molecule of the unsaturated fatty acid is not limited to those generally confirmed in nature in the present invention, but can also be used at any position set by chemical synthesis. .
The above-mentioned fats and oils (animal oil, vegetable oil) have one or more of these fatty acid groups, and the fatty acids they have vary depending on the type of fat. For example, coconut oil has a relatively large amount of saturated fatty acids such as lauric acid and myristic acid, while rapeseed oil and soybean oil have a large amount of unsaturated fatty acids such as oleic acid and linoleic acid.

これらの油脂中の脂肪酸組成の定量はガスクロマトグラフを用いて行うことができる。分析条件を以下に示すが、遊離脂肪酸型カラム(FFAP)を用いることで、容易にかつ正確にこれらの物質を定量することができる。
カラム:FFAP(φ0.32mm×25m)
キャリアガス:He(26psi)
検出器:FID
インジェクション温度:280℃
検出器温度:300℃
オーブン温度:100〜260℃(10分)
昇温速度:5℃/分
インジェクション量:0.4μL(メタノール溶液)
The fatty acid composition in these fats and oils can be quantified using a gas chromatograph. Analytical conditions are shown below. By using a free fatty acid type column (FFAP), these substances can be easily and accurately quantified.
Column: FFAP (φ0.32mm × 25m)
Carrier gas: He (26 psi)
Detector: FID
Injection temperature: 280 ° C
Detector temperature: 300 ° C
Oven temperature: 100-260 ° C (10 minutes)
Temperature increase rate: 5 ° C./min Injection amount: 0.4 μL (methanol solution)

(配合)
本発明のアスファルト再生添加剤組成物は、舗装廃材の再生能力、さらには繰り返しの再生能力を充分に確保するために、前述の鉱油の配合割合はアスファルト再生添加剤組成物全量に対し10〜90質量%であることが好ましい。また、前述の油脂(グリセライド化合物)の配合割合はアスファルト再生添加剤組成物全量に対し90〜10質量%であることが好ましい。ここで、鉱油と油脂の合計が100質量%。油脂の配合割合が10質量%未満の場合、使用する鉱油によっては舗装廃材中の劣化アスファルトの伸度を十分に回復することができないため、10質量%以上が好ましく、20質量%以上がより好ましく、30質量%以上がさらに好ましい。一方、油脂の配合割合が90重量%を越えた場合、針入度、伸度を回復させるために必要な添加量が極端に少なくなるため、舗装廃材中の劣化アスファルトに再生添加剤が均一に行き渡らず、不均一に再生されたアスファルト舗装混合物となる懸念が生じるため、90質量%以下が好ましく、85質量%以下がより好ましく、80質量%以下がさらに好ましい。
(Combination)
The asphalt regeneration additive composition of the present invention has the above-mentioned mineral oil blending ratio of 10 to 90 with respect to the total amount of the asphalt regeneration additive composition in order to sufficiently secure the regeneration ability of paving waste materials and further the ability of repeated regeneration. It is preferable that it is mass%. Moreover, it is preferable that the mixture ratio of the above-mentioned fats and oils (glyceride compound) is 90-10 mass% with respect to the asphalt reproduction | regeneration additive composition whole quantity. Here, the sum total of mineral oil and fats and oils is 100 mass%. When the blending ratio of fats and oils is less than 10% by mass, the elongation of the deteriorated asphalt in the pavement waste material cannot be sufficiently recovered depending on the mineral oil used, preferably 10% by mass or more, more preferably 20% by mass or more. 30% by mass or more is more preferable. On the other hand, when the blending ratio of fats and oils exceeds 90% by weight, the amount of addition necessary to recover the penetration and elongation is extremely reduced, so that the regenerated additive is uniformly applied to the deteriorated asphalt in the paving waste material. 90% by mass or less is preferable, 85% by mass or less is more preferable, and 80% by mass or less is more preferable because there is a concern that the asphalt pavement mixture is not spread and is regenerated unevenly.

(再生添加剤組成物の動粘度)
本発明のアスファルト再生添加剤組成物の動粘度(40℃)は40〜400mm/sであることが必要である。動粘度(40℃)が400mm/s以上の場合、舗装廃材中の劣化アスファルトの針入度を回復するための必要添加量が大きくなり、また取り扱い上のハンドリング性が低下する。一方、動粘度(40℃)が40mm/s以下の場合、舗装廃材中の劣化アスファルトの針入度、伸度を回復させるために必要な添加量が極端に少なくなるため、舗装廃材中の劣化アスファルトに再生添加剤が均一に行き渡らず、不均一に再生されたアスファルト舗装混合物となる懸念が生じる。かかる理由から、本発明のアスファルト再生添加剤組成物の動粘度(40℃)は50mm/s以上が好ましく、80mm/s以上がより好ましい。一方、上限は350mm/s以下が好ましく、300mm/s以下がより好ましい。
(Kinematic viscosity of regenerated additive composition)
The kinematic viscosity (40 ° C.) of the asphalt regeneration additive composition of the present invention needs to be 40 to 400 mm 2 / s. When kinematic viscosity (40 degreeC) is 400 mm < 2 > / s or more, the required addition amount for recovering the penetration of the degradation asphalt in a paving waste material becomes large, and the handleability on handling falls. On the other hand, when the kinematic viscosity (40 ° C.) is 40 mm 2 / s or less, the amount of addition required for recovering the penetration and elongation of deteriorated asphalt in the paving waste material is extremely reduced. There is a concern that the regenerated additive does not spread uniformly over the deteriorated asphalt, resulting in a non-uniformly regenerated asphalt pavement mixture. For this reason, the kinematic viscosity (40 ° C.) of the asphalt regeneration additive composition of the present invention is preferably 50 mm 2 / s or more, and more preferably 80 mm 2 / s or more. On the other hand, the upper limit is preferably at most 350 mm 2 / s, more preferably at most 300 mm 2 / s.

(再生添加剤組成物の引火点)
本発明のアスファルト再生添加剤組成物の引火点は220℃以上であることが必要である。アスファルト再生添加剤組成物の引火点が220℃未満の場合は、アスファルト舗装混合物の製造時の安全性が低下するため好ましくない。かかる理由から引火点は、230℃以上がより好ましく、250℃以上がさらに好ましい。
なお、ここでいう引火点とはJIS K2265「原油及び石油製品−引火点試験方法」のクリーブランド開放式引火点試験方法により測定される引火点(℃)を意味する。
(Flash point of regenerated additive composition)
The flash point of the asphalt regeneration additive composition of the present invention needs to be 220 ° C. or higher. When the flash point of the asphalt regeneration additive composition is less than 220 ° C., safety during production of the asphalt pavement mixture is lowered, which is not preferable. For this reason, the flash point is more preferably 230 ° C. or higher, and further preferably 250 ° C. or higher.
The flash point here means the flash point (° C.) measured by the Cleveland open-type flash point test method of JIS K2265 “Crude oil and petroleum products—Flash point test method”.

(再生添加剤組成物中の多環芳香族の含有量)
本発明のアスファルト再生添加剤組成物の多環芳香族分(PCA)は、3質量%未満であることが必要である。鉱油中のPCAが3質量%以上であると、環境及び人体に対する負荷が高まる恐れがあるため好ましくない。かかる理由からPCAは、2.8質量%未満が好ましく、2質量%未満がより好ましい、さらには1質量%未満が好ましい。さらに言うなら0.2質量%未満が特に好ましい。
なお、ここでいう多環芳香族分(PCA)とは、”The Institute of Petroleum”のIP346/92 ”Determination of polycyclic aromatics in unused lubricating base oils and asphaltene free petroleum fractions - Dimethyl sulphoxide extraction refractive index method”の方法に準拠して得られる多環芳香族炭化水素化合物の含有量(質量%)のことを意味する。
(Polycyclic aromatic content in the regenerative additive composition)
The polycyclic aromatic content (PCA) of the asphalt regeneration additive composition of the present invention needs to be less than 3% by mass. If the PCA in the mineral oil is 3% by mass or more, the load on the environment and the human body may increase, such being undesirable. For this reason, PCA is preferably less than 2.8% by mass, more preferably less than 2% by mass, and even more preferably less than 1% by mass. Furthermore, if it says, less than 0.2 mass% is especially preferable.
The polycyclic aromatics (PCA) here refers to “The Institute of Petroleum” IP346 / 92 “Determination of polycyclic aromatics in unused lubricant base oils and asphaltene free petroleum fractions-Dimethyl sulphoxide extraction refractive index method”. It means the content (% by mass) of the polycyclic aromatic hydrocarbon compound obtained according to the method.

(再生添加剤組成物の薄膜加熱質量変化率)
本発明のアスファルト再生添加剤組成物の薄膜加熱質量変化率は−3.0質量%以下(薄膜加熱減量が3.0質量%以下)であることが好ましい。薄膜加熱質量変化率が−3.0質量%を超える(薄膜加熱減量が3.0質量%を超える)場合、軽質成分を多く含むため、舗装廃材の再生時に白煙が生じやすくなり好ましくない。かかる理由から−2.0質量%以下(薄膜加熱減量が2.0質量%以下)がより好ましく、−1.0質量%以下(薄膜加熱減量が1.0質量%以下)がさらに好ましい。さらに言うなら、−0.5質量%以下(薄膜加熱減量が0.5質量%以下)がより好ましい。
なお、ここでいう薄膜加熱質量変化率とは、JIS K2207「石油アスファルト−薄膜加熱試験法」により測定される薄膜加熱質量変化率(質量%)を指し、負の値は質量の減量を意味する。
(Thin film heating mass change rate of regeneration additive composition)
The thin film heating mass change rate of the asphalt regeneration additive composition of the present invention is preferably -3.0 mass% or less (thin film heating loss is 3.0 mass% or less). When the thin film heating mass change rate exceeds −3.0 mass% (thin film heating loss exceeds 3.0 mass%), since it contains a large amount of light components, white smoke is likely to be generated during the regeneration of paving waste, which is not preferable. For this reason, −2.0 mass% or less (thin film heating loss is 2.0 mass% or less) is more preferable, and −1.0 mass% or less (thin film heating loss is 1.0 mass% or less) is more preferable. If it says further, -0.5 mass% or less (a thin film heating loss will be 0.5 mass% or less) is more preferable.
The thin film heating mass change rate here refers to the thin film heating mass change rate (mass%) measured by JIS K2207 “Petroleum Asphalt—Thin Film Heating Test Method”, and a negative value means a weight loss. .

(鉱油、油脂以外の添加剤構成物)
本発明のアスファルト再生添加剤組成物は上述した所定の性状を満たしさえすれば、鉱油と油脂以外に、酪酸メチルエステル(CCOOCH)、カプロン酸メチルエステル(C11COOCH)、カプリル酸メチルエステル(C15COOCH)、カプリン酸メチルエステル(C19COOCH)、ラウリン酸メチルエステル(C1123COOCH)、ミリスチン酸メチルエステル(C1327COOCH)、パルミチン酸メチルエステル(C1531COOCH)、ステアリン酸メチルエステル(C1735COOCH)、オレイン酸メチルエステル(C1733COOCH)、リノール酸メチルエステル(C1731COOCH)、リノレン酸メチルエステル(C1729COOCH)、リシノレン酸メチルエステル(C1732(OH)COOCH)、酪酸エチルエステル(CCOOC)、カプロン酸エチルエステル(C11COOC)、カプリル酸エチルエステル(C15COOC)、カプリン酸エチルエステル(C19COOC)、ラウリン酸エチルエステル(C1123COOC)、ミリスチン酸エチルエステル(C1327COOC)、パルミチン酸エチルエステル(C1531COOC)、ステアリン酸エチルエステル(C1735COOC)、オレイン酸エチルエステル(C1733COOC)、リノール酸エチルエステル(C1731COOC)、リノレン酸エチルエステル(C1729COOC)、リシノレン酸エチルエステル(C1732(OH)COOC)等の植物油脂、動物油脂、あるいは廃油を原料とした脂肪酸アルキルエステル化合物、酪酸(CCOOH)、カプロン酸(C11COOH)、カプリル酸(C15COOH)、カプリン酸(C19COOH)、ラウリン酸(C1123COOH)、ミリスチン酸(C1327COOH)、パルミチン酸(C1531COOH)、ステアリン酸(C1735COOH)等の炭素数3〜24の飽和脂肪酸、オレイン酸(C1733COOH)、リノール酸(C1731COOH)、リノレン酸(C1729COOH)、リシノレン酸(C1732(OH)COOH)等の炭素数3〜24の不飽和脂肪酸等を1種あるいは2種以上配合してもよい。
(Additive composition other than mineral oil and fat)
As long as the asphalt regeneration additive composition of the present invention satisfies the above-described predetermined properties, butyric acid methyl ester (C 3 H 7 COOCH 3 ), caproic acid methyl ester (C 5 H 11 COOCH 3 ), in addition to mineral oil and fats and oils. ), Caprylic acid methyl ester (C 7 H 15 COOCH 3 ), capric acid methyl ester (C 9 H 19 COOCH 3 ), lauric acid methyl ester (C 11 H 23 COOCH 3 ), myristic acid methyl ester (C 13 H 27) COOCH 3 ), palmitic acid methyl ester (C 15 H 31 COOCH 3 ), stearic acid methyl ester (C 17 H 35 COOCH 3 ), oleic acid methyl ester (C 17 H 33 COOCH 3 ), linoleic acid methyl ester (C 17 H 31 COOCH 3), Li Ren acid methyl ester (C 17 H 29 COOCH 3) , ricinoleic acid methyl ester (C 17 H 32 (OH) COOCH 3), ethyl butyrate ester (C 3 H 7 COOC 2 H 5), caproic acid ethyl ester (C 5 H 11 COOC 2 H 5 ), caprylic acid ethyl ester (C 7 H 15 COOC 2 H 5 ), capric acid ethyl ester (C 9 H 19 COOC 2 H 5 ), lauric acid ethyl ester (C 11 H 23 COOC 2 H 5 ), myristic acid ethyl ester (C 13 H 27 COOC 2 H 5 ), palmitic acid ethyl ester (C 15 H 31 COOC 2 H 5 ), stearic acid ethyl ester (C 17 H 35 COOC 2 H 5 ), oleic acid ethyl ester (C 17 H 33 COOC 2 H 5), Nord acid ethyl ester (C 17 H 31 COOC 2 H 5), linolenic acid ethyl ester (C 17 H 29 COOC 2 H 5), ricinoleic acid ethyl ester (C 17 H 32 (OH) COOC 2 H 5) or the like of the plant Fatty acid alkyl ester compounds made from fats and oils, animal fats and oils, butyric acid (C 3 H 7 COOH), caproic acid (C 5 H 11 COOH), caprylic acid (C 7 H 15 COOH), capric acid (C 9 H 19 COOH), lauric acid (C 11 H 23 COOH), myristic acid (C 13 H 27 COOH), palmitic acid (C 15 H 31 COOH), stearic acid (C 17 H 35 COOH), etc. 24 saturated fatty acids, oleic acid (C 17 H 33 COOH), linoleic acid (C 17 H 31 C OH), linolenic acid may be mixed (C 17 H 29 COOH), ricinoleic acid (C 17 H 32 (OH) COOH) an unsaturated fatty acid having a carbon number of 3 to 24 such as one or more kinds.

(再生添加剤の使用方法)
本発明のアスファルト再生添加剤組成物は、プラント再生工法においても、路上再生工法においても使用できる。プラント再生工法では、バッチ式プラント、または連続式プラントにて再生が行われるが、本発明のアスファルト再生添加剤組成物はこれらプラントの形式によらず使用できる。骨材、アスファルト、再生骨材を混合するプラントミキサーに本発明のアスファルト再生添加剤組成物を所定量添加し、ミキシングすることで再生アスファルト混合物が製造できる。一方、路上再生工法では、リミックス方式とリペーブ方式があるが、本発明のアスファルト再生添加剤組成物はこれらの方式によらず使用できる。すなわち、リミックス方式においては加熱、かきほぐした既設表層混合物に本発明のアスファルト再生添加剤組成物を加え、これと新規アスファルト混合物とを混合して敷きならし、締め固めることができる。またリペーブ方式では、加熱、かきほぐした既設表層混合物に本発明のアスファルト再生添加剤組成物を加え、攪拌し敷きならしたうえ、その上部に新規アスファルト混合物を敷きならして、これらを同時に締め固めることができる。
(How to use regenerative additives)
The asphalt regeneration additive composition of the present invention can be used in both a plant regeneration method and a road regeneration method. In the plant regeneration method, regeneration is performed in a batch plant or a continuous plant, but the asphalt regeneration additive composition of the present invention can be used regardless of the type of these plants. A regenerated asphalt mixture can be produced by adding a predetermined amount of the asphalt regenerating additive composition of the present invention to a plant mixer for mixing aggregate, asphalt, and regenerated aggregate, and mixing. On the other hand, in the road regeneration method, there are a remix method and a repave method, but the asphalt regeneration additive composition of the present invention can be used regardless of these methods. That is, in the remix method, the asphalt regeneration additive composition of the present invention can be added to an existing surface mixture heated and loosened, and this and the new asphalt mixture can be mixed and spread and compacted. In addition, in the repebing method, the asphalt regeneration additive composition of the present invention is added to the existing surface mixture that has been heated and cracked, and the mixture is stirred and laid, and then the new asphalt mixture is laid on top and simultaneously compacted. be able to.

本発明のアスファルト再生添加剤組成物の舗装廃材への添加量は、舗装廃材中の劣化したアスファルトの針入度および伸度などを所望の値にまで回復させるのに必要な量であり、
舗装廃材中の劣化したアスファルト100重量部に対し4〜30重量部であることが望ましい。この量が4重量部未満の場合、添加剤が劣化アスファルト全体に行き渡らず不均一な再生となる。一方、30重量部を超える場合、再生効果が過剰となり、特に針入度が所望の値を越えてしまう。かかる理由から好ましい添加量は5〜25重量部、さらに好ましくは、6〜20重量部である。
The amount of the asphalt regeneration additive composition of the present invention added to the paving waste is an amount necessary to restore the penetration and elongation of the deteriorated asphalt in the paving waste to desired values,
The amount is preferably 4 to 30 parts by weight with respect to 100 parts by weight of the deteriorated asphalt in the pavement waste material. When this amount is less than 4 parts by weight, the additive does not spread throughout the deteriorated asphalt, resulting in uneven regeneration. On the other hand, when the amount exceeds 30 parts by weight, the regeneration effect becomes excessive, and in particular, the penetration exceeds a desired value. For this reason, the preferred addition amount is 5 to 25 parts by weight, and more preferably 6 to 20 parts by weight.

以下、実施例により本発明を具体的に説明するが、本発明はこれらによって何ら限定されるものではない。   EXAMPLES Hereinafter, although an Example demonstrates this invention concretely, this invention is not limited at all by these.

[実施例および比較例]
(鉱油)
鉱油は混合基原油を処理して得られたブライトストック(鉱油A)、およびナフテン基原油を処理して得られた潤滑油留分(鉱油B)、および混合基原油を処理し得られたフルフラールエキストラクト(鉱油C)の3種類を使用した。具体的は、鉱油Aは新日本石油(株)製のブライトストックを使用した。鉱油Bは三共油化(株)のSNH440を使用した。鉱油Cは富士興産(株)のアロマックス3を使用した。A、B、Cの性状を表1に示す。鉱油の性状は下記の方法にて分析した。
密度(15℃)はJIS K2249「原油及び石油製品−密度試験方法」により測定される15℃における密度(g/cm)を指す。
引火点(COC)はJIS K2265「原油及び石油製品−引火点試験方法」のクリーブランド開放式引火点試験方法により測定される引火点(℃)を指す。
動粘度(40℃、60℃、100℃)はJIS K2283「原油及び石油製品−動粘度試験方法及び粘度指数算出方法」により測定される40℃、60℃、100℃における動粘度(mm/s)を指す。
アニリン点はJIS K2256「石油製品アニリン点及び混合アニリン点試験方法」により測定されるアニリン点(℃)を指す。
%CP、%CNおよび%CAはそれぞれASTM D3238“Standard Test Method for Calculation of Carbon Distribution and Structural Group Analysis of Petroleum Oils by the n-d-M Method”により測定される全炭素数に対するパラフィン、ナフテン環および芳香族環炭素数の百分率(%)を指す。
PCA含有量は”The Institute of Petroleum”のIP346/92 ”Determination of polycyclic aromatics in unused lubricating base oils and asphaltene free petroleum fractions - Dimethyl sulphoxide extraction refractive index method”の方法に準拠して得られる多環芳香族炭化水素化合物の含有量(質量%)のことを指す。
薄膜加熱質量変化率はJIS K2207「石油アスファルト−薄膜加熱試験法」により測定される薄膜加熱質量変化率(質量%)を指し、正の値は質量の増量を、負の値は質量の減量を意味する。
[Examples and Comparative Examples]
(Mineral oil)
Mineral oil is bright stock (mineral oil A) obtained by processing mixed base crude oil, lubricating oil fraction (mineral oil B) obtained by processing naphthenic base crude oil, and furfural obtained by processing mixed base crude oil Three types of extract (mineral oil C) were used. Specifically, mineral oil A used Bright Stock manufactured by Nippon Oil Corporation. Mineral oil B used was Sankyo Yuka SNH440. Mineral oil C was Aromax 3 from Fuji Kosan. Table 1 shows the properties of A, B, and C. The properties of the mineral oil were analyzed by the following method.
The density (15 ° C.) refers to the density (g / cm 3 ) at 15 ° C. measured by JIS K2249 “Crude oil and petroleum products—Density test method”.
The flash point (COC) refers to the flash point (° C.) measured by the Cleveland open-type flash point test method of JIS K2265 “Crude oil and petroleum products—flash point test method”.
Kinematic viscosity (40 ℃, 60 ℃, 100 ℃) is JIS K2283 - 40 ° C. as measured by the "Crude petroleum and petroleum products kinematic viscosity and calculation of viscosity index", 60 ° C., a kinematic viscosity at 100 ℃ (mm 2 / s).
The aniline point refers to the aniline point (° C.) measured by JIS K2256 “Petroleum product aniline point and mixed aniline point test method”.
% CP,% CN and% CA are paraffin, naphthenic ring and aromatic ring carbon relative to the total number of carbons measured by ASTM D3238 “Standard Test Method for Calculation of Carbon Distribution and Structural Group Analysis of Petroleum Oils by the ndM Method”, respectively. Refers to the percentage (%) of the number.
PCA content is polycyclic aromatic carbonization obtained in accordance with “The Institute of Petroleum” IP346 / 92 “Determination of polycyclic aromatics in unused lubricating base oils and asphaltene free petroleum fractions-Dimethyl sulphoxide extraction refractive index method” It refers to the content (% by mass) of the hydrogen compound.
Thin film heating mass change rate refers to thin film heating mass change rate (% by mass) measured by JIS K2207 “Petroleum Asphalt-Thin Film Heating Test Method”. Positive value indicates mass increase, negative value indicates mass decrease. means.

(油脂)
油脂は菜種油、大豆油、ひまわり油、菜種油と大豆油を主成分とした使用済みのサラダ油(廃食油)の4種類を使用した。使用した油脂の脂肪酸組成を表2に示す。
なお、油脂の脂肪酸組成は上述した遊離脂肪酸型カラム(FFAP)を用いたガスクロマトグラフにより分析した。
(Oil and fat)
Four types of oils and fats were used: rapeseed oil, soybean oil, sunflower oil, used salad oil (waste cooking oil) mainly composed of rapeseed oil and soybean oil. Table 2 shows the fatty acid composition of the fats and oils used.
The fatty acid composition of the fat was analyzed by gas chromatography using the above-mentioned free fatty acid type column (FFAP).

(アスファルト再生添加剤)
上記の鉱油と油脂を所定の重量比で混合し、60℃下で15分攪拌混合し均一なアスファルト再生添加剤組成物:添加剤1〜11を得た。混合比率、混合後の性状を表3に示す。
比較例4(添加剤11)のPCA含有量は20.5質量%と非常に高く、3質量%を超えているため環境および人体に対する負荷が高く、安全性が懸念されるものであることが分かる。
なお、表3に示したアスファルト再生添加剤組成物の性状は下記の方法にて分析した。
密度(15℃)はJIS K2249「原油及び石油製品−密度試験方法」により測定される15℃における密度(g/cm)を指す。
引火点(COC)はJIS K2265「原油及び石油製品−引火点試験方法」のクリーブランド開放式引火点試験方法により測定される引火点(℃)を指す。
動粘度(40℃、60℃、100℃)はJIS K2283「原油及び石油製品−動粘度試験方法及び粘度指数算出方法」により測定される40℃、60℃、100℃における動粘度(mm/s)を指す。
薄膜加熱試験後の質量変化率はJIS K2207「石油アスファルト−薄膜加熱試験法」により測定される薄膜加熱質量変化率(質量%)を指し、正の値は質量の増量を、負の値は質量の減量を意味する。
薄膜加熱試験後の動粘度比(60℃)はJIS K2207「石油アスファルト−薄膜加熱試験法」に準拠して試験を行った後の試料の60℃における動粘度を、試験前の試料の60℃における動粘度にて除した値を指す。
PCA含有量は”The Institute of Petroleum”のIP346/92 ”Determination of polycyclic aromatics in unused lubricating base oils and asphaltene free petroleum fractions - Dimethyl sulphoxide extraction refractive index method”の方法に準拠して得られる多環芳香族炭化水素化合物の含有量(質量%)のことを指す。
(Asphalt regeneration additive)
Said mineral oil and fats and oils were mixed by predetermined weight ratio, and it stirred and mixed under 60 degreeC for 15 minutes, and obtained uniform asphalt reproduction | regeneration additive composition: Additives 1-11. Table 3 shows the mixing ratio and the properties after mixing.
The PCA content of Comparative Example 4 (Additive 11) is very high at 20.5% by mass, and exceeds 3% by mass. Therefore, the load on the environment and the human body is high, and safety may be a concern. I understand.
The properties of the asphalt regeneration additive composition shown in Table 3 were analyzed by the following method.
The density (15 ° C.) refers to the density (g / cm 3 ) at 15 ° C. measured by JIS K2249 “Crude oil and petroleum products—Density test method”.
The flash point (COC) refers to the flash point (° C.) measured by the Cleveland open-type flash point test method of JIS K2265 “Crude oil and petroleum products—flash point test method”.
Kinematic viscosity (40 ℃, 60 ℃, 100 ℃) is JIS K2283 - 40 ° C. as measured by the "Crude petroleum and petroleum products kinematic viscosity and calculation of viscosity index", 60 ° C., a kinematic viscosity at 100 ℃ (mm 2 / s).
The mass change rate after the thin film heating test refers to the thin film heating mass change rate (% by mass) measured by JIS K2207 “Petroleum Asphalt-Thin Film Heating Test Method”. A positive value indicates an increase in mass and a negative value indicates a mass. Means weight loss.
The kinematic viscosity ratio (60 ° C.) after the thin film heating test is the kinematic viscosity at 60 ° C. of the sample after testing in accordance with JIS K2207 “Petroleum Asphalt—Thin Film Heating Test Method”. The value divided by the kinematic viscosity at
PCA content is polycyclic aromatic carbonization obtained in accordance with “The Institute of Petroleum” IP346 / 92 “Determination of polycyclic aromatics in unused lubricating base oils and asphaltene free petroleum fractions-Dimethyl sulphoxide extraction refractive index method” It refers to the content (% by mass) of the hydrogen compound.

(劣化アスファルト)
針入度70のストレートアスファルトを薄膜加熱試験にて163℃、5時間試験した後、
さらに米国SHRPが提案する加圧促進劣化試験により劣化アスファルトを得た。すなわち温度100℃、空気圧2.07MPaの条件下で20時間試験を行い、劣化アスファルトを得た。劣化アスファルトの性状を表4に示す。
針入度(25℃)はJIS K2207「石油アスファルト−針入度試験方法」により測定される針入度を指す。
軟化点はJIS K2207「石油アスファルト−軟化点試験方法」により測定される軟化点(℃)を指す。
伸度(15℃)はJIS K2207「石油アスファルト−伸度試験方法」により測定される15℃における伸度を指す。
(Deteriorated asphalt)
After testing straight asphalt with a penetration of 70 in a thin film heating test at 163 ° C. for 5 hours,
Furthermore, deteriorated asphalt was obtained by the pressure accelerated deterioration test proposed by US SHRP. That is, the test was conducted for 20 hours under the conditions of a temperature of 100 ° C. and an air pressure of 2.07 MPa to obtain deteriorated asphalt. Table 4 shows the properties of the deteriorated asphalt.
The penetration (25 ° C.) refers to the penetration measured according to JIS K2207 “Petroleum Asphalt—Penetration Test Method”.
The softening point refers to a softening point (° C.) measured according to JIS K2207 “Petroleum Asphalt—Softening Point Test Method”.
Elongation (15 ° C.) refers to the elongation at 15 ° C. measured by JIS K2207 “Petroleum Asphalt—Elongation Test Method”.

(実施例1〜7、比較例1〜3)
加熱溶融状態の劣化アスファルトに目標針入度70となるように添加剤1〜10を添加、攪拌し再生を行った。得られた再生アスファルトの物性を測定し、その再生効果を確認した。再生アスファルトの性状を表5に示す。再生アスファルトの性状は下記の方法にて分析を行った。なお、表5に記載のない引火点(COC)、トルエン可溶分、蒸発試験後の針入度比は、いずれも表6に示す日本道路協会の定める道路舗装用ストレートアスファルトの規格を満足するものであった。
密度はJIS K2207「石油アスファルト−密度試験方法」により測定される15℃に換算した密度(g/cm3)を指す。
針入度(25℃)はJIS K2207「石油アスファルト−針入度試験方法」により測定される針入度を指す。
軟化点はJIS K2207「石油アスファルト−軟化点試験方法」により測定される軟化点(℃)を指す。
伸度(15℃)はJIS K2207「石油アスファルト−伸度試験方法」により測定される15℃における伸度を指す。
薄膜加熱試験後の針入度残留率はJIS K2207「石油アスファルト−薄膜加熱試験方法」により測定される薄膜加熱後の針入度の原針入度に対する百分率(%)を指す。
薄膜加熱質量変化率はJIS K2207「石油アスファルト−薄膜加熱試験法」により測定される薄膜加熱質量変化率(質量%)を指し、正の値は質量の増量を、負の値は質量の減量を意味する。
(Examples 1-7, Comparative Examples 1-3)
Additives 1 to 10 were added to the deteriorated asphalt in a heated and melted state so as to achieve a target penetration of 70, followed by regeneration by stirring. The physical properties of the obtained recycled asphalt were measured, and the regeneration effect was confirmed. Table 5 shows the properties of the recycled asphalt. The properties of recycled asphalt were analyzed by the following method. Note that the flash point (COC), toluene soluble content, and penetration ratio after the evaporation test not listed in Table 5 all satisfy the standards of straight asphalt for road paving established by the Japan Road Association shown in Table 6. It was a thing.
The density refers to the density (g / cm 3 ) converted to 15 ° C. measured by JIS K2207 “Petroleum Asphalt—Density Test Method”.
The penetration (25 ° C.) refers to the penetration measured according to JIS K2207 “Petroleum Asphalt—Penetration Test Method”.
The softening point refers to a softening point (° C.) measured according to JIS K2207 “Petroleum Asphalt—Softening Point Test Method”.
The elongation (15 ° C.) refers to the elongation at 15 ° C. measured by JIS K2207 “Petroleum Asphalt—Elongation Test Method”.
The penetration residual rate after the thin film heating test refers to the percentage (%) of the penetration after the thin film heating measured by JIS K2207 “Petroleum Asphalt—Thin Film Heating Test Method” with respect to the original penetration.
Thin film heating mass change rate refers to thin film heating mass change rate (% by mass) measured by JIS K2207 “Petroleum Asphalt-Thin Film Heating Test Method”. Positive value indicates mass increase, negative value indicates mass decrease. means.

実施例1〜7の再生後のアスファルト性状は、いずれも表6に示す日本道路協会の定める道路舗装用ストレートアスファルトの規格を満足するものであった。
比較例1の添加剤9は油脂を含有しないため、再生後のアスファルトの伸度が50cmと小さく、日本道路協会の定める道路舗装用ストレートアスファルトの規格を満足する試料に再生できなかった。
比較例2、3は加熱溶融状態の劣化アスファルトに目標針入度70となるように添加剤9、10を添加、攪拌し再生を行った。添加剤9、10は油脂(グリセライド化合物)を必要以上に配合しているため、再生時の必要添加量が極めて少なく、添加剤が劣化アスファルト全体に行き渡らず不均一な再生しかできなかった。そのため再生試料の針入度の値は非常にばらつきの多い結果となった。
The asphalt properties after regeneration in Examples 1 to 7 all satisfied the standards of straight asphalt for road paving established by the Japan Road Association shown in Table 6.
Since additive 9 of Comparative Example 1 does not contain fats and oils, the asphalt elongation after regeneration was as small as 50 cm, and could not be regenerated into a sample that satisfied the standard of road asphalt straight asphalt established by the Japan Road Association.
In Comparative Examples 2 and 3, Additives 9 and 10 were added to the deteriorated asphalt in the heat-melted state so that the target penetration was 70, and the mixture was stirred and regenerated. Since Additives 9 and 10 contain fats and oils (glyceride compound) more than necessary, the amount of addition required during regeneration is extremely small, and the additive does not reach the entire deteriorated asphalt and only non-uniform regeneration is possible. As a result, the penetration values of the regenerated samples varied greatly.

Figure 0004257186
Figure 0004257186

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Claims (5)

40℃における動粘度が300〜900mm/s、多環芳香族分(PCA)が3質量%未満である鉱油と油脂を配合して得られる組成物であって、40℃における動粘度が40〜400mm/s、多環芳香族分(PCA)が3質量%未満、引火点が220℃以上であることを特徴としたアスファルト再生添加剤組成物。 A kinematic viscosity at 40 ° C. is 300 to 900 mm 2 / s, and a polycyclic aromatic component (PCA) is a composition obtained by blending mineral oil and fat with less than 3% by mass, and the kinematic viscosity at 40 ° C. is 40 ~400mm 2 / s, polycyclic aromatic components (PCA) is less than 3 wt%, asphalt regeneration additive composition flash point is characterized in that at 220 ° C. or higher. 鉱油と油脂の配合割合が、鉱油10〜90質量%、油脂90〜10質量%(合計100質量%)であることを特徴とする請求項1記載のアスファルト再生添加剤組成物。   The asphalt regeneration additive composition according to claim 1, wherein the blending ratio of mineral oil and fat is 10 to 90% by weight of mineral oil and 90 to 10% by weight (total 100% by weight) of fat and oil. 油脂の脂肪酸部分が炭素数3から18である飽和脂肪酸、不飽和脂肪酸、又はこれらの混合物であることを特徴とする請求項1または記載のアスファルト再生添加剤組成物。 The asphalt regeneration additive composition according to claim 1 or 2 , wherein the fatty acid portion of the fat is a saturated fatty acid having 3 to 18 carbon atoms, an unsaturated fatty acid, or a mixture thereof. 油脂が動物油脂又は植物油脂であることを特徴とする請求項1〜3のいずれか一項に記載のアスファルト再生添加剤組成物。 The asphalt regeneration additive composition according to any one of claims 1 to 3 , wherein the fat is animal fat or vegetable fat. 油脂が動物油脂又は植物油脂の廃油脂であることを特徴とする請求項1〜3のいずれか一項に記載のアスファルト再生添加剤組成物。 The asphalt regeneration additive composition according to any one of claims 1 to 3 , wherein the fat is animal fat or vegetable waste oil.
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