JP5121210B2 - Low temperature fluid fuel composition - Google Patents
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- 239000000203 mixture Substances 0.000 title claims description 44
- 239000012530 fluid Substances 0.000 title claims description 34
- 239000000446 fuel Substances 0.000 title description 6
- 239000000295 fuel oil Substances 0.000 claims description 67
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 56
- 229910052799 carbon Inorganic materials 0.000 claims description 56
- 239000003921 oil Substances 0.000 claims description 51
- 239000003607 modifier Substances 0.000 claims description 41
- 239000003245 coal Substances 0.000 claims description 37
- 239000002199 base oil Substances 0.000 claims description 29
- 125000003118 aryl group Chemical group 0.000 claims description 24
- 229910052717 sulfur Inorganic materials 0.000 claims description 15
- 239000011593 sulfur Substances 0.000 claims description 15
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 13
- 238000004458 analytical method Methods 0.000 claims description 13
- 125000001931 aliphatic group Chemical group 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 238000000214 vapour pressure osmometry Methods 0.000 claims description 9
- 239000000284 extract Substances 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 7
- 239000004215 Carbon black (E152) Substances 0.000 claims description 5
- 229930195733 hydrocarbon Natural products 0.000 claims description 5
- 150000002430 hydrocarbons Chemical class 0.000 claims description 5
- 239000013256 coordination polymer Substances 0.000 claims 1
- 238000005481 NMR spectroscopy Methods 0.000 description 14
- 239000012467 final product Substances 0.000 description 13
- 238000012360 testing method Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 239000002283 diesel fuel Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 238000009530 blood pressure measurement Methods 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000010779 crude oil Substances 0.000 description 6
- 239000003085 diluting agent Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000006477 desulfuration reaction Methods 0.000 description 3
- 230000023556 desulfurization Effects 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- 239000010763 heavy fuel oil Substances 0.000 description 3
- 230000001771 impaired effect Effects 0.000 description 3
- 238000000638 solvent extraction Methods 0.000 description 3
- 238000005292 vacuum distillation Methods 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 239000010426 asphalt Substances 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 238000004440 column chromatography Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000005038 ethylene vinyl acetate Substances 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000003350 kerosene Substances 0.000 description 2
- 239000010687 lubricating oil Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003209 petroleum derivative Substances 0.000 description 2
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 235000021028 berry Nutrition 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000004231 fluid catalytic cracking Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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Description
本発明は、低温下で優れた流動性を有する低温流動性を改良した燃料油組成物に関する。 The present invention relates to a fuel oil composition having improved low temperature fluidity having excellent fluidity at low temperatures.
周知の通り、Ａ重油は一般的にハウス加温栽培用暖房機、ビル等の暖房機、漁船の燃料等に用いられるが、ここで問題となるのが低温時の流動性である。かねてより、Ａ重油には冬季における低温下あるいは寒冷地でのワックス分の析出、さらには流動性の悪化という重大な問題がある。例えば、Ａ重油中に含まれるワックス析出により、夾雑物阻止用のろ過器中のフィルターを閉塞させたり、さらに低温下で、Ａ重油が流動性を失い、燃料ラインそのものを閉塞させるといったような例が多くみられる。こうしたＡ重油の低温流動性を改善することが大きな課題となっていた。 As is well known, heavy fuel oil A is generally used as a heater for house warming cultivation, a heater for buildings, fuel for fishing boats, etc., but the problem here is the fluidity at low temperatures. For a long time, A heavy oil has a serious problem of precipitation of wax in a low temperature or in a cold region in winter and further deterioration of fluidity. For example, the precipitation of wax contained in heavy oil A causes the filter in the filter for preventing contaminants to be blocked, or even under low temperatures, heavy fuel oil A loses fluidity and blocks the fuel line itself. Is often seen. Improving the low-temperature fluidity of such A heavy oil has been a major issue.
従来、Ａ重油の低温下における流動性を改善する方法として、残油を添加する方法があり、アスファルテン含有量が６.０質量％以上あるいは残留炭素分が９.５質量％以上である残油を添加物として、Ａ重油基油に対して０.５〜２.０容量％添加することにより低温流動性が改良されることが知られている（例えば、特許文献１参照）。しかし、残油を多量に添加する方法は、スラッジの発生という点から好ましくなく、また、改善効果も小さいので、基材の変更を行いにくく、経済的なＡ重油の生産に支障をきたすという欠点がある。 Conventionally, there is a method of adding residual oil as a method for improving fluidity of A heavy oil at low temperature, and residual oil having an asphaltene content of 6.0% by mass or more or a residual carbon content of 9.5% by mass or more. As an additive, it is known that low temperature fluidity is improved by adding 0.5 to 2.0% by volume with respect to A heavy oil base oil (see, for example, Patent Document 1). However, the method of adding a large amount of residual oil is not preferable from the viewpoint of generation of sludge, and since the improvement effect is small, it is difficult to change the base material and hinders economical A heavy oil production. There is.
また、Ａ重油の低温流動性を改善する他の方法として、Ａ重油中の１０％残留炭素分、−１０℃におけるワックス含有量、アスファルテン分及び流動性向上剤の量が低温流動性に対する重要な因子であるとの知見に基づく、これらの量を特定の範囲にする方法が知られている（例えば、特許文献２参照）。しかし、この従来方法で使用されているＡ重油の基油は、当時の硫黄分規制値から見て５００〜２０００質量ｐｐｍ程度の硫黄分を含有した軽油が使用されている。軽油の硫黄分規制は環境への影響を考慮し規制が厳しくなる傾向にあり、現在では１０質量ｐｐｍ以下のいわゆるサルファーフリーの軽油が製造されている。しかしこのサルファーフリー軽油をＡ重油基油として用いる場合には、脱硫率の増加に伴い基油の低アロマ化が進行し、溶解性能が低下すると同時にワックス量が増加し、低温流動性能の面で悪化が懸念されるため、より一層の低温流動性の改善が求められている。 As another method for improving the low temperature fluidity of heavy oil A, the 10% residual carbon content in heavy oil A, the wax content at −10 ° C., the asphaltene content and the amount of fluidity improver are important for low temperature fluidity. Based on the knowledge that it is a factor, a method for bringing these amounts into a specific range is known (for example, see Patent Document 2). However, as the base oil of A heavy oil used in this conventional method, a light oil containing a sulfur content of about 500 to 2000 mass ppm is used in view of the sulfur content regulation value at that time. The regulation of sulfur content in light oil tends to be stricter in consideration of the impact on the environment. At present, so-called sulfur-free diesel oil with a mass of 10 mass ppm or less is produced. However, when this sulfur-free light oil is used as A heavy oil base oil, the base oil is reduced in aroma as the desulfurization rate is increased, so that the dissolving performance is lowered and the amount of wax is increased. Since there is concern about deterioration, there is a need for further improvement in low-temperature fluidity.
本発明は、上記従来の状況に鑑みてなされたものであり、低硫黄分のＡ重油基油を用いながらも低温流動性に優れた低温流動性燃料油組成物を提供することを目的とするものである。 This invention is made | formed in view of the said conventional condition, and it aims at providing the low-temperature fluidity fuel oil composition excellent in low-temperature fluidity | liquidity, using A heavy oil base oil of a low sulfur content. Is.
そこで、本発明者らは、上記目的を達成すべく、流動性向上剤と、種々の残油又はエキストラクトの共存下で十分な低温流動性を有するＡ重油について鋭意研究を行った結果、硫黄分が１０質量ｐｐｍ以下のいわゆるサルファーフリーのＡ重油基油を使用する場合であっても、基油に添加する常圧残油、減圧残油、脱硫残油、スラリーオイル及びエキストラクトなどの残炭調整材中のアスファルテン分の分子量及びアスファルテン含有量が低温流動性に対して重要な因子であって、これらの量を特定の範囲にすることにより、流動性向上剤の効果が十分に発揮され、低温流動性に優れた低温流動性燃料油組成物が得られることを見出して本発明を完成するに至った。 In order to achieve the above object, the present inventors have conducted earnest research on a heavy oil having sufficient low-temperature fluidity in the presence of a fluidity improver and various residual oils or extracts. Even when a so-called sulfur-free A heavy oil base oil with a content of 10 mass ppm or less is used, residues such as atmospheric residual oil, vacuum residual oil, desulfurized residual oil, slurry oil, and extract added to the base oil The molecular weight and asphaltene content of the asphaltene in the charcoal adjusting material are important factors for low-temperature fluidity, and by making these amounts within a specific range, the effect of the fluidity improver is fully demonstrated. The inventors have found that a low-temperature fluid fuel oil composition excellent in low-temperature fluidity can be obtained, and have completed the present invention.
すなわち、本発明は、次の低温流動性燃料油組成物を提供するものである。
（１）硫黄分１０質量ｐｐｍ以下の脱硫軽油を１０〜７０容量％含有するＡ重油基油と、
常圧残油、減圧残油、脱硫残油、スラリーオイル及びエキストラクトから選ばれた少なくとも１種の炭化水素油からなる残炭調整材と、
流動性向上剤とを含有してなる低温流動性燃料油組成物であって、
蒸気圧オスモメトリー法（ＶＰＯ）にて測定した前記残炭調整材中のアスファルテン分の分子量が５１４０〜５６９０であり、前記残炭調整材中のアスファルテン分含有量が組成分析値で１．５３〜７．８８質量％であり、前記アスファルテン分の平均構造パラメータである芳香環数（ＲＮ）が１５０以下であり、芳香族炭素（ＣＡ）が２００〜３００、かつ、脂肪族炭素（ＣＰ）が１００〜２００であり、
前記流動性向上剤の含有量が燃料油組成物基準で１００〜１０００容量ｐｐｍであり、
前記残炭調整材を、前記低温流動性燃料油組成物中の１０％残留炭素分が０．２質量％以上になるように添加してなることを特徴とする低温流動性燃料油組成物。
That is, the present invention provides the following low-temperature fluid fuel oil composition.
(1) A heavy oil base oil containing 10 to 70% by volume of desulfurized gas oil having a sulfur content of 10 mass ppm or less;
A residual carbon modifier comprising at least one hydrocarbon oil selected from atmospheric residual oil, vacuum residual oil, desulfurized residual oil, slurry oil, and extract;
A low-temperature fluid fuel oil composition comprising a fluidity improver,
The molecular weight of asphaltene in the residual coal modifier as measured by the vapor pressure osmometry method (VPO) is 5140-5690 , and the asphaltene content in the residual coal modifier is 1.53 as a compositional analysis value. 7.88% by mass, the number of aromatic rings (RN), which is an average structural parameter of the asphaltenes , is 150 or less, aromatic carbon (CA) is 200 to 300, and aliphatic carbon (CP) is 100. ~ 200,
The content of the fluidity improver is 100 to 1000 ppm by volume based on the fuel oil composition,
A low-temperature fluid fuel oil composition, wherein the residual coal modifier is added so that a 10% residual carbon content in the low-temperature fluid fuel oil composition is 0.2 mass% or more .
本発明によれば、硫黄分１０質量ｐｐｍ以下のいわゆるサルファーフリーのＡ重油基油を使用した場合でも、特定の分子量のアスファルテン分を含有する残炭調整材を配合し、低温流動性燃料油組成物最終製品中の１０％残留炭素分、及び流動性向上剤の量を特定の範囲にすることにより、極めて優れた低温流動性を示す低温流動性燃料油組成物を提供することができて、低温流動性の優れた低温流動性燃料油組成物の製造において極めて有用である。また、本発明に従った低温流動性燃料油組成物は、冬季における低温下あるいは寒冷地でのＡ重油を燃料とする動力機器や暖房機等の安定運転を行うことができる。 According to the present invention, even when a so-called sulfur-free A heavy oil base oil having a sulfur content of 10 mass ppm or less is used, a residual coal modifier containing an asphaltene component having a specific molecular weight is blended to produce a low-temperature fluid fuel oil composition By making the amount of the 10% residual carbon content and the fluidity improver in the final product into a specific range, it is possible to provide a low temperature fluid fuel oil composition exhibiting extremely excellent low temperature fluidity, This is extremely useful in the production of a low-temperature fluid fuel oil composition having excellent low-temperature fluidity. In addition, the low-temperature fluid fuel oil composition according to the present invention can perform stable operation of power equipment, heaters, and the like using A heavy oil as fuel at low temperatures in winter or in cold regions.
以下、本発明を詳細に説明する。
本発明の低温流動性燃料油組成物は、Ａ重油基油として硫黄分１０質量ｐｐｍ以下の脱硫軽油を１０〜７０容量％、好ましくは２０〜６０容量％含有する。硫黄分１０質量ｐｐｍ以下の脱硫軽油が１０容量％以上ならば、従来の硫黄分５００〜２０００質量ｐｐｍ程度の比較的硫黄分の多い軽油を用いた場合と同等の低温流動性能を確保でき、また、７０容量％以下ならばＡ重油基油の過剰な低アロマ化を防止し、その溶解性の過剰な低下による低温流動性能の悪化を防止することができる。Ａ重油基油としては、上記脱硫軽油以外に、灯油、脱硫灯油、間脱軽質軽油、間脱重質軽油、直脱軽質軽油、直脱重質軽油、直留軽油、分解軽油、減圧軽油などから選ばれた少なくとも１種を用いることができ、それらがＡ重油基油に３０〜９０容量％配合される。
Hereinafter, the present invention will be described in detail.
The low-temperature fluid fuel oil composition of the present invention contains 10 to 70% by volume, preferably 20 to 60% by volume, of desulfurized gas oil having a sulfur content of 10 mass ppm or less as A heavy oil base oil. If the desulfurized gas oil having a sulfur content of 10 mass ppm or less is 10 vol% or more, the low-temperature fluidity equivalent to the conventional case of using a relatively sulfur-rich gas oil having a sulfur content of about 500 to 2000 mass ppm can be secured. If it is 70% by volume or less, it is possible to prevent excessive lowering of the A heavy oil base oil, and it is possible to prevent deterioration in low-temperature flow performance due to excessive decrease in its solubility. A heavy oil base oil includes kerosene, desulfurized kerosene, lightly degassed light oil, lightly degassed light oil, lightly degassed light oil, direct delighted heavy light oil, straight-run light oil, cracked light oil, vacuum light oil, etc. At least one selected from the group consisting of 30 to 90% by volume in the A heavy oil base oil.
本発明の低温流動性燃料油組成物は、上記Ａ重油基油に加え、常圧残油、減圧残油、脱硫残油、スラリーオイル及びエキストラクトから選ばれた少なくとも１種の炭化水素油からなる残炭調整材を含む。この残炭調整材は、含まれるアスファルテン分の分子量が８０００以下、好ましくは７０００以下のものである。残炭調整材に含まれるアスファルテン分は、流動性向上剤と同等の働きをする傾向がある。分子量が高いアスファルテン分は、添加した流動性向上剤と負の相互作用が働き、結果として低温流動性能を低下してしまうため、含有するアスファルテン分の分子量を８０００以下に限定することで、Ａ重油基油に低硫黄な基材を使用した場合であっても流動性向上剤の添加効果を損なわず、残炭調整材自体も流動性向上の働きをする傾向があって、好適に低温流動性を向上させることが可能となる。 The low-temperature fluid fuel oil composition of the present invention comprises at least one hydrocarbon oil selected from atmospheric residue, reduced residue, desulfurized residue, slurry oil, and extract in addition to the A heavy oil base oil. The remaining charcoal adjustment material. This residual carbon modifier has a molecular weight of 8,000 or less, preferably 7000 or less, asphaltene content. The asphaltene content contained in the residual coal modifier tends to perform the same function as the fluidity improver. Since the asphaltene component having a high molecular weight has a negative interaction with the added fluidity improver, resulting in a decrease in low-temperature fluidity, the molecular weight of the asphaltene component is limited to 8000 or less. Even when a low-sulfur base material is used for the base oil, the effect of adding a fluidity improver is not impaired, and the residual coal modifier itself tends to work to improve fluidity. Can be improved.
ここで上記残炭調整材に用いる常圧残油とは、常圧蒸留装置で原油を常圧において蒸留して得られる残油である。減圧残油とは、減圧蒸留装置で常圧残油を減圧下で蒸留して得られる残油である。脱硫残油とは、直接脱硫装置で常圧残油又は減圧残油を処理して得られる残油である。これらの残油は、原料及び装置の条件により性状が変化するが、残油中のアスファルテンの分子量が８０００以下になるよう、原料や常圧蒸留、減圧蒸留装置の運転条件を変更することで得ることができる。常圧残油、減圧残油中のアスファルテンの分子量が８０００以下となる原料としては、例えば、ザコム原油、アッパーザクム原油、マーバン原油、ベリー原油などが挙げられる。
スラリーオイルとは、流動接触分解装置から得られる残油であり、沸点が３５０℃以上のものである。エキストラクトとは、潤滑油原料用減圧蒸留装置からの留分を、溶剤抽出法により抽出分離したもののうち潤滑油に適さない芳香族成分のことである。残炭調整材に用いるスラリーオイル、エキストラクトも、含まれるアスファルテンの分子量が８０００以下になるよう、原料や運転条件を変更することで得ることができる。これらの残炭調整材に用いる炭化水素油は、１種単独で添加してもよいが、２種以上を組み合わせて添加してもよい。なお、残炭調整材のアスファルテンは、n−ヘプタンとトルエンを用いた溶剤抽出により分離し、得られたアスファルテン分の分子量を蒸気圧オスモメトリー法にて測定した。
Here, the atmospheric residual oil used for the residual coal modifier is a residual oil obtained by distilling crude oil at atmospheric pressure with an atmospheric distillation apparatus. The vacuum residue is a residue obtained by distilling atmospheric residue under reduced pressure using a vacuum distillation apparatus. A desulfurization residual oil is a residual oil obtained by processing an atmospheric residue or a vacuum residue with a direct desulfurization apparatus. The properties of these residual oils vary depending on the conditions of the raw materials and equipment, but are obtained by changing the operating conditions of the raw materials, atmospheric distillation, and vacuum distillation equipment so that the molecular weight of asphaltenes in the residual oil is 8000 or less. be able to. Examples of the raw material in which the molecular weight of asphaltenes in the atmospheric residue and the vacuum residue is 8000 or less include Zacom crude oil, upper Zakum crude oil, Marvan crude oil, and berry crude oil.
Slurry oil is residual oil obtained from a fluid catalytic cracking apparatus, and has a boiling point of 350 ° C. or higher. The extract is an aromatic component that is not suitable for lubricating oil among the fractions extracted from the vacuum distillation apparatus for lubricating oil raw material by solvent extraction. The slurry oil and extract used for the residual coal modifier can also be obtained by changing the raw materials and operating conditions so that the molecular weight of the asphaltenes contained is 8000 or less. The hydrocarbon oil used for these residual coal modifiers may be added singly or in combination of two or more. In addition, the asphaltene of the residual coal adjusting material was separated by solvent extraction using n-heptane and toluene, and the molecular weight of the obtained asphaltene was measured by a vapor pressure osmometry method.
本発明の低温流動性燃料油組成物に添加する残炭調整材中のアスファルテン含有量は、０．５〜１０質量％（組成分析値）、好ましくは３〜８質量％以下が望ましい。低硫黄分のＡ重油基油を使用した場合、残炭調整材中のアスファルテン含有量が０．５質量％以上もしくは、１０質量％以下ならば、より添加した流動性向上剤との負の相互作用を防止できるため、より低温流動性向上剤の添加効果が損なわれず低温性能を向上できる。なお、アスファルテン含有量は、アスファルトのカラムクロマトグラフィーによる組成分析法（ＪＰＩ−５Ｓ−２２−８３）により求めた。 The asphaltene content in the residual coal modifier added to the low-temperature fluid fuel oil composition of the present invention is 0.5 to 10% by mass (composition analysis value), preferably 3 to 8% by mass or less. When using a low-sulfur A heavy oil base oil, if the asphaltene content in the residual coal modifier is 0.5% by mass or more or 10% by mass or less, a negative mutual relationship with the added fluidity improver Since the action can be prevented, the low temperature performance can be improved without impairing the effect of adding the low temperature fluidity improver. In addition, asphaltene content was calculated | required by the composition analysis method (JPI-5S-22-83) by the column chromatography of asphalt.
本発明の低温流動性燃料油組成物に添加する残炭調整材において、残炭調整材中のアスファルテン分の平均構造パラメータ芳香環数（ＲＮ）は、１５０以下、好ましくは７０〜１００であることが望ましい。低硫黄分のＡ重油基油を使用した場合、残炭調整材中のアスファルテン分の平均構造パラメータ芳香環数（ＲＮ）が１５０以下ならば、より流動性向上剤の添加効果が損なわれず低温流動性能を向上できる。なお、アスファルテン分の平均構造パラメータ芳香環数（ＲＮ）は、核磁気共鳴装置NMR（Nuclear Magnetic Resonance）により測定する。 In the residual coal modifier added to the low-temperature fluid fuel oil composition of the present invention, the average structural parameter aromatic ring number (RN) of asphaltenes in the residual coal modifier is 150 or less, preferably 70-100. Is desirable. When using A heavy oil base oil with low sulfur content, if the average structural parameter aromatic ring number (RN) of asphaltene in the residual coal modifier is 150 or less, the effect of adding a fluidity improver will not be impaired and low temperature flow Performance can be improved. In addition, the average structural parameter aromatic ring number (RN) for asphaltenes is measured by a nuclear magnetic resonance apparatus NMR (Nuclear Magnetic Resonance).
本発明の低温流動性燃料油組成物に添加する残炭調整材において、残炭調整材中のアスファルテン分の平均構造パラメータ芳香族炭素（ＣＡ）は、３００以下で、かつ、脂肪族炭素（ＣＰ）は２５０以下、好ましくは芳香族炭素（ＣＡ）が２００〜３００、かつ、脂肪族炭素（ＣＰ）が１００〜２００であることが望ましい。低硫黄分のＡ重油基油を使用した場合、残炭調整材中のアスファルテン分の平均構造パラメータ芳香族炭素（ＣＡ）が３００以下、かつ脂肪族炭素（ＣＰ）が２５０以下ならば、より流動性向上剤の添加効果が損なわれず低温流動性能を向上できる。なお、アスファルテン分の平均構造パラメータの芳香族炭素（ＣＡ）と脂肪族炭素（ＣＰ）は核磁気共鳴装置NMR（Nuclear Magnetic Resonance）により測定する。 In the residual coal modifier added to the low-temperature fluid fuel oil composition of the present invention, the average structural parameter aromatic carbon (CA) of asphaltenes in the residual coal modifier is 300 or less, and aliphatic carbon (CP ) Is 250 or less, preferably aromatic carbon (CA) is 200 to 300, and aliphatic carbon (CP) is 100 to 200. When low sulfur A heavy oil base oil is used, if the average structural parameter aromatic carbon (CA) of asphaltene in the residual coal modifier is 300 or less and aliphatic carbon (CP) is 250 or less, more fluid The effect of adding the property improver is not impaired, and the low temperature flow performance can be improved. In addition, the aromatic carbon (CA) and the aliphatic carbon (CP) of the average structure parameter of asphaltenes are measured by a nuclear magnetic resonance apparatus NMR (Nuclear Magnetic Resonance).
本発明で使用する流動性向上剤は、市販のものをはじめ各種流動性向上剤を使用することができ、特に制限はないがエチレン−エチレン性不飽和エステル共重合体に代表されるポリマータイプ、例えばエチレン−酢酸ビニル共重合体、あるいは長鎖ジカルボン酸アミドに代表される油溶性分散剤タイプが好ましい。
本発明においては、流動性向上剤の添加量は、燃料油組成物基準で１００〜１０００容量ｐｐｍであり、好ましくは２００〜５００容量ｐｐｍである。１００容量ｐｐｍより添加量が少ない場合、流動性向上剤の効果が現れにくくなる。逆に１０００容量ｐｐｍを超えて添加しても、コストアップに見合うだけの効果は得られない。
As the fluidity improver used in the present invention, various fluidity improvers including commercially available ones can be used. Although there is no particular limitation, a polymer type represented by an ethylene-ethylenically unsaturated ester copolymer, For example, an oil-soluble dispersant type represented by an ethylene-vinyl acetate copolymer or a long-chain dicarboxylic acid amide is preferable.
In the present invention, the addition amount of the fluidity improver is 100 to 1000 ppm by volume, preferably 200 to 500 ppm by volume, based on the fuel oil composition. When the amount added is less than 100 ppm by volume, the effect of the fluidity improver is less likely to appear. On the other hand, even if it is added in excess of 1000 ppm by volume, an effect sufficient for cost increase cannot be obtained.
本発明において、常圧残油、減圧残油、脱硫残油、スラリーオイル、及びエキストラクトから選ばれた少なくとも１種の炭化水素油からなる残炭調整材を加えて得られる低温流動性燃料油組成物最終製品中の１０％残留炭素分は、０.２質量％以上であり、好ましくは０.２〜５.０質量％、さらに好ましくは０.２〜１.０質量％である。１０％残留炭素分が０.２質量％以上ならば、「１０％残油の残留炭素分０.２質量％以上」というＡ重油の免税条件を満足することができ、また、１０％残留炭素分がここに示す好ましい範囲内ならば、スラッジの発生を防止することができて好ましい。 In the present invention, a low-temperature fluid fuel oil obtained by adding a residual coal modifier comprising at least one hydrocarbon oil selected from atmospheric residue, vacuum residue, desulfurized residue, slurry oil, and extract The 10% residual carbon content in the final composition composition is 0.2% by mass or more, preferably 0.2 to 5.0% by mass, and more preferably 0.2 to 1.0% by mass. If the 10% residual carbon content is 0.2% by mass or more, the duty-free condition of heavy fuel oil A “residual carbon content of 10% residual oil is 0.2% by mass or more” can be satisfied. If the minute content is within the preferred range shown here, it is possible to prevent generation of sludge.
上記本発明の低温流動性燃料油組成物の各成分の添加方法には、特に制限はなく、残炭調整材を先にＡ重油基油に添加した後流動性向上剤を添加してもよく、逆に流動性向上剤を先にＡ重油基油に添加した後残炭調整材を添加してもよく、さらに残炭調整材と流動性向上剤とを予め混合した後Ａ重油基油に添加してもよい。また、残炭調整材や流動性向上剤は適当な溶剤の溶液として添加してもよい。また、本発明の低温流動性燃料油組成物は、石油留分燃料油に通常添加される防錆剤、酸化防止剤、防食剤、静電気防止剤などの添加剤を添加してもよい。 The method for adding each component of the low-temperature fluid fuel oil composition of the present invention is not particularly limited, and a fluidity improver may be added after the residual coal modifier is first added to the A heavy oil base oil. On the contrary, after adding the fluidity improver to the A heavy oil base oil, the residual coal modifier may be added, and after further mixing the residual coal modifier and the fluidity improver in advance, It may be added. Moreover, you may add a residual coal modifier and a fluidity improver as a solution of a suitable solvent. Moreover, the low-temperature fluid fuel oil composition of the present invention may contain additives such as a rust inhibitor, an antioxidant, an anticorrosive, and an antistatic agent that are usually added to petroleum distillate fuel oils.
以下に本発明を実施例及び比較例により具体的に説明するが、本発明はこれらの例によって何ら限定されるものではない。
以下の実施例及び比較例において、１０％残留炭素分、アスファルテン分などは次に示す方法により求めた。すなわち、１０％残留炭素分は、ＪＩＳ Ｋ-２２７０（原油及び石油製品残留炭素分試験方法）により求めた。アスファルテン含有量は、アスファルトのカラムクロマトグラフィーによる組成分析法（ＪＰＩ−５Ｓ−２２−８３）により求めた。さらに、n-ヘプタンとトルエンを用いた溶剤抽出により分離したアスファルテン分を核磁気共鳴装置 NMR（Nuclear Magnetic Resonance）により、平均構造パラメータを求めた。また、アスファルテンの分子量は蒸気圧オスモメトリー法（VPO）にて測定した。
The present invention will be specifically described below with reference to examples and comparative examples, but the present invention is not limited to these examples.
In the following Examples and Comparative Examples, 10% residual carbon content, asphaltene content and the like were determined by the following methods. That is, 10% residual carbon content was determined according to JIS K-2270 (crude oil and petroleum product residual carbon content test method). The asphaltene content was determined by a composition analysis method (JPI-5S-22-83) using asphalt column chromatography. Furthermore, the average structural parameters of the asphaltenes separated by solvent extraction using n-heptane and toluene were determined by nuclear magnetic resonance NMR (Nuclear Magnetic Resonance). The molecular weight of asphaltenes was measured by vapor pressure osmometry (VPO).
核磁気共鳴装置 NMR（Nuclear Magnetic Resonance）における主要な分析条件を表１に記載した。 Table 1 shows the main analysis conditions in the nuclear magnetic resonance apparatus NMR (Nuclear Magnetic Resonance).
蒸気圧オスモメトリー法（VPO）の主要な分析条件を表２に記載した。 Table 2 shows the main analysis conditions of the vapor pressure osmometry method (VPO).
実施例及び比較例において、得られた低温流動性燃料油組成物最終製品の実用流動性の評価は、図１に記載した低温流動性試験器を用いて行った。この低温流動性試験器の燃料フィルターは、ハウス栽培用温風機に使用される金網の目開き１４９ミクロン（１００メッシュ）、濾過面積４７±３ｃｍ２で容器容量５０±５ｃｍ３である。試験条件として、冷却速度は冬季の平野部における気象条件をもとに１℃／ｈ、冷却開始温度は１０℃、試験温度は−６℃、ソーキングは試験温度で３時間とした。判定は、燃料フィルター前後で負圧を測定し、その値により行った。負圧の測定は１分毎に行い、６０分間続けた。通油開始直後から測定した負圧の最高値が１００ｍｍＨｇ以下の時、低温流動性は優れているものとし、○で表す。負圧の最高値が１００ｍｍＨｇより大きく２５０ｍｍＨｇ以下の時、低温流動性はあまりよくないものとし、△で表す。負圧の最高値が３００ｍｍＨｇより大きいとき、低温流動性は良くないものとし、×で表す。 In Examples and Comparative Examples, evaluation of practical fluidity of the obtained low-temperature fluid fuel oil composition final products was performed using the low-temperature fluidity tester described in FIG. The fuel filter of this low-temperature fluidity tester has a mesh size of 149 microns (100 mesh) for a wire net used for a house-cultivating hot air machine, a filtration area of 47 ± 3 cm 2 and a container capacity of 50 ± 5 cm 3 . As the test conditions, the cooling rate was 1 ° C./h based on the weather conditions in the plain in winter, the cooling start temperature was 10 ° C., the test temperature was −6 ° C., and the soaking was at the test temperature for 3 hours. The determination was made by measuring the negative pressure before and after the fuel filter and using the value. Negative pressure measurements were taken every minute and continued for 60 minutes. When the maximum value of the negative pressure measured immediately after the start of oil passage is 100 mmHg or less, the low temperature fluidity is assumed to be excellent, and is represented by ◯. When the maximum value of the negative pressure is greater than 100 mmHg and less than or equal to 250 mmHg, the low-temperature fluidity is assumed to be not very good and is represented by Δ. When the maximum value of the negative pressure is greater than 300 mmHg, the low temperature fluidity is not good and is represented by x.
実施例１
表３に性状を示したサルファーフリーの脱硫軽油Ａ４５容量％と、FCC-LCO（FCC-ライトサイクルオイル）、HGO（重質軽油）、L-VGO（軽質減圧軽油）等から構成され、表４に性状を示したその他基油５５容量％とからなる基油に、希釈溶剤で粘度調整した表５に性状を示す残炭調整材を加え、低温流動性燃料油組成物最終製品中の１０％残留炭素分が０．２質量％となるように調合し、それに流動性向上剤を５００容量ｐｐｍ添加した。
なお、実施例、比較例共に、残炭調整材としては減圧残油を用い、流動性向上剤としては市販のエチレン−酢酸ビニル共重合体系流動性向上剤を用いた。
用いた残炭調整材に含まれるアスファルテン含有量は１．５３質量％、アスファルテン分の分子量は５６５７であった。さらに、アスファルテン分のNMRによる構造パラメータの解析による芳香環数(ＲＮ)は７２、芳香族炭素(ＣＡ)は２５１、脂肪族炭素(ＣＰ)は１５１であった。
得られた低温流動性燃料油組成物最終製品の低温流動性試験器による負圧測定の最高負圧は６０ｍｍＨｇであった。
これらの試験結果を表５に纏めて示した。
Example 1
It consists of Sulfur-free desulfurized diesel oil A45% by volume shown in Table 3, FCC-LCO (FCC-light cycle oil), HGO (heavy diesel oil), L-VGO (light vacuum gas diesel), etc. 10% remaining in the final product of the low-temperature fluid fuel oil composition is added to the base oil consisting of 55% by volume of the other base oil that shows the properties, and the residual carbon modifier shown in Table 5 whose viscosity is adjusted with a diluent solvent. The carbon content was adjusted to 0.2% by mass, and 500 ppm by volume of a fluidity improver was added thereto.
In both Examples and Comparative Examples, a residual oil under reduced pressure was used as a residual coal modifier, and a commercially available ethylene-vinyl acetate copolymer fluidity improver was used as a fluidity improver.
The asphaltene content contained in the residual coal modifier used was 1.53% by mass, and the molecular weight of the asphaltene component was 5657. Furthermore, the number of aromatic rings (RN) by analysis of structural parameters by NMR of asphaltenes was 72, aromatic carbon (CA) was 251 and aliphatic carbon (CP) was 151.
The maximum negative pressure in the negative pressure measurement by the low temperature fluidity tester of the obtained low temperature fluid fuel oil composition final product was 60 mmHg.
These test results are summarized in Table 5.
実施例２
表３に性状を示したサルファーフリーの脱硫軽油Ｂが５０容量％、FCC-LCO、HGO、L-VGO等から構成され、表４に性状を示したその他基油が５０容量％の基油に、希釈溶剤で粘度調整した表５に性状を示す残炭調整材を加え、低温流動性燃料油組成物最終製品中の１０％残留炭素分が０．２１質量％となるように調合し、それに流動性向上剤を５００容量ｐｐｍ添加した。
用いた残炭調整材に含まれるアスファルテン含有量は５．０６質量％、アスファルテン分の分子量は５６９０であった。さらに、アスファルテン分のNMRによる構造パラメータの解析による芳香環数(ＲＮ)は８７、芳香族炭素(ＣＡ)は２６８、脂肪族炭素(ＣＰ)は１４９であった。
得られた低温流動性燃料油組成物最終製品の低温流動性試験器による負圧測定の最高負圧は７０ｍｍＨｇであった。
これらの試験結果を表５に纏めて示した。
Example 2
Sulfur-free desulfurized diesel oil B whose properties are shown in Table 3 is composed of 50% by volume, FCC-LCO, HGO, L-VGO, etc., and other base oils whose properties are shown in Table 4 are 50% by volume. In addition, a residual coal modifier showing properties is added to Table 5 whose viscosity is adjusted with a diluent solvent, and a 10% residual carbon content in the final product of the low-temperature fluid fuel oil composition is 0.21% by mass. 500 ppm by volume of fluidity improver was added.
The asphaltene content contained in the residual coal modifier used was 5.06% by mass, and the molecular weight of the asphaltene component was 5690. Furthermore, the number of aromatic rings (RN) was 87, the aromatic carbon (CA) was 268, and the aliphatic carbon (CP) was 149 by analysis of structural parameters by NMR of asphaltenes.
The maximum negative pressure in the negative pressure measurement by the low temperature fluidity tester of the obtained low temperature fluid fuel oil composition final product was 70 mmHg.
These test results are summarized in Table 5.
実施例３
表３に性状を示したサルファーフリーの脱硫軽油Ｃが５５容量％、FCC-LCO、HGO、L-VGO等から構成され、表４に性状を示したその他基油が４５容量％の基油に、希釈溶剤で粘度調整した表５に性状を示す残炭調整材を加え、低温流動性燃料油組成物最終製品中の１０％残留炭素分が０．３質量％となるように調合し、それに流動性向上剤を５００容量ｐｐｍ添加した。
用いた残炭調整材に含まれるアスファルテン含有量は７．８８質量％、アスファルテン分の分子量は５１４０であった。さらに、アスファルテン分のNMRによる構造パラメータの解析による芳香環数(ＲＮ)は６９、芳香族炭素(ＣＡ)は２１７、脂肪族炭素(ＣＰ)は１７５であった。
得られた低温流動性燃料油組成物最終製品の低温流動性試験器による負圧測定の最高負圧は８５ｍｍＨｇであった。
これらの試験結果を表５に纏めて示した。
Example 3
Sulfur-free desulfurized diesel oil C whose properties are shown in Table 3 is composed of 55% by volume, FCC-LCO, HGO, L-VGO, etc., and other base oils whose properties are shown in Table 4 are 45% by volume. In addition, a residual carbon modifier showing properties is added to Table 5 whose viscosity is adjusted with a diluent solvent, and the low-temperature fluid fuel oil composition is prepared so that the 10% residual carbon content in the final product is 0.3% by mass. 500 ppm by volume of fluidity improver was added.
The asphaltene content contained in the used residual coal modifier was 7.88% by mass, and the molecular weight of the asphaltene component was 5140. Further, the number of aromatic rings (RN) was 69, the number of aromatic carbons (CA) was 217, and the number of aliphatic carbons (CP) was 175 by analysis of structural parameters by NMR of asphaltenes.
The maximum negative pressure in the negative pressure measurement by the low temperature fluidity tester of the obtained low temperature fluid fuel oil composition final product was 85 mmHg.
These test results are summarized in Table 5.
比較例１
表３に性状を示したサルファーフリーの脱硫軽油Ａが７５容量％、FCC-LCO、HGO、L-VGO等から構成され、表４に性状を示したその他基油が２５容量％の基油に、希釈溶剤で粘度調整した表５に性状を示す残炭調整材を加え、低温流動性燃料油組成物最終製品中の１０％残留炭素分が０．３９質量％となるように調合し、それに流動性向上剤を５００容量ｐｐｍ添加した。
用いた残炭調整材に含まれるアスファルテン含有量は６．５質量％、アスファルテン分の分子量は８１００であった。さらに、アスファルテン分のNMRによる構造パラメータの解析による芳香環数(ＲＮ)は１５０、芳香族炭素(ＣＡ)は３２０、脂肪族炭素(ＣＰ)は２５５であった。
得られた低温流動性燃料油組成物最終製品の低温流動性試験器による負圧測定の最高負圧は４００ｍｍＨｇであった。
これらの試験結果を表５に纏めて示した。
Comparative Example 1
Sulfur-free desulfurized diesel oil A whose properties are shown in Table 3 is composed of 75% by volume, FCC-LCO, HGO, L-VGO, etc., and other base oils whose properties are shown in Table 4 are 25% by volume. In addition, a residual coal modifier showing properties is added to Table 5 whose viscosity is adjusted with a diluent solvent, and the low-temperature fluid fuel oil composition is prepared so that the 10% residual carbon content in the final product is 0.39% by mass, 500 ppm by volume of fluidity improver was added.
The asphaltene content contained in the residual coal modifier used was 6.5% by mass, and the molecular weight of the asphaltene component was 8100. Furthermore, the number of aromatic rings (RN) by analysis of structural parameters by NMR of asphaltene content was 150, aromatic carbon (CA) was 320, and aliphatic carbon (CP) was 255.
The maximum negative pressure of the negative pressure measurement by the low temperature fluidity tester of the obtained low temperature fluidity fuel oil composition final product was 400 mmHg.
These test results are summarized in Table 5.
比較例２
表３に性状を示したサルファーフリーの脱硫軽油Ｂが５０容量％、FCC-LCO、HGO、L-VGO等から構成され、表４に性状を示したその他基油が５０容量％の基油に、希釈溶剤で粘度調整した表５に性状を示す残炭調整材を加え、低温流動性燃料油組成物最終製品中の１０％残留炭素分が０．３１質量％となるように調合し、それに流動性向上剤を５００容量ｐｐｍ添加した。
用いた残炭調整材に含まれるアスファルテン含有量は８．７１質量％、アスファルテン分の分子量は１１６００であった。さらに、アスファルテン分のNMRによる構造パラメータの解析による芳香環数(ＲＮ)は１９０、芳香族炭素(ＣＡ)は５７１、脂肪族炭素(ＣＰ)は３２４であった。
得られた低温流動性燃料油組成物最終製品の低温流動性試験器による負圧測定の最高負圧は５５０ｍｍＨｇであった。
これらの試験結果を表５に纏めて示した。
Comparative Example 2
Sulfur-free desulfurized diesel oil B whose properties are shown in Table 3 is composed of 50% by volume, FCC-LCO, HGO, L-VGO, etc., and other base oils whose properties are shown in Table 4 are 50% by volume. In addition, a residual coal modifier showing properties is added to Table 5 whose viscosity is adjusted with a diluent solvent, and the low-temperature fluid fuel oil composition is prepared so that the 10% residual carbon content in the final product is 0.31% by mass, 500 ppm by volume of fluidity improver was added.
The asphaltene content contained in the residual coal modifier used was 8.71% by mass, and the molecular weight of the asphaltene component was 11600. Furthermore, the number of aromatic rings (RN) was 190, aromatic carbon (CA) was 571, and aliphatic carbon (CP) was 324 by analysis of structural parameters by NMR of asphaltenes.
The maximum negative pressure of the negative pressure measurement by the low-temperature fluidity tester of the obtained low-temperature fluid fuel oil composition final product was 550 mmHg.
These test results are summarized in Table 5.
比較例３
表３に性状を示したサルファーフリーの脱硫軽油Ｃが５０容量％、FCC-LCO、HGO、L-VGO等から構成され、表４に性状を示したその他基油が５０容量％の基油に、希釈溶剤で粘度調整した表５に性状を示す残炭調整材を加え、低温流動性燃料油組成物最終製品中の１０％残留炭素分が０．３２質量％となるように調合し、それに流動性向上剤を５００容量ｐｐｍ添加した。
用いた残炭調整材に含まれるアスファルテン含有量は１０．３質量％、アスファルテン分の分子量は９３７０であった。さらに、アスファルテン分のNMRによる構造パラメータの解析による芳香環数(ＲＮ)は１５５、芳香族炭素(ＣＡ)は４６０、脂肪族炭素(ＣＰ)は２６３であった。
得られた低温流動性燃料油組成物最終製品の低温流動性試験器による負圧測定の最高負圧は５２０ｍｍＨｇであった。
これらの試験結果を表５に纏めて示した。
Comparative Example 3
Sulfur-free desulfurized diesel oil C whose properties are shown in Table 3 is composed of 50% by volume, FCC-LCO, HGO, L-VGO, etc., and other base oils whose properties are shown in Table 4 are 50% by volume of base oil. In addition, a residual coal modifier showing properties is added to Table 5 whose viscosity is adjusted with a diluent solvent, and the low-temperature fluid fuel oil composition is prepared so that the 10% residual carbon content in the final product is 0.32% by mass. 500 ppm by volume of fluidity improver was added.
The asphaltene content contained in the used residual coal modifier was 10.3% by mass, and the molecular weight of asphaltene was 9370. Furthermore, the number of aromatic rings (RN) was 155, aromatic carbon (CA) was 460, and aliphatic carbon (CP) was 263 by analysis of structural parameters by NMR of asphaltenes.
The maximum negative pressure of the negative pressure measurement by the low-temperature fluidity tester of the obtained low-temperature fluid fuel oil composition final product was 520 mmHg.
These test results are summarized in Table 5.
Claims (1)
常圧残油、減圧残油、脱硫残油、スラリーオイル及びエキストラクトから選ばれた少なくとも１種の炭化水素油からなる残炭調整材と、
流動性向上剤とを含有してなる低温流動性燃料油組成物であって、
蒸気圧オスモメトリー法（ＶＰＯ）にて測定した前記残炭調整材中のアスファルテン分の分子量が５１４０〜５６９０であり、前記残炭調整材中のアスファルテン分含有量が組成分析値で１．５３〜７．８８質量％であり、前記アスファルテン分の平均構造パラメータである芳香環数（ＲＮ）が１５０以下であり、芳香族炭素（ＣＡ）が２００〜３００、かつ、脂肪族炭素（ＣＰ）が１００〜２００であり、
前記流動性向上剤の含有量が燃料油組成物基準で１００〜１０００容量ｐｐｍであり、
前記残炭調整材を、前記低温流動性燃料油組成物中の１０％残留炭素分が０．２質量％以上になるように添加してなることを特徴とする低温流動性燃料油組成物。 A heavy oil base oil containing 10 to 70% by volume of desulfurized gas oil having a sulfur content of 10 mass ppm or less;
A residual carbon modifier comprising at least one hydrocarbon oil selected from atmospheric residual oil, vacuum residual oil, desulfurized residual oil, slurry oil, and extract;
A low-temperature fluid fuel oil composition comprising a fluidity improver,
The molecular weight of asphaltene in the residual coal modifier as measured by the vapor pressure osmometry method (VPO) is 5140-5690 , and the asphaltene content in the residual coal modifier is 1.53 as a compositional analysis value. 7.88% by mass, the number of aromatic rings (RN), which is an average structural parameter of the asphaltenes , is 150 or less, aromatic carbon (CA) is 200 to 300, and aliphatic carbon (CP) is 100. ~ 200,
The content of the fluidity improver is 100 to 1000 ppm by volume based on the fuel oil composition,
A low-temperature fluid fuel oil composition, wherein the residual coal modifier is added so that a 10% residual carbon content in the low-temperature fluid fuel oil composition is 0.2 mass% or more.
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