JP5744766B2 - Reclaimed asphalt reclaim additive composition and reclaimed asphalt pavement material - Google Patents

Reclaimed asphalt reclaim additive composition and reclaimed asphalt pavement material Download PDF

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JP5744766B2
JP5744766B2 JP2012018703A JP2012018703A JP5744766B2 JP 5744766 B2 JP5744766 B2 JP 5744766B2 JP 2012018703 A JP2012018703 A JP 2012018703A JP 2012018703 A JP2012018703 A JP 2012018703A JP 5744766 B2 JP5744766 B2 JP 5744766B2
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好和 中村
好和 中村
理 田村
理 田村
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Eneos 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。詳しくは多環芳香族炭化水素(PCA)の含有量が低く、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ものである。   The present invention relates to a paving asphalt regeneration additive. Specifically, the content of polycyclic aromatic hydrocarbons (PCA) is low, the safety to the environment and the human body is excellent, and the deteriorated asphalt contained in the pavement waste material is restored to the initial softness, that is, the penetration is reduced. The present invention relates to an asphalt regeneration additive composition having an excellent ability to restore elongation.

舗装廃材の再生方法は、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再生合材を製造する時、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。   As for the recycling method of paving waste material, when the recycled material is manufactured by mixing the three members of paving waste material, new aggregate, and new asphalt with the mixer of the asphalt compound factory, the asphalt cured by the deterioration contained in the paving waste material. Asphalt regeneration additives are added to restore the initial penetration and elongation to the initial softness. 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.

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結果、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、その芳香族性を規定したアスファルト再生添加剤組成物が公知となっている(例えば、特許文献1,2参照)。
ところが、芳香族性の高い鉱油には多量の多環芳香族炭化水素(PCA:Polycyclic Aromatics)が含まれているため、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の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。
Such a highly aromatic mineral oil has a high ability to recover the penetration and elongation greatly reduced by deterioration as a result of supplementing the aromatic component in the deteriorated asphalt. In particular, in order to greatly recover the elongation, the added mineral oil is required to have high aromaticity, and an asphalt regeneration additive composition that defines the aromaticity is known (for example, Patent Document 1, Patent Document 1). 2).
However, mineral oils with high aromaticity contain a large amount of polycyclic aromatic hydrocarbons (PCA), so there is a heavy burden on the environment and the human body. Currently, asphalt is highly safe for the environment and the human body. There is a growing demand for the development of regenerative additives.

さらに近年、舗装廃材中の劣化したアスファルトの性状が従来以上に劣化程度が増す傾向にあること、また再生合材中への舗装廃材の配合割合が増す傾向にあること、さらに1回のみの再生にとどまらず、すでに複数回再生を受けた舗装廃材が配合されているケースが生じていることなど、舗装廃材の再生は従来以上に高い再生能力、とりわけ繰り返し再生後のアスファルトの伸度を初期なみに回復させるアスファルト再生添加剤の開発が望まれている。一方、高芳香族系鉱油に含まれる多環芳香族炭化水素(PCA)の有害性が問題となっていることから、PCAの含有量を削減することが必要となっている。また、舗装廃材中の劣化したアスファルトの伸度を十分に回復せず施工した舗装体は、一般にひび割れが生じる懸念があるため、針入度、伸度の回復は重要である。   Furthermore, in recent years, the properties of degraded asphalt in pavement waste materials tend to be more deteriorated than before, and the proportion of pavement waste materials in recycled composite materials tends to increase. In addition, there are cases where paving waste materials that have been regenerated multiple times have already been blended, and the regeneration of paving waste materials has a higher regeneration capacity than before, especially the asphalt elongation after repeated regeneration. Development of an asphalt regeneration additive that can be restored to a high level is desired. On the other hand, since the harmfulness of polycyclic aromatic hydrocarbons (PCA) contained in highly aromatic mineral oil is a problem, it is necessary to reduce the content of PCA. Moreover, since the pavement constructed without fully recovering the elongation of the deteriorated asphalt in the pavement waste generally has a risk of cracking, recovery of the penetration and elongation is important.

特開平02−091303号公報Japanese Patent Laid-Open No. 02-091303 特開平08−333515号公報Japanese Patent Application Laid-Open No. 08-333515

そのため、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。   Therefore, asphalt regeneration addition that is excellent in safety to the environment and the human body, and repeatedly recovers asphalt hardened due to deterioration contained in paving waste materials to the initial softness, that is, it repeatedly recovers greatly reduced penetration and elongation There is a need for agents.

本発明者らは、前記課題について鋭意研究を重ねた結果、2種以上の鉱油を配合することにより、多環芳香族炭化水素(PCA)の含有量が一定量以下であり、動粘度、ガスクロ蒸留で求める5容量%留出温度、引火点、芳香族分(%CA)が一定の範囲内になるように調整した鉱油が、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 blended two or more mineral oils so that the polycyclic aromatic hydrocarbon (PCA) content is not more than a certain amount, and kinematic viscosity, gas chromatography Mineral oil adjusted so that 5 vol% distillation temperature, flash point, and aromatic content (% CA) determined by distillation are within a certain range is highly safe for the environment and human body, and deteriorated asphalt in pavement waste As a result, the present inventors have found that the needle penetration and elongation can be remarkably recovered repeatedly and have completed the present invention.

すなわち本発明は、(A)減圧蒸留残油を極性溶剤で抽出し40℃における動粘度が2000〜2500mm /s、多環芳香族炭化水素含有量が3質量%未満に調整したエキストラクトを50〜90質量%および(B)40℃における動粘度が80〜180mm /sの潤滑油基油を10〜50質量%配合して製造される、多環芳香族炭化水素(PCA)含有量が3質量%未満、40℃における動粘度が900〜1500mm/s、ガスクロ蒸留による5容量%留出温度が350℃以上、引火点が260℃以上、および芳香族分(%CA)が10〜25%であることを特徴とするアスファルト再生添加剤組成物に関する。 That is, the present invention provides (A) an extract obtained by extracting a vacuum distillation residue with a polar solvent and adjusting the kinematic viscosity at 40 ° C. to 2000 to 2500 mm 2 / s and the polycyclic aromatic hydrocarbon content to less than 3% by mass. Polycyclic aromatic hydrocarbon (PCA) content produced by blending 50 to 90% by mass and (B) 10 to 50% by mass of a lubricating base oil having a kinematic viscosity at 40 ° C. of 80 to 180 mm 2 / s Is less than 3% by mass, the kinematic viscosity at 40 ° C. is 900-1500 mm 2 / s, the 5% by volume distillation temperature by gas chromatography is 350 ° C. or higher, the flash point is 260 ° C. or higher, and the aromatic content (% CA) is 10 It is related with the asphalt regeneration additive composition characterized by being -25%.

また本発明は、前記記載のアスファルト再生添加剤組成物を、劣化アスファルト100重量部に対して4〜30重量部の割合で配合してなることを特徴とする再生アスファルト舗装材に関する。   The present invention also relates to a reclaimed asphalt pavement characterized in that the asphalt regenerating additive composition described above is blended at a ratio of 4 to 30 parts by weight with respect to 100 parts by weight of deteriorated asphalt.

さらに本発明は、(A)減圧蒸留残油を極性溶剤で抽出し40℃における動粘度が2000〜2500mm /s、多環芳香族炭化水素含有量が3質量%未満に調整したエキストラクトを50〜90質量%および(B)40℃における動粘度が80〜180mm /sの潤滑油基油を10〜50質量%配合することにより、多環芳香族炭化水素(PCA)含有量が3質量%未満、40℃における動粘度が900〜1500mm/s、ガスクロ蒸留による5容量%留出温度が350℃以上、引火点が260℃以上、および芳香族分(%CA)が10〜25%であるアスファルト再生添加剤組成物を得ることを特徴とするアスファルト再生添加剤組成物の製造方法に関する。
Furthermore, the present invention provides (A) an extract obtained by extracting a vacuum distillation residue with a polar solvent and adjusting the kinematic viscosity at 40 ° C. to 2000 to 2500 mm 2 / s and the polycyclic aromatic hydrocarbon content to less than 3% by mass. 50-90 mass% and (B) Polycyclic aromatic hydrocarbon (PCA) content is 3 by mix | blending 10-50 mass% of lubricant base oil whose dynamic viscosity in 40 degreeC is 80-180 mm < 2 > / s. Less than mass%, kinematic viscosity at 40 ° C. is 900-1500 mm 2 / s, 5% by volume distillation temperature by gas chromatography is 350 ° C. or more, flash point is 260 ° C. or more, and aromatic content (% CA) is 10-25 % Asphalt regeneration additive composition, characterized in that the asphalt regeneration additive composition is obtained.

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 greatly recovered. Can be made.

以下、本発明について詳述する。
本発明のアスファルト再生添加剤組成物の多環芳香族炭化水素(PCA)の含有量は、3質量%未満であることが必要である。PCAが3質量%以上であると、環境およ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%以下が好ましく、2.5質量%以下がより好ましく、2.0質量%以下がさらに好ましい。
なお、ここでいう多環芳香族炭化水素とは、“The Institute of Petroleum“のIP346/92“Determination of polycyclic aromatics in unused Lubricating base oil 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。
Hereinafter, the present invention will be described in detail.
The polycyclic aromatic hydrocarbon (PCA) content of the asphalt regeneration additive composition of the present invention needs to be less than 3% by mass. If the PCA is 3% by mass or more, there is a risk of increasing the load on the environment and the human body, which is not preferable. For this reason, PCA is preferably 2.8% by mass or less, more preferably 2.5% by mass or less, and further preferably 2.0% by mass or less.
The polycyclic aromatic hydrocarbon referred to here is the method of “The Institute of Petroleum” IP346 / 92 “Determination of polycyclic aromatics in unused Lubricating base oil and asphaltene free petroleum fractions-Dimethyl sulphoxide extraction refractive index method”. It means the content (% by mass) of the polycyclic aromatic hydrocarbon compound obtained in compliance.

本発明のアスファルト再生添加剤組成物の40℃における動粘度は、900〜1500mm/sであることが必要である。40℃における動粘度が900mm/sに満たない場合は、再生アスファルトの伸度の回復が十分望めない。一方、40℃における動粘度が1500mm/sを超える場合は、流動性が低下してハンドリング性が極度に悪くなるとともに、針入度、伸度を回復させるために多量のアスファルト再生添加剤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950mm/s以上が好ましく、1000mm/s以上がより好ましい。また、上限は1450mm/s以下が好ましく、1400mm/s以下がより好ましく、1300mm/s以下がさらに好ましい。
なお、ここでいう動粘度(40℃)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40℃における動粘度を意味する。
The kinematic viscosity at 40 ° C. of the asphalt regeneration additive composition of the present invention needs to be 900 to 1500 mm 2 / s. When the kinematic viscosity at 40 ° C. is less than 900 mm 2 / s, it is not possible to sufficiently recover the elongation of the regenerated asphalt. On the other hand, when the kinematic viscosity at 40 ° C. exceeds 1500 mm 2 / s, the fluidity is lowered, the handling property is extremely deteriorated, and a large amount of asphalt regeneration additive is used to recover the penetration and elongation. This is not preferable because it is necessary. For this reason, the lower limit of the kinematic viscosity at 40 ° C. is preferably 950 mm 2 / s or more, and more preferably 1000 mm 2 / s or more. The upper limit is preferably 1450 mm 2 / s or less, more preferably 1400 mm 2 / s or less, and still more preferably 1300 mm 2 / s or less.
In addition, kinematic viscosity (40 degreeC) here means the kinematic viscosity in 40 degreeC measured by JISK2283 "Crude oil and petroleum products-kinematic viscosity test method and viscosity index calculation method".

本発明のアスファルト再生添加剤組成物のガスクロ蒸留による5容量%留出温度は、350℃以上であることが必要である。ガスクロ蒸留による5容量%留出温度が350℃未満であると、再生アスファルトの伸度の回復が十分望めない。かかる理由からガスクロ蒸留による5容量%留出温度は360℃以上が好ましく、370℃以上がより好ましい。
なお、ここでいう5容量%留出温度は、JIS K2254「石油製品-蒸留試験方法」のガスクロマトグラフ法蒸留試験方法により測定される5容量%留出温度を意味する。
The 5 vol% distillation temperature of the asphalt regeneration additive composition of the present invention by gas chromatography must be 350 ° C or higher. If the 5% by volume distillation temperature by gas chromatography is less than 350 ° C., it is not possible to sufficiently recover the elongation of the regenerated asphalt. For this reason, the 5 vol% distillation temperature by gas chromatography is preferably 360 ° C. or higher, and more preferably 370 ° C. or higher.
The 5 vol% distillation temperature mentioned here means the 5 vol% distillation temperature measured by the gas chromatographic distillation test method of JIS K2254 “Petroleum products-distillation test method”.

本発明のアスファルト再生添加剤組成物の引火点は、260℃以上であることが必要である。引火点が260℃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270℃以上が好ましく、280℃以上がより好ましい。
なお、ここでいう引火点(COC)はJIS K2265「引火点の求め方−第4部:クリーブランド開放法」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 the asphalt regeneration additive composition of the present invention needs to be 260 ° C. or higher. A flash point of less than 260 ° C. is not preferable because safety during production of the asphalt pavement mixture is lowered. For this reason, the flash point is preferably 270 ° C. or higher, and more preferably 280 ° C. or higher.
The flash point (COC) here means the flash point (° C.) measured by the Cleveland open type flash point test method of JIS K2265 “How to find the flash point—Part 4: Cleveland open method”.

本発明のアスファルト再生添加剤組成物の芳香族分(%CA)は10%以上25%以下であることが必要である。%CAが25%を超えると再生添加剤のPCAが3質量%以上になる可能性があり、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20%以下が好ましく、18%以下がより好ましい。一方、%CAが10%未満であると、劣化アスファルトを再生した時の再生アスファルトの伸度が回復しにくくなるため好ましくない。
なお、ここでいう芳香族分(%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。
The aromatic content (% CA) of the asphalt regeneration additive composition of the present invention needs to be 10% or more and 25% or less. If% CA exceeds 25%, the PCA of the regenerative additive may be 3% by mass or more, which is not preferable because the load on the environment and the human body increases. For this reason, 20% or less is preferable, and 18% or less is more preferable. On the other hand, if% CA is less than 10%, it is not preferable because the elongation of the regenerated asphalt is difficult to recover when the deteriorated asphalt is regenerated.
The aromatic content (% CA) here refers to the aromatic ring carbon relative to the total number of carbon atoms measured by ASTM D3238 “Standard Test Method for Calculation of Carbon Distribution and Structural Group Analysis of Petroleum Oils by the ndM Method”. It means the percentage (%) of the number.

本発明のアスファルト再生添加剤組成物の15℃における密度は、0.900〜0.970g/cmであることが好ましい。再生添加剤組成物の15℃における密度が0.900g/cm未満である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。したがって、密度の下限は0.910g/cm以上がより好ましい。一方、密度の上限は0.970g/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0.960g/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−密度試験方法及び密度・質量・容量換算表」により測定される15℃における密度(g/cm)を意味する。
The density at 15 ° C. of the asphalt regeneration additive composition of the present invention is preferably 0.900 to 0.970 g / cm 3 . If the density of the regenerated additive composition at 15 ° C. is less than 0.900 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 0.910 g / cm 3 or more. On the other hand, if the upper limit of the density exceeds 0.970 g / cm 3 , the ratio of the aromatic component is high, the PCA may be 3% by mass or more, and the load on the environment and the human body is increased. For this reason, 0.960 g / cm 3 or less is more preferable.
The density here means a density (g / cm 3 ) at 15 ° C. measured by JIS K2249 “Crude oil and petroleum products—Density test method and density / mass / capacity conversion table”.

本発明のアスファルト再生添加剤組成物は、多環芳香族炭化水素(PCA)、動粘度、ガスクロ蒸留による5容量%留出温度、引火点、芳香族分(%CA)が上述の範囲を満たすように、2種以上の鉱油を配合して製造される。   In the asphalt regeneration additive composition of the present invention, polycyclic aromatic hydrocarbon (PCA), kinematic viscosity, 5% by volume distillation temperature by gas chromatography, flash point, aromatic content (% CA) satisfy the above-mentioned ranges. Thus, it manufactures by mix | blending 2 or more types of mineral oil.

本発明のアスファルト再生添加剤組成物に使用される鉱油を製造する際に用いられ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ア原油、ミナス原油、大慶原油等パラフィン基原油、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、クウェート原油、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く用いられる。   The crude oil used in producing the mineral oil used in the asphalt regeneration additive composition of the present invention is not particularly limited, and examples thereof include paraffin base crude oil such as Pennsylvania crude oil, Minas crude oil, Daqing crude oil, California crude oil, Texas Crude oil, naphthenic crude oil such as Venezuela 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, Lataway crude oil, Allian crude oil, Eosin crude oil, Solish crude oil, etc. A mixed base crude oil or the like is preferably used.

本発明のアスファルト再生添加剤組成物に使用される鉱油は、特に限定されものではないが、上述の原油を常圧蒸留して得られる常圧残油を減圧蒸留し、得られた留分を使用することが好ましい。減圧蒸留工程から得られた留分は、プロパン脱れき等で代表される溶剤脱れき、フルフラール抽出等で代表される溶剤抽出、MEK(メチルエチルケトン)を用いてろう分を除去するMEK脱ろう等で代表される溶剤脱ろう、水素化分解脱ろう、接触脱ろう、水素化精製、硫酸洗浄、白土処理等の処理を適宜組み合わせて精製されることが好ましい。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取り除くフルフラール抽出により得られるラフィネート(潤滑油基油)及びそのラフィネートをさらに水素化精製・MEK脱ろう等を組み合わせて処理して得られる精製ラフィネート(潤滑油基油)、減圧蒸留残油から潤滑油留分を抽出することを目的として行うプロパン脱れきにより得られるPDAエキストラクト、PDAエキストラクトをフルフラール抽出して得られるPDAフルフラールエキストラクト、PDAエキストラクトをフルフラール抽出して得られたPDAフルフラールラフィネートを、MEK脱ろう・水素化精製等を組み合わせて処理して得られる高粘度高級潤滑油成分(ブライトストック:潤滑油基油)などが好適に用いられる。   The mineral oil used in the asphalt regeneration additive composition of the present invention is not particularly limited, but the atmospheric residue obtained by atmospheric distillation of the crude oil described above is distilled under reduced pressure, and the resulting fraction is It is preferable to use it. The fraction obtained from the reduced-pressure distillation step is obtained by solvent removal such as propane removal, solvent extraction represented by furfural extraction, MEK dewaxing, etc., which removes wax using MEK (methyl ethyl ketone). It is preferable to purify by appropriately combining treatments such as solvent dewaxing, hydrocracking dewaxing, catalytic dewaxing, hydrorefining, sulfuric acid washing and clay treatment. In particular, a lubricating oil fraction obtained by distilling crude oil under reduced pressure, a raffinate (lubricating oil base oil) obtained by furfural extraction that removes aromatic compounds and resins in the lubricating oil fraction using furfural, and its raffinate are further added. PDA extra obtained by propane deburring for the purpose of extracting a lubricating oil fraction from a refined raffinate (lubricating base oil) obtained by combining hydrorefining and MEK dewaxing, etc. , PDA furfural extract obtained by furfural extraction of PDA extract, PDA furfural raffinate obtained by furfural extraction of PDA extract, combined with MEK dewaxing, hydrorefining, etc. Viscosity high-grade lubricating oil component (bright stock: lubricating base oil) It is preferably used.

本発明のアスファルト再生添加剤組成物は、上記した鉱油の中から任意の2種以上を配合して製造することできるが、(A)減圧蒸留残油をフルフラール等の極性溶剤で抽出して多環芳香族炭化水素含有量が3質量%未満に調整したエキストラクトおよび(B)潤滑油基油を使用することが好ましい。この場合、(A)を50〜90質量%、(B)を10〜50質量%の割合で配合することが好ましく、より好ましくは(A)を60〜80質量%、(B)を20〜40質量%である。なお、(B)成分の潤滑油基油としては、減圧蒸留残油から潤滑油留分を抽出することを目的として行うプロパン脱れきにより得られるPDAエキストラクトをフルフラール抽出して得られたPDAフルフラールラフィネートを、MEK脱ろう・水素化精製等を組み合わせて処理して得られる高粘度高級潤滑油成分(ブライトストック)が好ましい。   The asphalt regeneration additive composition of the present invention can be produced by blending any two or more of the above-mentioned mineral oils. (A) A vacuum distillation residue is extracted with a polar solvent such as furfural. It is preferable to use an extract having a ring aromatic hydrocarbon content adjusted to less than 3% by mass and (B) a lubricating base oil. In this case, it is preferable to blend (A) in a proportion of 50 to 90% by mass and (B) in a proportion of 10 to 50% by mass, more preferably 60 to 80% by mass of (A) and 20 to 20% of (B). 40% by mass. In addition, as the lubricating base oil of component (B), PDA furfural obtained by furfural extraction of PDA extract obtained by propane deburring for the purpose of extracting a lubricating oil fraction from vacuum distillation residue A high-viscosity high-grade lubricating oil component (bright stock) obtained by treating raffinate with a combination of MEK dewaxing and hydrorefining is preferred.

本発明のアスファルト再生添加剤組成物に使用する鉱油の性状は、最終製品である再生添加剤組成物の動粘度、多環芳香族炭化水素(PCA)、引火点、芳香族分(%CA)、ガスクロ蒸留による5容量%留出温度が上述の範囲内にあれば特に限定されるものではないが、以下の性状を有することが好ましい。   The properties of the mineral oil used in the asphalt regeneration additive composition of the present invention are the kinematic viscosity, polycyclic aromatic hydrocarbon (PCA), flash point, aromatic content (% CA) of the regeneration additive composition as the final product. The 5 vol% distillation temperature by gas chromatography is not particularly limited as long as it is within the above range, but preferably has the following properties.

本発明のアスファルト再生添加剤組成物に使用する鉱油の40℃における動粘度は、80〜2500mm/sであることが好ましい。なお、最終製品である再生添加剤組成物の40℃における動粘度が900〜1500mm/sの範囲内にあれば、特に限定されるものではない。
ただし、最終製品である再生添加剤組成物の40℃における動粘度が1500mm/sを超える場合は、流動性が低下してハンドリング性が極度に悪くなるとともに、針入度、伸度を回復させるために多量のアスファルト再生添加剤が必要となることから好ましくない。かかる理由から、2種の鉱油を配合する場合には、一方の鉱油の40℃における動粘度の下限は900mm/s以上が好ましく、950mm/s以上がより好ましい。また、上限は1500mm/s以下が好ましく、1400mm/s以下がより好ましく、1300mm/s以下がさらに好ましい。また、他方の鉱油の40℃における動粘度の下限は80mm/s以上が好ましく、90mm/s以上がより好ましい。また、上限は200mm/s以下が好ましく、180mm/s以下がより好ましい。
It is preferable that the kinematic viscosity at 40 ° C. of the mineral oil used in the asphalt regeneration additive composition of the present invention is 80 to 2500 mm 2 / s. In addition, if the kinematic viscosity in 40 degreeC of the reproduction | regeneration additive composition which is a final product exists in the range of 900-1500 mm < 2 > / s, it will not specifically limit.
However, when the regenerative additive composition as the final product has a kinematic viscosity at 40 ° C. exceeding 1500 mm 2 / s, the fluidity is lowered and the handling property is extremely deteriorated, and the penetration and elongation are recovered. Therefore, a large amount of an asphalt regeneration additive is required for the purpose. For this reason, when two mineral oils are blended, the lower limit of the kinematic viscosity at 40 ° C. of one mineral oil is preferably 900 mm 2 / s or more, and more preferably 950 mm 2 / s or more. The upper limit is preferably 1500 mm 2 / s or less, more preferably 1400 mm 2 / s or less, and still more preferably 1300 mm 2 / s or less. The lower limit of the kinematic viscosity at 40 ° C. of the other mineral oil is preferably 80 mm 2 / s or more, and more preferably 90 mm 2 / s or more. The upper limit is preferably at most 200mm 2 / s, 180mm 2 / s or less is more preferable.

本発明のアスファルト再生添加剤組成物に使用する鉱油の多環芳香族炭化水素(PCA)の含有量は、3質量%未満であることが好ましい。鉱油中のPCAが3質量%以上であると、環境およ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%以下がより好ましく、2.5質量%以下がさらに好ましい。
鉱油の引火点は260℃以上であることが好ましい。鉱油の引火点が260℃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270℃以上がより好ましく、280℃以上がより好ましい。
鉱油の芳香族分(%CA)は10%以上28%以下であることが好ましい。%CAが28%を超えると再生添加剤のPCAが3質量%以上になる可能性があり、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、芳香族分(%CA)は25%以下がより好ましく、20%以下がさらに好ましい。
鉱油のガスクロ蒸留による5容量%留出温度は350℃以上であることが好ましい。ガスクロ蒸留による5容量%留出温度350℃未満であると、再生アスファルトの伸度の回復が十分望めない。かかる理由から、ガスクロ蒸留による5容量%留出温度は350℃以上がより好ましく、360℃以上がさらに好ましく、370℃以上が特に好ましい。
The content of polycyclic aromatic hydrocarbon (PCA) in the mineral oil used in the asphalt regeneration additive composition of the present invention is preferably 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 more preferably 2.8% by mass or less, and further preferably 2.5% by mass or less.
The flash point of the mineral oil is preferably 260 ° C. or higher. When the flash point of mineral oil is less than 260 ° C., the safety during production of the asphalt pavement mixture is lowered, which is not preferable. For this reason, the flash point is more preferably 270 ° C. or higher, and more preferably 280 ° C. or higher.
The aromatic content (% CA) of the mineral oil is preferably 10% or more and 28% or less. If% CA exceeds 28%, the PCA of the regenerative additive may be 3% by mass or more, which increases the load on the environment and the human body, which is not preferable. For this reason, the aromatic content (% CA) is more preferably 25% or less, and further preferably 20% or less.
The 5 vol% distillation temperature of mineral oil by gas chromatography is preferably 350 ° C or higher. If the 5 vol% distillation temperature by gas chromatography is less than 350 ° C., it is not possible to sufficiently recover the elongation of the regenerated asphalt. For this reason, the 5 vol% distillation temperature by gas chromatography is more preferably 350 ° C. or higher, more preferably 360 ° C. or higher, and particularly preferably 370 ° C. or higher.

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、リミクッス方式においては加熱、かきほぐし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。
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重量部に対して4〜30重量部であることが好ましい。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超えてしまう。かかる理由からより好ましい添加量は5〜25重量部、さらに好ましくは6〜20重量部である。
The 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 remixing method, the asphalt regeneration additive of the present invention is added to the existing surface layer mixture that has been heated and loosened, and the mixture is stirred and laid, and then the new asphalt mixture is laid on top and simultaneously compacted. Can do.
The amount of the asphalt regeneration additive composition of the present invention added to the paving waste is an amount necessary to recover the penetration and elongation of the deteriorated asphalt in the paving waste to a desired value. It is preferable that it is 4-30 weight part with respect to 100 weight part of inside asphalt deteriorated. 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 the penetration particularly exceeds a desired value. For this reason, the amount added is more preferably 5 to 25 parts by weight, still more preferably 6 to 20 parts by weight.

以下、実施例によりこの発明の内容を更に具体的に説明するが、本発明はこれら実施例に何ら限定されるものではない。   Hereinafter, the content of the present invention will be described more specifically with reference to examples. However, the present invention is not limited to these examples.

[実施例および比較例]
下記により得られた鉱油Aおよび鉱油Bを用いて、アスファルト再生添加剤組成物1〜6を製造した。
鉱油Aは、混合基原油を常圧蒸留して得られた残油を減圧蒸留処理し、その減圧蒸留残油をプロパン脱れきして芳香族含有量の多い脱瀝油(DAO:De-Asphalted Oil)を得る。このようにして得られた沸点530℃以下のDAOをさらにPCAを選択的に分離する条件でフルフラール抽出処理を行い、PCAが3質量%以下、動粘度(40℃)が2000〜2500mm/s程度のエキストラクトを得、鉱油Aとした。
鉱油Bは、混合基原油を常圧蒸留して得られた残油を減圧蒸留処理し、その減圧蒸留残油をプロパン脱れきして芳香族含有量の多い脱瀝油(DAO:De-Asphalted Oil)を得、得られた沸点530℃以下のDAOをさらにPCAを選択的に分離する条件でフルフラール抽出処理して得られたラフィネートを、水素化精製ならびにMEK脱ろう処理を施し、動粘度(40℃)が100mm/s程度になるように調整した潤滑油基油である。
鉱油A、鉱油Bの性状を表1に示す。
[Examples and Comparative Examples]
Asphalt regeneration additive compositions 1 to 6 were produced using mineral oil A and mineral oil B obtained as follows.
Mineral oil A is obtained by subjecting residual oil obtained by atmospheric distillation of mixed base crude oil to reduced-pressure distillation, and removing the reduced-pressure distillation residual oil from propane to remove deodorized oil (DAO: De-Asphalted Oil with a high aromatic content). ) The thus-obtained DAO having a boiling point of 530 ° C. or lower is further subjected to a furfural extraction treatment under conditions for selectively separating PCA, and PCA is 3% by mass or less, and the kinematic viscosity (40 ° C.) is 2000 to 2500 mm 2 / s. A degree of extract was obtained, which was designated as mineral oil A.
Mineral oil B is obtained by subjecting residual oil obtained by atmospheric distillation of mixed base crude oil to reduced-pressure distillation, and removing the reduced-pressure distillation residual oil from propane to remove deodorized oil (DAO: De-Asphalted Oil with a high aromatic content). The raffinate obtained by subjecting the obtained DAO having a boiling point of 530 ° C. or less to a furfural extraction treatment under the condition for selectively separating PCA was subjected to hydrorefining and MEK dewaxing treatment to obtain a kinematic viscosity (40). C.) is a lubricating base oil adjusted so as to be about 100 mm 2 / s.
Properties of mineral oil A and mineral oil B are shown in Table 1.

なお、本実施例において、鉱油、アスファルト再生添加剤組成物、劣化アスファルトおよび再生アスファルト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−密度試験方法及び密度・質量・容量換算表」により測定される15℃における密度(g/cm)を指す。
引火点は(COC)は、JIS K2265「引火点の求め方−第4部:クリーブランド開放法」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℃、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℃、100℃における動粘度(mm/s)を指す。
PCA(多環芳香族炭化水素)含有量は、“The Institute of Petroleum“のIP346/92“Determination of polycyclic aromatics in unused Lubricating base oil 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。
芳香族分(%CA)は、ASTM D3238“Standard Test Method for Calculation of Carbon Distribution and Structural Group Analysis of Petroleum Oil 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。
ガスクロ蒸留による5容量%留出温度は、JIS K2254「石油製品−蒸留試験方法」のガスクロマトグラフ法蒸留試験方法により測定される5容量%留出温度を意味する。
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。
In this example, the properties of mineral oil, asphalt regeneration additive composition, deteriorated asphalt and regenerated asphalt were analyzed by the following method.
Density (15 ℃) is, JIS K2249 - refers to density at 15 ℃ as measured by "Crude Oil and Petroleum Products Density Test Method and density, mass, volume conversion tables" (g / cm 3).
The flash point (COC) refers to a flash point (° C.) measured by the Cleveland open flash point test method of JIS K2265 “How to find a flash point—Part 4: Cleveland open method”.
A kinematic viscosity (40 degreeC, 100 degreeC) points out the kinematic viscosity (mm < 2 > / s) in 40 degreeC and 100 degreeC measured by JISK2283 "Crude oil and petroleum products-kinematic viscosity test method and viscosity index calculation method."
PCA (polycyclic aromatic hydrocarbon) content conforms to “The Institute of Petroleum” IP346 / 92 “Determination of polycyclic aromatics in unused Lubricating base oil and asphaltene free petroleum fractions-Dimethyl sulphoxide extraction refractive index method” It refers to the content (% by mass) of the polycyclic aromatic hydrocarbon compound obtained in this way.
Aromatics (% CA) is the percentage of aromatic ring carbons as a percentage of total carbons measured by ASTM D3238 “Standard Test Method for Calculation of Carbon Distribution and Structural Group Analysis of Petroleum Oil by the ndM Method”. Point to.
An aniline point refers to the aniline point (° C.) measured according to JIS K2256 “Petroleum products—aniline point and mixed aniline point test method”.
The 5 volume% distillation temperature by gas chromatography means the 5 volume% distillation temperature measured by the gas chromatographic distillation test method of JIS K2254 “Petroleum products-distillation test method”.
The penetration (25 ° C.) refers to the penetration measured by JIS K2207 “Petroleum Asphalt—Penetration Test Method”.
The softening point refers to a softening point measured by 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”.

Figure 0005744766
Figure 0005744766

(アスファルト再生添加剤組成物)
上記の鉱油単独、または鉱油Aと鉱油Bを所定の質量比で混合し、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1〜6を得た。混合比、混合後の性状を表2に示す。
ハンドリング性は、アスファルト再生添加剤組成物を調製した時に評価した。その結果、アスファルト再生添加剤組成物1〜6のうち、1は動粘度が高く、ハンドリング性が悪い。1以外はハンドリング性に問題がなかった。なお、ハンドリング性が良い場合を○、悪い場合を×と記載した。
(Asphalt regeneration additive composition)
The above mineral oil alone or mineral oil A and mineral oil B were mixed at a predetermined mass ratio and stirred and mixed at 60 ° C. for 15 minutes to obtain uniform asphalt regeneration additive compositions 1 to 6. Table 2 shows the mixing ratio and the properties after mixing.
Handling was evaluated when the asphalt regeneration additive composition was prepared. As a result, among the asphalt regeneration additive compositions 1 to 6, 1 has a high kinematic viscosity and poor handling properties. Other than 1, there was no problem in handling. In addition, the case where handling property was good was described as “◯” and the case where it was bad was described as “X”.

Figure 0005744766
Figure 0005744766

(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3に示す。
(Deteriorated asphalt)
A straight asphalt with a penetration of 70 was tested in a thin film heating test at 163 ° C. for 5 hours, and then further deteriorated asphalt was obtained by a 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 3 shows the properties of the deteriorated asphalt.

Figure 0005744766
Figure 0005744766

(再生効果の確認)
針入度60〜80の新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て100℃×20時間×空気圧2.07MPaの条件下で劣化させ、針入度25、軟化点61℃、伸度5cmの劣化アスファルトを得た。
この劣化アスファルトに、目標針入度70±1となるように各再生添加剤組成物を添加し、加熱混合し再生した。得られた再生アスファルトの針入度、軟化点および伸度を測定し、再生添加剤組成物による再生効果を確認した。その結果を表4に示す。
(Check playback effect)
A new straight asphalt with a penetration of 60 to 80 was tested in a thin film heating test at 163 ° C. for 5 hours, and further subjected to a pressure accelerated deterioration test proposed by US SHRP at 100 ° C. for 20 hours × air pressure 2.07 MPa. Deteriorated under the condition, a deteriorated asphalt having a penetration of 25, a softening point of 61 ° C. and an elongation of 5 cm was obtained.
Each regeneration additive composition was added to the deteriorated asphalt so that the target penetration was 70 ± 1, and the mixture was regenerated by heating and mixing. The regenerated asphalt obtained was measured for penetration, softening point, and elongation, and the regenerating effect of the regenerating additive composition was confirmed. The results are shown in Table 4.

実施例1〜3の再生後のアスファルトの性状は、いずれも表5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品質規格を満足するものであった。なお、表4に記載していないが、引火点(COC)、トルエン可溶分、蒸発試験後の針入度比も日本道路協会の定める品質規格を満足するものであった。
比較例1に使用した再生添加剤組成物5及び比較例2に使用した再生添加剤組成物6は、ガスクロ蒸留による5容量%留出温度が低く、再生アスファルトの伸度の回復が悪く、日本道路協会の定める品質規格を満足しない。
比較例3に使用した再生添加剤組成物1は、40℃における動粘度が1500mm/sを超えるため、再生効果は認められるが、再生添加剤組成物の流動性が低く、ハンドリング性が極度に悪い。
The properties of the asphalt after regeneration in Examples 1 to 3 all satisfied the quality standards of straight asphalt for road paving established by the Japan Road Association shown in Table 5. Although not listed in Table 4, the flash point (COC), the toluene soluble content, and the penetration ratio after the evaporation test also satisfied quality standards established by the Japan Road Association.
The regeneration additive composition 5 used in Comparative Example 1 and the regeneration additive composition 6 used in Comparative Example 2 have a low 5% by volume distillation temperature by gas chromatography, and the recovery of regenerated asphalt is poor. Does not satisfy the quality standards set by the Road Association.
Since the regenerative additive composition 1 used in Comparative Example 3 has a kinematic viscosity at 40 ° C. exceeding 1500 mm 2 / s, a regenerative effect is observed, but the regenerative additive composition has low fluidity and extremely high handling properties. It ’s bad.

Figure 0005744766
Figure 0005744766

Figure 0005744766
Figure 0005744766

Claims (3)

(A)減圧蒸留残油を極性溶剤で抽出し40℃における動粘度が2000〜2500mm /s、多環芳香族炭化水素含有量が3質量%未満に調整したエキストラクトを50〜90質量%および(B)40℃における動粘度が80〜180mm /sの潤滑油基油を10〜50質量%配合して製造される、多環芳香族炭化水素(PCA)含有量が3質量%未満、40℃における動粘度が900〜1500mm/s、ガスクロ蒸留による5容量%留出温度が350℃以上、引火点が260℃以上、および芳香族分(%CA)が10〜25%であることを特徴とするアスファルト再生添加剤組成物。 (A) 50 to 90% by mass of an extract obtained by extracting the vacuum distillation residue with a polar solvent and adjusting the kinematic viscosity at 40 ° C. to 2000 to 2500 mm 2 / s and the polycyclic aromatic hydrocarbon content to less than 3% by mass. And (B) a polycyclic aromatic hydrocarbon (PCA) content of less than 3% by mass produced by blending 10-50% by mass of a lubricating base oil having a kinematic viscosity at 40 ° C. of 80-180 mm 2 / s The kinematic viscosity at 40 ° C. is 900-1500 mm 2 / s, the 5 vol% distillation temperature by gas chromatography is 350 ° C. or higher, the flash point is 260 ° C. or higher, and the aromatic content (% CA) is 10-25%. An asphalt regeneration additive composition characterized by that. 請求項1に記載のアスファルト再生添加剤組成物を、劣化アスファルト100重量部に対して4〜30重量部の割合で配合してなることを特徴とする再生アスファルト舗装材。 A recycled asphalt pavement comprising the asphalt regeneration additive composition according to claim 1 in a proportion of 4 to 30 parts by weight with respect to 100 parts by weight of deteriorated asphalt. (A)減圧蒸留残油を極性溶剤で抽出し40℃における動粘度が2000〜2500mm /s、多環芳香族炭化水素含有量が3質量%未満に調整したエキストラクトを50〜90質量%および(B)40℃における動粘度が80〜180mm /sの潤滑油基油を10〜50質量%配合することにより、多環芳香族炭化水素(PCA)含有量が3質量%未満、40℃における動粘度が900〜1500mm/s、ガスクロ蒸留による5容量%留出温度が350℃以上、引火点が260℃以上、および芳香族分(%CA)が10〜25%であるアスファルト再生添加剤組成物を得ることを特徴とするアスファルト再生添加剤組成物の製造方法。 (A) 50 to 90% by mass of an extract obtained by extracting the vacuum distillation residue with a polar solvent and adjusting the kinematic viscosity at 40 ° C. to 2000 to 2500 mm 2 / s and the polycyclic aromatic hydrocarbon content to less than 3% by mass. And (B) The polycyclic aromatic hydrocarbon (PCA) content is less than 3% by mass by blending 10 to 50% by mass of a lubricant base oil having a kinematic viscosity at 40 ° C. of 80 to 180 mm 2 / s. Asphalt regeneration with a kinematic viscosity at 900 ° C. of 900-1500 mm 2 / s, 5 vol% distillation temperature by gas chromatography, 350 ° C. or higher, flash point of 260 ° C. or higher, and aromatic content (% CA) of 10-25% A method for producing an asphalt regeneration additive composition, characterized by obtaining an additive composition.
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