JP2007112824A - Process oil and rubber composition - Google Patents
Process oil and rubber composition Download PDFInfo
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- JP2007112824A JP2007112824A JP2005294088A JP2005294088A JP2007112824A JP 2007112824 A JP2007112824 A JP 2007112824A JP 2005294088 A JP2005294088 A JP 2005294088A JP 2005294088 A JP2005294088 A JP 2005294088A JP 2007112824 A JP2007112824 A JP 2007112824A
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- process oil
- rubber
- rubber composition
- weather resistance
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- 239000010734 process oil Substances 0.000 title claims abstract description 53
- 229920001971 elastomer Polymers 0.000 title claims abstract description 45
- 239000005060 rubber Substances 0.000 title claims abstract description 41
- 239000000203 mixture Substances 0.000 title claims abstract description 21
- 238000002835 absorbance Methods 0.000 claims abstract description 19
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 14
- 229920002943 EPDM rubber Polymers 0.000 claims description 6
- 239000000806 elastomer Substances 0.000 claims description 4
- 229920002397 thermoplastic olefin Polymers 0.000 claims description 3
- 230000001747 exhibiting effect Effects 0.000 abstract 1
- 230000000704 physical effect Effects 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 48
- 230000000052 comparative effect Effects 0.000 description 17
- 238000012360 testing method Methods 0.000 description 11
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 10
- 239000007789 gas Substances 0.000 description 10
- 238000004821 distillation Methods 0.000 description 9
- 239000003054 catalyst Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- 238000005292 vacuum distillation Methods 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000010779 crude oil Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 125000003118 aryl group Chemical group 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000004040 coloring Methods 0.000 description 5
- 239000001294 propane Substances 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 238000004517 catalytic hydrocracking Methods 0.000 description 4
- 238000004898 kneading Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 229920002725 thermoplastic elastomer Polymers 0.000 description 4
- 229910052721 tungsten Inorganic materials 0.000 description 4
- 230000004580 weight loss Effects 0.000 description 4
- 230000002411 adverse Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000007730 finishing process Methods 0.000 description 3
- 238000005984 hydrogenation reaction Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 244000043261 Hevea brasiliensis Species 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 239000010426 asphalt Substances 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 229920003052 natural elastomer Polymers 0.000 description 2
- 229920001194 natural rubber Polymers 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 229920003051 synthetic elastomer Polymers 0.000 description 2
- 239000005061 synthetic rubber Substances 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- 229920002633 Kraton (polymer) Polymers 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000004508 fractional distillation Methods 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 238000010058 rubber compounding Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L21/00—Compositions of unspecified rubbers
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M101/00—Lubricating compositions characterised by the base-material being a mineral or fatty oil
- C10M101/02—Petroleum fractions
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/01—Hydrocarbons
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M171/00—Lubricating compositions characterised by purely physical criteria, e.g. containing as base-material, thickener or additive, ingredients which are characterised exclusively by their numerically specified physical properties, i.e. containing ingredients which are physically well-defined but for which the chemical nature is either unspecified or only very vaguely indicated
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
- C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/08—Resistance to extreme temperature
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/20—Colour, e.g. dyes
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2040/00—Specified use or application for which the lubricating composition is intended
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
Description
本発明は、プロセスオイル、このプロセスオイルを天然ゴムや合成ゴムに適用したゴム組成物に関する。 The present invention relates to a process oil and a rubber composition in which the process oil is applied to natural rubber or synthetic rubber.
機械・電気製品等種々の分野で使用されるゴムには、機械的特性や加工性を向上させるため、一般にプロセスオイルが配合されている。このプロセスオイルは、天然ゴム、合成ゴム等のゴム基材に配合されるほか、熱可塑性樹脂の可塑剤や印刷用インキの構成成分、再生アスファルトの軟化剤等に使用する潤滑油や溶剤成分としても使用されている。 In general, process oil is blended in rubbers used in various fields such as machinery and electrical products in order to improve mechanical properties and processability. This process oil is blended with rubber base materials such as natural rubber and synthetic rubber, as a lubricant and solvent component used as a plasticizer for thermoplastic resins, components for printing ink, softener for recycled asphalt, etc. Has also been used.
一方、近年になって、自動車用内装材としてEPDM(エチレン−プロピレン−ジエンゴム)、オレフィン系熱可塑性エラストマー、あるいは、スチレン系熱可塑性エラストマーを用いたゴム組成物の需要が増加している。このようなゴム組成物を自動車用内装材として用いるには、耐熱性、耐候性が必要とされるため、一般に高純度の白色パラフィン系プロセスオイルが使用される。例えば、40℃における動粘度が95〜300mm2/sの範囲にあり、蒸留性状における5容量%流出温度が445℃以上であり、かつ、色相(セーボルト色)が+15以上であるプロセスオイルが知られている(例えば、特許文献1)。 On the other hand, in recent years, the demand for rubber compositions using EPDM (ethylene-propylene-diene rubber), olefin-based thermoplastic elastomers, or styrene-based thermoplastic elastomers as automobile interior materials is increasing. In order to use such a rubber composition as an automobile interior material, heat resistance and weather resistance are required, and therefore, a high-purity white paraffin process oil is generally used. For example, a process oil having a kinematic viscosity at 40 ° C. in the range of 95 to 300 mm 2 / s, a 5% by volume outflow temperature in distillation properties of 445 ° C. or higher, and a hue (Saebold color) of +15 or higher is known. (For example, Patent Document 1).
しかしながら、特許文献1のプロセスオイルは、耐候性が十分ではなく、例えば、自動車の内装材のように、直射日光に長時間さらされる用途に用いるとゴム材料が変色してしまうおそれがある。 However, the process oil of Patent Document 1 does not have sufficient weather resistance, and the rubber material may be discolored when used in applications that are exposed to direct sunlight for a long period of time, such as automobile interior materials.
そこで、本発明の目的は、従来のプロセスオイルと同等の特性を発揮することができ、かつ、耐熱性、耐候性に優れたプロセスオイル、及びこのプロセスオイルを用いたゴム組成物を提供することにある。 Accordingly, an object of the present invention is to provide a process oil that can exhibit characteristics equivalent to those of conventional process oils and that has excellent heat resistance and weather resistance, and a rubber composition using the process oil. It is in.
本発明のプロセスオイルは、下記(a)〜(c)の性状を有することを特徴とする。
(a)引火点 250℃以上
(b)セーボルト色 +28以上
(c)紫外吸光度(198nm) 1.7以下
The process oil of the present invention has the following properties (a) to (c).
(A) Flash point 250 ° C. or higher (b) Saybolt color +28 or higher (c) Ultraviolet absorbance (198 nm) 1.7 or lower
本発明のプロセスオイルによれば、引火点が250℃以上であるため、蒸発性が低く、例えばゴム基材に混練・配合したときに油蒸気の発生が少なく作業性に優れる。そして、紫外吸光度(198nm)が1.7以下であるので、ゴム組成物としたときに非常に優れた耐候性を有する。
ここで、本発明は、白色系プロセスオイルの耐候性が、オイル中の微量な芳香族分の濃度に依存することを発見したことにより生まれたものである。すなわち、紫外吸光度を目安としてこの微量な芳香族分を実質的に所定量以下とすることで耐候性が非常に向上した白色系プロセスオイルを得ることができたものである。
According to the process oil of the present invention, since the flash point is 250 ° C. or higher, the evaporability is low. For example, when kneaded and blended with a rubber base material, the generation of oil vapor is small and the workability is excellent. And since an ultraviolet light absorbency (198 nm) is 1.7 or less, when it is set as a rubber composition, it has the outstanding weather resistance.
Here, the present invention was born by discovering that the weather resistance of the white process oil depends on the concentration of a small amount of aromatic component in the oil. That is, a white process oil having a very improved weather resistance can be obtained by making the minute amount of aromatic component substantially equal to or less than a predetermined amount with reference to ultraviolet absorbance.
本発明のゴム組成物は、前記したプロセスオイルを配合したことを特徴とする。
本発明のゴム組成物によれば、前記した性状を有するプロセスオイルを用いているため、ゴム基材に混練・配合したときに油蒸気の発生が少なく作業性に優れる。そして、セーボルト色が+28以上であり、紫外吸光度(198nm)が1.7以下であるので、ゴム組成物としたときであっても十分な耐候性を有する。
The rubber composition of the present invention is characterized by blending the process oil described above.
According to the rubber composition of the present invention, since the process oil having the above-mentioned properties is used, the generation of oil vapor is small and the workability is excellent when kneaded and blended with the rubber base material. And since Saybolt color is +28 or more and ultraviolet light absorbency (198 nm) is 1.7 or less, even when it is set as a rubber composition, it has sufficient weather resistance.
本発明のゴム組成物は、ゴム基材がEPDM、オレフィン系熱可塑性エラストマー、及びスチレン系エラストマーから選ばれる少なくとも一種であることが好ましい。
この構成によれば、EPDM、オレフィン系熱可塑性エラストマー、及びスチレン系エラストマーといった汎用性の高いゴム基材について、耐候性を高めたゴム組成物とすることにより、特に自動車内装材分野における技術的価値を一層高めることができる。
In the rubber composition of the present invention, the rubber substrate is preferably at least one selected from EPDM, olefinic thermoplastic elastomers, and styrene elastomers.
According to this configuration, the technical value particularly in the automotive interior material field can be obtained by using a rubber composition having high weather resistance for rubber base materials having high versatility such as EPDM, olefin-based thermoplastic elastomer, and styrene-based elastomer. Can be further enhanced.
本発明のプロセスオイルは、下記(a)〜(c)の性状を有するものである。
(a)引火点 250℃以上
(b)セ−ボルト色 +28以上
(c)紫外吸光度(198nm) 1.7以下
The process oil of the present invention has the following properties (a) to (c).
(A) Flash point 250 ° C. or higher (b) Cevolt color +28 or higher (c) Ultraviolet absorbance (198 nm) 1.7 or lower
(a)引火点:
本発明のプロセスオイルは、引火点が250℃以上であり、260℃以上であることが好ましい。引火点が250℃よりも低いと、ゴム基材との混練時に蒸発量が多くなり、作業性が悪くなる。
なお、プロセスオイルの引火点は、ASTM−D92に準拠して測定すればよい。
(A) Flash point:
The process oil of the present invention has a flash point of 250 ° C. or higher, and preferably 260 ° C. or higher. When the flash point is lower than 250 ° C., the amount of evaporation increases during kneading with the rubber base material, resulting in poor workability.
Note that the flash point of the process oil may be measured according to ASTM-D92.
(b)セ−ボルト色:
本発明のプロセスオイルは、セ−ボルト色が+28以上であり、+30以上であることが好ましい。セ−ボルト色が+28未満であると、芳香族分の濃度の増加により、耐候性に悪影響を及ぼす。
なお、セ−ボルト色はASTM D 1500に準拠して測定すればよい。
(B) Sebolt color:
The process oil of the present invention has a Sebolt color of +28 or more, preferably +30 or more. When the Sebolt color is less than +28, the weather resistance is adversely affected due to an increase in the concentration of aromatic components.
In addition, what is necessary is just to measure a Sebolt color based on ASTMD1500.
(c)紫外吸光度(198nm):
本発明のプロセスオイルは、紫外吸光度が1.7以下であり、1.6以下であることが好ましい。紫外吸光度が1.7を越えると、耐候性に悪影響を与える芳香族分が多いことから、耐候性が悪化する。
なお、紫外吸光度は、JIS K 0115に準拠して測定すればよい。具体的には、試料2.00グラムをヘキサンで希釈して50mlにしたものを1mmセルでヘキサンをブランクとして198nmの波長で測定したときの吸光度である。
(C) UV absorbance (198 nm):
The process oil of the present invention has an ultraviolet absorbance of 1.7 or less and preferably 1.6 or less. If the ultraviolet absorbance exceeds 1.7, the weather resistance deteriorates because there are many aromatic components that adversely affect the weather resistance.
The ultraviolet absorbance may be measured according to JIS K 0115. Specifically, it is the absorbance when 2.00 grams of a sample diluted to 50 ml with hexane was measured at a wavelength of 198 nm using a 1 mm cell with hexane as a blank.
以下に、前記した本発明のプロセスオイルを製造する手段の一例について詳細に説明する。
〔減圧軽油の製造(減圧軽油製造工程)〕
減圧軽油製造工程では、原油を常圧蒸留した後の常圧蒸留残渣油を減圧蒸留して減圧軽油を得る。
ここで、原油を常圧蒸留するには、公知の常圧蒸留装置および蒸留条件で行うことができる。例えば、精製対象となるパラフィン系原油やナフテン系原油等からなる原油を、加熱炉等で約350℃程度に熱せられたのちに常圧蒸留塔に送り出し、常圧蒸留塔内部で石油蒸気とされ、冷却後、沸点の低いものから高いものへと順に分離する。
Hereinafter, an example of means for producing the process oil of the present invention described above will be described in detail.
[Production of vacuum gas oil (vacuum gas oil production process)]
In the vacuum gas oil production process, a vacuum distillation oil is obtained by vacuum distillation of the atmospheric distillation residue after the crude oil is distilled at atmospheric pressure.
Here, the crude oil can be distilled at atmospheric pressure using a known atmospheric distillation apparatus and distillation conditions. For example, crude oil composed of paraffinic crude oil or naphthenic crude oil to be refined is heated to about 350 ° C. in a heating furnace or the like and then sent to an atmospheric distillation tower to be converted into petroleum vapor inside the atmospheric distillation tower. After cooling, the product is separated in order from low to high boiling point.
次に、得られた常圧残油に対して、減圧下における蒸留(減圧蒸留)をさらに実施する。減圧蒸留を行うには、従来公知の減圧蒸留装置および運転条件で行えばよく、かかる減圧蒸留により減圧ナフサ、減圧軽油、減圧残渣油の各留分に分留されることになり、この中から減圧軽油を得るようにすればよい。 Next, distillation under reduced pressure (vacuum distillation) is further performed on the obtained atmospheric residue. In order to carry out the vacuum distillation, it may be carried out with a conventionally known vacuum distillation apparatus and operating conditions, and by such vacuum distillation, fractionation is carried out into each fraction of vacuum naphtha, vacuum gas oil, and vacuum residue oil. What is necessary is just to obtain a vacuum gas oil.
〔脱れき油の製造(脱れき油製造工程)〕
前記した工程で得られた減圧残渣油を、例えば液化プロパン(または液化プロパン/ブタン混合溶剤)等の溶剤を用いて、油分(脱れき油)とアスファルト分とに分離する。液化プロパンによる脱れきは、例えば、減圧残渣油に対して4.5〜6倍の液化プロパンを混合して、抽出温度を塔頂/塔底=85〜95℃/60〜75℃として脱れき油を抽出すればよい。
[Manufacture of desiccated oil (process for manufacturing desorbed oil)]
The reduced-pressure residual oil obtained in the above-described step is separated into an oil (desorbed oil) and an asphalt using a solvent such as liquefied propane (or liquefied propane / butane mixed solvent). The deliquescent by liquefied propane is, for example, mixed with 4.5 to 6 times liquefied propane to the vacuum residue oil, and the extraction temperature is tower top / column bottom = 85 to 95 ° C./60 to 75 ° C. What is necessary is just to extract oil.
〔水素化分解工程〕
上述の各工程で得られた減圧軽油、脱れき油、あるいは、これらの混合油は、以下の条件で水素化分解される。
触媒としては、アルミナやシリカを担体としてNi、Mo、W、及びCoの一種又は二種以上を担持したもの、あるいはゼオライトにPt、Pdなどの貴金属を担持したものが好適に用いられる。
好ましい分解温度は、300〜450℃であり、より好ましくは350〜400℃である。好ましい水素/原料油比は、500〜10000Nm3/KLであり、より好ましくは800〜2000Nm3/KLである。好ましいLHSVは、0.1〜10Hr−1であり、より好ましくは0.5〜2.0Hr−1である。好ましい水素圧力は、10〜25MPaであり、より好ましくは15〜20MPaである。
[Hydrolysis process]
The vacuum gas oil, de-oiled oil, or mixed oil obtained in each of the above steps is hydrocracked under the following conditions.
As the catalyst, a catalyst in which one or more of Ni, Mo, W, and Co are supported using alumina or silica as a carrier, or a catalyst in which a noble metal such as Pt or Pd is supported on zeolite is preferably used.
A preferable decomposition temperature is 300 to 450 ° C, more preferably 350 to 400 ° C. Preferred hydrogenation / feedstock ratio is 500~10000Nm 3 / KL, more preferably 800~2000Nm 3 / KL. A preferred LHSV is 0.1 to 10 Hr −1 , more preferably 0.5 to 2.0 Hr −1 . A preferable hydrogen pressure is 10 to 25 MPa, and more preferably 15 to 20 MPa.
〔水素化仕上工程〕
上述の水素化分解工程で得られた水素化分解油は、減圧蒸留にて所定の粘度を有する2種以上の留出油に分けられる。そして、以下のような条件でさらに精製されて芳香族分の濃度が非常に低い精製油となる。
触媒としては、アルミナやシリカを担体としてNi、Mo、W、及びCoの一種又は二種以上を担持したもの、あるいはゼオライトにPt、Pdなどの貴金属を担持したものが好適に用いられる。
[Hydrogen finishing process]
The hydrocracked oil obtained in the above hydrocracking step is divided into two or more distillate oils having a predetermined viscosity by vacuum distillation. And it refine | purifies further on the following conditions, and becomes a refined oil with very low concentration of aromatics.
As the catalyst, a catalyst in which one or more of Ni, Mo, W, and Co are supported using alumina or silica as a carrier, or a catalyst in which a noble metal such as Pt or Pd is supported on zeolite is preferably used.
好ましい仕上げ温度は、200〜350℃であり、より好ましくは220〜320℃である。好ましい水素/原料油比は、500〜10000Nm3/KLであり、より好ましくは500〜1000Nm3/KLである。好ましいLHSVは、0.1〜10Hr−1であり、より好ましくは0.5〜2.0Hr−1である。好ましい水素圧力は、10〜25MPaであり、より好ましくは15〜20MPaである。このような水素化仕上げの条件により、セーボルト色及び紫外吸光度を調節することができる。 A preferable finishing temperature is 200 to 350 ° C, and more preferably 220 to 320 ° C. A preferable hydrogen / feed oil ratio is 500 to 10000 Nm 3 / KL, more preferably 500 to 1000 Nm 3 / KL. A preferred LHSV is 0.1 to 10 Hr −1 , more preferably 0.5 to 2.0 Hr −1 . A preferable hydrogen pressure is 10 to 25 MPa, and more preferably 15 to 20 MPa. The Saebold color and ultraviolet absorbance can be adjusted according to the conditions of such hydrofinishing.
上述の水素化仕上げ工程で得られた生成油は、プロセスオイルとして用いることもできるが、必要に応じて減圧蒸留されて、軽質分が除去され、引火点が250℃以上になるように調整される。 The product oil obtained in the above hydrofinishing step can be used as a process oil, but if necessary, it is distilled under reduced pressure to remove light components and to adjust the flash point to 250 ° C or higher. The
このようにして得られた本発明のプロセスオイルは、前記した(a)〜(c)の性状を有することにより、蒸発性が低く、耐候性に優れるプロセスオイルとなる。
このプロセスオイルは、ゴム基材であるEPDM、オレフィン系熱可塑性エラストマー、及びスチレン系エラストマーから選ばれる少なくとも一種に配合することにより、各種ゴム組成物を好適に提供することとなる。また、得られたゴム組成物は、耐候性が要求される自動車用内装材として特に好適に使用される。
The process oil of the present invention thus obtained has the properties (a) to (c) described above, so that it becomes a process oil having low evaporability and excellent weather resistance.
This process oil suitably provides various rubber compositions by blending with at least one selected from EPDM, which is a rubber base material, olefinic thermoplastic elastomer, and styrene elastomer. Further, the obtained rubber composition is particularly suitably used as an automobile interior material that requires weather resistance.
ここで、本発明のプロセスオイルを用いてゴム(ゴム組成物)を製造する場合にあっては、例えば、ゴム成分100重量部に対して、本発明のプロセスオイルを10〜50重量部、好ましくは20〜40重量部配合して製造すればよい。
また、ゴム組成物を製造する場合には、本発明のプロセスオイルやゴム成分のほかに、カーボンブラック、シリカ等の補強剤、加硫剤、加硫促進剤、充填剤、ワックス類等の劣化防止剤、本発明のゴム配合油以外の軟化剤または可塑剤等の通常ゴム業界で用いられるものを適宜配合してもよい。
Here, in the case of producing rubber (rubber composition) using the process oil of the present invention, for example, the process oil of the present invention is preferably 10 to 50 parts by weight, preferably 100 parts by weight of the rubber component. May be produced by blending 20 to 40 parts by weight.
In addition, when producing a rubber composition, in addition to the process oil and rubber component of the present invention, carbon black, silica and other reinforcing agents, vulcanizing agents, vulcanization accelerators, fillers, waxes, etc. Those usually used in the rubber industry such as an inhibitor and a softener or a plasticizer other than the rubber compounding oil of the present invention may be appropriately blended.
なお、以上説明した態様は、本発明の一態様を示したものであって、本発明は、前記した実施形態に限定されるものではなく、本発明の目的及び効果を達成できる範囲内での変形や改良が、本発明の内容に含まれるものであることはいうまでもない。また、本発明を実施する際における具体的な構造及び形状等は、本発明の目的及び効果を達成できる範囲内において、他の構造や形状等としてもよい。
例えば、当該(a)〜(c)の性状を有するのであれば、プロセスオイルを得る手段は適宜調整しても問題はない。
The aspect described above shows one aspect of the present invention, and the present invention is not limited to the above-described embodiment, and is within the scope of achieving the object and effect of the present invention. Needless to say, modifications and improvements are included in the content of the present invention. In addition, the specific structure, shape, and the like when implementing the present invention may be other structures, shapes, and the like as long as the objects and effects of the present invention can be achieved.
For example, as long as it has the properties (a) to (c), there is no problem even if the means for obtaining the process oil is appropriately adjusted.
以下、実施例および比較例を挙げて、本発明をより具体的に説明するが、本発明はこれらの実施例等に何ら制約されるものではない。
[実施例1、2]
(減圧軽油製造工程)
中東系原油を常圧蒸留して灯油、軽油などの燃料油を取り出し、蒸留塔底部から流出した常圧残渣油に対し、さらに減圧蒸留して減圧軽油を得た。
EXAMPLES Hereinafter, although an Example and a comparative example are given and this invention is demonstrated more concretely, this invention is not restrict | limited at all by these Examples.
[Examples 1 and 2]
(Depressurized gas oil production process)
Middle-east crude oil was subjected to atmospheric distillation to remove fuel oils such as kerosene and light oil, and the atmospheric residue obtained from the bottom of the distillation tower was further distilled under reduced pressure to obtain vacuum gas oil.
(脱れき工程)
上述の工程において、減圧軽油などを分留した後の減圧残渣油に対し、プロパンを溶剤として脱れき油を得た。
(Escape process)
In the above-mentioned process, devolatilized oil was obtained using propane as a solvent for the vacuum residue oil after fractional distillation of vacuum gas oil and the like.
(混合工程)
上述の各工程で得られた減圧軽油と脱れき油とを60/40の容量比で混合して混合油を得た。
(水素化分解工程)
アルミナにNiとWを担持した触媒を用いて、反応圧力が200Kg/cm2、反応温度が384℃、LHSVが1.0Hr−1、水素/混合油の比が1000Nm3/KLの条件で混合油の水素化分解を行った。水素化分解で得られた生成油を減圧蒸留して抽出により4種類の粘度留分に分留し、重質留分である40℃粘度94mm2/sの留分と430mm2/sの留分を次の水素化仕上工程に送った。
(Mixing process)
The vacuum gas oil obtained in each of the above-described steps and the exfoliated oil were mixed at a volume ratio of 60/40 to obtain a mixed oil.
(Hydrolysis process)
Using a catalyst in which Ni and W are supported on alumina, the reaction pressure is 200 kg / cm 2 , the reaction temperature is 384 ° C., the LHSV is 1.0 Hr −1 , and the hydrogen / mixed oil ratio is 1000 Nm 3 / KL. Oil hydrocracking was performed. The product oil obtained by hydrocracking is distilled under reduced pressure and fractionated into four types of viscosity fractions by extraction, and the heavy fractions are a 40 ° C. viscosity fraction of 94 mm 2 / s and a 430 mm 2 / s fraction. The minute was sent to the next hydrofinishing step.
(水素化仕上工程)
前記した2種類の留分に対し、アルミナにNiとWを担持した触媒を用い、生成油の紫外吸光度が1.7以下となるような反応温度と、反応圧力が20MPa、LHSVが0.5Hr−1、水素/混合油の比が1000Nm3/KLの条件で水素化仕上げを行った。最終的に、40℃粘度94mm2/sの留分からは、40℃粘度92mm2/sの生成油が得られ、40℃粘度430mm2/sの留分からは、40℃粘度380mm2/sの生成油が得られた。これらを各々実施例1,2のプロセスオイルとした。
(Hydrogen finishing process)
For the above-mentioned two types of fractions, a catalyst in which Ni and W are supported on alumina is used, the reaction temperature at which the ultraviolet absorbance of the product oil is 1.7 or less, the reaction pressure is 20 MPa, and the LHSV is 0.5 Hr. The hydrogenation finish was performed under the conditions of −1 , hydrogen / mixed oil ratio of 1000 Nm 3 / KL. Finally, a product oil having a viscosity of 92 mm 2 / s at 40 ° C. is obtained from a fraction having a viscosity of 94 mm 2 / s at 40 ° C., and a product having a viscosity of 380 mm 2 / s at 40 ° C. is obtained from a fraction having a viscosity of 430 mm 2 / s at 40 ° C. A product oil was obtained. These were used as the process oils of Examples 1 and 2, respectively.
[比較例1、2]
実施例1、2の水素化仕上工程において、反応温度を10℃低くした以外は同じ条件で水素化仕上げを行った。その結果、紫外吸光度が1.8と2.0の生成油を得た。これらを、各々比較例1、2のプロセスオイルとした。
[Comparative Examples 1 and 2]
In the hydrofinishing steps of Examples 1 and 2, hydrofinishing was performed under the same conditions except that the reaction temperature was lowered by 10 ° C. As a result, oils having ultraviolet absorbances of 1.8 and 2.0 were obtained. These were used as process oils of Comparative Examples 1 and 2, respectively.
[比較例3]
実施例2の水素化仕上工程により得られた高粘度生成油(40℃粘度 380mm2/
s)に対して、40℃粘度が32mm2/sの留分(実施例1で得られた4種の粘度留分のうちの軽質留分)を水素化仕上げして紫外吸光度1.2としたものを混合して40℃粘度が95mm2/sの生成油を得た。これを比較例3のプロセスオイルとした。
[Comparative Example 3]
High viscosity product oil obtained by the hydrogenation finishing process of Example 2 (40 ° C. viscosity 380 mm 2 /
s), a fraction having a viscosity of 40 mm at 32 mm 2 / s (light fraction of the four types of viscosity fractions obtained in Example 1) was hydrofinished to obtain an ultraviolet absorbance of 1.2. Were mixed to obtain a product oil having a viscosity of 95 mm 2 / s at 40 ° C. This was used as the process oil of Comparative Example 3.
[比較例4]
実施例2の水素化分解工程により得られた高粘度生成油(430mm2/s)を硫酸処理及び白土処理により精製し、セーボルト色+30の白色生成油を得た。これを、比較例4のプロセスオイルとした。
[Comparative Example 4]
The high-viscosity product oil (430 mm 2 / s) obtained by the hydrocracking process of Example 2 was purified by a sulfuric acid treatment and a clay treatment to obtain a white product oil of Saybolt +30. This was used as the process oil of Comparative Example 4.
[比較例5]
実施例1の水素化仕上工程において、40℃粘度が94mm2/sの留分を、反応温度を5℃低くした以外は同じ条件で水素化仕上げを行った。その結果、紫外吸光度が1.79の生成油を得た。これを、比較例5のプロセスオイルとした。
[Comparative Example 5]
In the hydrofinishing step of Example 1, hydrofinishing was performed under the same conditions except that the fraction having a viscosity of 94 mm 2 / s at 40 ° C. was lowered by 5 ° C. As a result, a product oil having an ultraviolet absorbance of 1.79 was obtained. This was used as the process oil of Comparative Example 5.
[試験例1]
実施例1、2及び比較例1〜4のプロセスオイルについて耐候性試験を行った後のセーボルト色を測定した。さらに、各プロセスオイルの蒸発性についても評価を行った。表1に、各プロセスオイルの性状とともに結果を示す。なお、これらの試験・評価方法は下記の通りである。
[Test Example 1]
The Saybolt color after the weather resistance test was performed on the process oils of Examples 1 and 2 and Comparative Examples 1 to 4 was measured. Furthermore, the evaporability of each process oil was also evaluated. Table 1 shows the results together with the properties of each process oil. These test / evaluation methods are as follows.
(耐候性試験)
65℃の温度で、キセノンランプにより8時間照射して、プロセスオイルの着色の有無(セーボルト色)を測定した。なお、この時間は、夏場一ヶ月間戸外に晒した条件に相当する。耐候性に優れたプロセスオイルはほとんど着色が認められないが、耐候性が悪いと数時間で著しい着色が認められる。
(Weather resistance test)
Irradiation with a xenon lamp at a temperature of 65 ° C. for 8 hours was performed to determine whether the process oil was colored (Saebold color). This time corresponds to the condition of being exposed outdoors for one month in summer. The process oil having excellent weather resistance is hardly colored, but if the weather resistance is poor, significant coloration is recognized in several hours.
(蒸発性)
JIS K 2540「石油製品―潤滑油―熱安定度試験方法」に準拠して測定した。具体的には、試料のプロセスオイル10gを所定の容器に入れ、200℃で1時間加熱し、その減量により以下の基準で評価した。
○:減量が0.2質量%以下であるもの
△:減量が0.2質量%を越え、0.3質量%以下であるもの
×:減量が0.3質量%を越えるもの
(Evaporation)
Measured according to JIS K 2540 “Petroleum products—lubricating oil—thermal stability test method”. Specifically, 10 g of sample process oil was put in a predetermined container, heated at 200 ° C. for 1 hour, and evaluated according to the following criteria based on the weight loss.
○: Weight loss is 0.2% by mass or less
Δ: Weight loss exceeds 0.2% by mass and is 0.3% by mass or less
X: Weight loss exceeds 0.3% by mass
(結 果)
表1より、実施例1、2のプロセスオイルは、引火点が高いため蒸発性に優れる。また、紫外吸光度が1.7以下であり、耐候性に悪影響を与える芳香族分が少ないため、耐候性試験後のセーボルト色がいずれも無色であり、耐候性に優れていることがわかる。
一方、比較例1、2、4は、いずれも紫外吸光度が1.7を越えており、耐候性が悪いため、耐候性試験後にはいずれも着色が認められた。特に、比較例4は、紫外吸光度が10以上と非常に大きいため、着色が著しい。比較例3は、着色はないものの、引火点が250℃未満であり、蒸発性が悪く(大きく)、ゴムへの混練時に作業性が悪い。比較例5は、セーボルト色は+30であるが、紫外吸光度が1.7を越えているため、耐候性試験後に着色が認められた。
(Result)
From Table 1, the process oils of Examples 1 and 2 are excellent in evaporability because of high flash point. Further, since the ultraviolet absorbance is 1.7 or less and the aromatic content that adversely affects the weather resistance is small, the Saybolt color after the weather resistance test is all colorless, indicating that the weather resistance is excellent.
On the other hand, since Comparative Examples 1, 2, and 4 all had an ultraviolet absorbance exceeding 1.7 and poor weather resistance, coloring was observed after the weather resistance test. In particular, since Comparative Example 4 has a very high ultraviolet absorbance of 10 or more, coloring is remarkable. In Comparative Example 3, although there is no coloring, the flash point is less than 250 ° C., the evaporation property is poor (large), and the workability is poor when kneading into rubber. In Comparative Example 5, the Saybolt color was +30, but since the ultraviolet absorbance exceeded 1.7, coloring was observed after the weather resistance test.
[試験例2]
前記の実施例1、2及び比較例1〜5により得られたプロセスオイルを用いて、以下のようにスチレン系ゴムを製造した。
スチレン系熱可塑性エラストマー(シェルジャパン社製「KratonG 1652」)100質量部と、プロセスオイル70質量部とを混練し、2本ロールでシート練りしたのち、200℃で金型成形を行い、厚さ2mmのシートを得た。
このシートを用いて、試験例1と同様の条件で2通り(照射時間:24時間及び78時間)の耐候性試験を行い、ゴムの変色(着色)の有無を目視により以下の基準で評価した。結果を表2に示す。
◎:着色無し
○:微かに着色
△:黄色に変色
×:褐色に変色
[Test Example 2]
Using the process oils obtained in Examples 1 and 2 and Comparative Examples 1 to 5, styrene rubber was produced as follows.
After kneading 100 parts by mass of styrene thermoplastic elastomer (“Kraton G 1652” manufactured by Shell Japan Co., Ltd.) and 70 parts by mass of process oil and kneading the sheet with two rolls, the mold is molded at 200 ° C. A 2 mm sheet was obtained.
Using this sheet, two kinds of weather resistance tests (irradiation time: 24 hours and 78 hours) were performed under the same conditions as in Test Example 1, and the presence or absence of discoloration (coloring) of the rubber was visually evaluated according to the following criteria. . The results are shown in Table 2.
◎: Not colored ○: Slightly colored △: Discolored to yellow ×: Discolored to brown
(結 果)
表2より、実施例1、2では、78時間の耐候性試験を行っても、ゴムにほとんど着色がないことがわかる。一方、比較例1、2、5では、いずれのゴムも、78時間後には黄色に変色していた。特に比較例4のゴムでは変色が著しいため、耐候性試験を24時間で打ち切った。
(Result)
From Table 2, it can be seen that in Examples 1 and 2, the rubber is hardly colored even after a 78-hour weather resistance test. On the other hand, in Comparative Examples 1, 2, and 5, all the rubbers turned yellow after 78 hours. In particular, since the discoloration was remarkable in the rubber of Comparative Example 4, the weather resistance test was terminated in 24 hours.
本発明のプロセスオイルは、自動車内装材に用いられるゴム組成物のプロセスオイルとして好適に使用することができる。 The process oil of the present invention can be suitably used as a process oil for rubber compositions used for automobile interior materials.
Claims (3)
(a)引火点 250℃以上
(b)セーボルト色 +28以上
(c)紫外吸光度(198nm) 1.7以下 A process oil having the following properties (a) to (c):
(A) Flash point 250 ° C. or higher (b) Saybolt color +28 or higher (c) Ultraviolet absorbance (198 nm) 1.7 or lower
該ゴム組成物のゴム基材がEPDM、オレフィン系熱可塑性エラストマー、及びスチレン系エラストマーから選ばれる少なくとも一種であることを特徴とするゴム組成物。 The rubber composition according to claim 2,
A rubber composition, wherein the rubber base material of the rubber composition is at least one selected from EPDM, an olefinic thermoplastic elastomer, and a styrene elastomer.
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JP2010047682A (en) * | 2008-08-21 | 2010-03-04 | Japan Energy Corp | Manufacturing method of rubber process oil |
WO2013141123A1 (en) | 2012-03-21 | 2013-09-26 | 出光興産株式会社 | Process oil and rubber composition |
WO2023101031A1 (en) * | 2021-12-03 | 2023-06-08 | 出光興産株式会社 | Mineral oil, and process oil and grease |
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CN102796607B (en) * | 2011-05-27 | 2014-11-12 | 王文兵 | Device and method for regenerating phosphate ester fire-resistant oil |
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CN107108777B (en) * | 2014-11-12 | 2021-02-05 | 埃克森美孚化学专利公司 | Purification of plasticizers and their use in polymer production processes and apparatus |
KR20230155684A (en) | 2022-05-04 | 2023-11-13 | 디엘케미칼 주식회사 | Process oil for rubber processing, and rubber composition comprising the same |
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JP2010047682A (en) * | 2008-08-21 | 2010-03-04 | Japan Energy Corp | Manufacturing method of rubber process oil |
WO2013141123A1 (en) | 2012-03-21 | 2013-09-26 | 出光興産株式会社 | Process oil and rubber composition |
WO2023101031A1 (en) * | 2021-12-03 | 2023-06-08 | 出光興産株式会社 | Mineral oil, and process oil and grease |
Also Published As
Publication number | Publication date |
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KR101281975B1 (en) | 2013-07-03 |
KR20080063318A (en) | 2008-07-03 |
TW200712130A (en) | 2007-04-01 |
JP4850472B2 (en) | 2012-01-11 |
WO2007034598A1 (en) | 2007-03-29 |
CN101268137B (en) | 2011-07-13 |
TWI444434B (en) | 2014-07-11 |
CN101268137A (en) | 2008-09-17 |
KR20130041386A (en) | 2013-04-24 |
KR101363718B1 (en) | 2014-02-14 |
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