KR100721600B1 - Composition of grease prodnced from distillated residuum - Google Patents

Composition of grease prodnced from distillated residuum Download PDF

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Publication number
KR100721600B1
KR100721600B1 KR1020070003691A KR20070003691A KR100721600B1 KR 100721600 B1 KR100721600 B1 KR 100721600B1 KR 1020070003691 A KR1020070003691 A KR 1020070003691A KR 20070003691 A KR20070003691 A KR 20070003691A KR 100721600 B1 KR100721600 B1 KR 100721600B1
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South Korea
Prior art keywords
grease composition
thickener
biodiesel
grease
oil
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KR1020070003691A
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Korean (ko)
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김광순
이문식
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주식회사 한국하우톤
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Priority to KR1020070003691A priority Critical patent/KR100721600B1/en
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Publication of KR100721600B1 publication Critical patent/KR100721600B1/en
Priority to JP2007242133A priority patent/JP4776603B2/en
Priority to US11/901,878 priority patent/US8481466B2/en
Priority to AT07118302T priority patent/ATE477317T1/en
Priority to ES07118302T priority patent/ES2352982T3/en
Priority to EP07118302A priority patent/EP1944352B1/en
Priority to DE602007008350T priority patent/DE602007008350D1/en

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    • 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
    • C10M101/04—Fatty oil fractions
    • 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
    • C10M109/00—Lubricating compositions characterised by the base-material being a compound of unknown or incompletely defined constitution
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M113/00—Lubricating compositions characterised by the thickening agent being an inorganic material
    • C10M113/08—Metal compounds
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • 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
    • C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/10—Compounds containing silicon
    • C10M2201/102—Silicates
    • C10M2201/103—Clays; Mica; Zeolites
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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
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    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
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    • C10M2207/1265—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic used as thickening agent
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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/127—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids polycarboxylic
    • C10M2207/1276—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids polycarboxylic used as thickening agent
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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/128—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
    • C10M2207/1285—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof used as thickening agents
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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
    • C10M2207/281—Esters of (cyclo)aliphatic monocarboxylic acids
    • C10M2207/2815—Esters of (cyclo)aliphatic monocarboxylic acids used as base material
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
    • C10M2207/287—Partial esters
    • C10M2207/289—Partial esters containing free hydroxy groups
    • C10M2207/2895—Partial esters containing free hydroxy groups used as base material
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/40—Fatty vegetable or animal oils
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/40—Fatty vegetable or animal oils
    • C10M2207/401—Fatty vegetable or animal oils used as base material
    • 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
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/08—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type
    • C10M2209/084—Acrylate; Methacrylate
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    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
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    • C10M2215/223—Five-membered rings containing nitrogen and carbon only
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    • C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
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    • C10N2010/02—Groups 1 or 11
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    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
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Abstract

A grease composition using lubricating base oil that is biodegradable by microorganisms in nature and has an affinity to the human body is provided. More particularly, a distillation residue secondarily generated in production of biodiesel from vegetable oil (soybean oil and canola oil) is used as the lubricating base oil. The grease composition is produced by adding 1 to 20wt% of additives to 100 to 95wt% of distillation residues, which is generated in production of biodiesel, and 1 to 30wt% of thickeners.

Description

바이오디젤 생산 시 생성되는 증류 잔류물을 이용한 생분해성 그리스 조성물{Composition of Grease prodnced from distillated Residuum}Biodegradable Grease Composition Using Distillation Residue in Biodiesel Production {Composition of Grease prodnced from distillated Residuum}

본 발명은 일반 산업에서 사용되어지는 기계나 설비, 장비의 윤활작용을 하는 그리스에 관한 것으로, 더욱 상세하게는 대두유 및 채종유의 탈취지방산을 이용한 바이오디젤 생산 시 생성되는 최종 잔류물을 10 ∼ 95 중량％ 기유로 사용하여 제조되는 그리스 조성물에 관한 것이다.The present invention relates to a grease for lubricating machinery, equipment and equipment used in the general industry, and more specifically, 10 to 95 weight of the final residue produced during biodiesel production using deodorized fatty acids of soybean oil and rapeseed oil. It is related with the grease composition manufactured using% base oil.

〈 일반적인 그리스의 구성성분 및 분류〉<Composition and Classification of General Greases>

Figure 112007500343354-pat00001
Figure 112007500343354-pat00001

윤활작용을 하는 그리스의 종류는 증주제에 따라 Ca, Na, Li, Al, Ba, Complex등의 금속염 비누계 그리스와 Bentone, Silica, Urea, Graphite, PTFE등과 같은 비비누계 그리스로 구분되며 기유의 종류에 따라서도 광유계 그리스, 합성유계 그리스 등으로 구분된다.Lubricant greases are classified into metal salt soap greases such as Ca, Na, Li, Al, Ba, and Complex, and soap-based greases such as Bentone, Silica, Urea, Graphite, and PTFE, depending on the type of thickener. Therefore, it is divided into mineral oil grease, synthetic oil grease and the like.

그리스의 기능은 윤활부위의 부품과 부품간의 마찰을 줄이고, 마멸과 마모를 감소시키며, 윤활표면의 특성을 좋게 하고, 금속 표면에 유착되거나 녹아 붙는 것을 줄이며, 발생되는 열을 제거하여 열에 의한 변형을 방지하고, 윤활작동 시에 발생되는 이물질 혼입방지와 밀봉효과를 극대화하여 설비와 윤활부품의 성능과 수명을 보존하는 것이다. 이러한 그리스의 기유로서 통상 원유 정제공정 중 가장 마지 막 공정에서 생산된 석유계 탄화수소 윤활기유를 주로 사용하여 왔다. 그러나, 상기와 같이 석유계 탄화수소를 사용하는 그리스는 환경손상을 가져올 수 있으며, 상기와 같은 그리스를 사용하는 사람의 건강을 위협할 수 있다.The grease function reduces friction between parts and parts of the lubrication area, reduces wear and wear, improves lubrication surface properties, reduces adhesion and melting of metal surfaces, and removes heat generated to remove heat deformation. It is to prevent the mixing of foreign matters generated during lubrication operation and to maximize the sealing effect, thus preserving the performance and life of the equipment and lubrication parts. As such grease base oils, petroleum hydrocarbon lubricating base oils produced in the last step of the crude oil refining process have been mainly used. However, grease using petroleum hydrocarbons as described above may cause environmental damage and may threaten the health of the person using such grease.

최근 전 세계적으로 환경보호의 중요성 및 작업자들에 대한 건강과 안전에 대한 관심이 늘어감에 따라 그리스 중에서 탄화수소계 윤활기유를 대체할 환경수용성 윤활기유에 대한 연구가 북미나 서유럽 등에서는 이미 국가적인 차원에서 진행되고 있다.Recently, as the importance of environmental protection and the interest in health and safety for workers have increased all over the world, studies on water-soluble lubricating base oils to replace hydrocarbon-based lubricating base oils in Greece have already been carried out at the national level in North America and Western Europe. It's going on.

본 발명은 이러한 추세에 맞춰 그리스 조성물의 유효성분인 윤활기유를 환경친화형 윤활기유로 바이오디젤 생산시 생성되는 증류 잔유물을 이용한 그리스 조성물을 개발하는 것이다.The present invention is to develop a grease composition using a distillation residue produced in the production of biodiesel from the lubricant base oil as an active ingredient of the grease composition in accordance with this trend.

바이오디젤이란 식물이나 동물에 있는 지방성분을 경유와 비슷한 물성을 갖도록 가공하여 경유를 대체하거나 경유에 혼합하여 디젤엔진에 사용할 수 있도록 만든 대체에너지이다. 바이오디젤은 일반적으로 대두유나 유채유등 식물성유지와 알코올(보통 메탄올)을 반응시켜 만든 지방산 메틸 에스테르를 말하며 순도가 95％이상인 것을 지칭한다. (산자부 고시 제2000-57호)Biodiesel is an alternative energy made by processing fat components in plants and animals to have properties similar to those of diesel, replacing diesel or mixing them with diesel. Biodiesel generally refers to fatty acid methyl ester made by reacting vegetable oil such as soybean oil or rapeseed oil with alcohol (usually methanol), and refers to a purity of 95% or more. (Ministry of Commerce, Industry and Energy Notice No. 2000-57)

위에서 식물성 유지는 물에 녹지 않는 소수성기를 포함한 화합물로서 일반적으로 다음과 같은 화학적 구조식으로 표시되는 Triglycerides로 구성되어 있다.The vegetable oil in the stomach is a compound containing a hydrophobic group that is insoluble in water, and is generally composed of triglycerides represented by the following chemical structural formula.

Figure 112007500343354-pat00016
Figure 112007500343354-pat00016

식물성 유지는 일반적으로 지방산의 함량에 따라 특징지어지는데, 유지를 구성하는 지방산의 길이, 함유량 및 포화정도가 오일의 물리적, 화학적 성질을 결정하는 중요한 요인으로 작용한다. 동물성 오일은 식물성에 비해 사용성이 낮으며 육지동물 중 돼지, 소, 양의 오일과 바다동물 중 청어와 Menhaden 만이 오늘날 상업적으로 중요시 되고 있다. 동물성 오일은 식물성 오일과 마찬가지로 포화 및 불포화 Triglycerides로 구성되어 있으나 식물성 오일과는 달리 지방산 분포가 넓으며 약간의 홀수 직쇄형 지방산을 포함하고 있다.Vegetable fats and oils are generally characterized by the content of fatty acids. The length, content and saturation of the fatty acids that make up the fats and fats play an important role in determining the physical and chemical properties of the oil. Animal oils are less usable than plants, and only herds of land animals, pigs, cattle and sheep, and herring and menhaden sea animals are of commercial importance today. Animal oils, like vegetable oils, are composed of saturated and unsaturated triglycerides. Unlike vegetable oils, animal oils have a broad fatty acid distribution and contain some odd linear fatty acids.

식물유 메틸 에스테르, 바이오디젤은 독성이 적고 생분해성이 높아 토양에 유출되었을 경우 토양의 오염이 탄화수소계 윤활기유에 비해 적다. 또한 기후 변화 협약 대응(Life Cycle CO2: 경유의 1/4 수준)의 방편으로 식물유 메틸 에스테르 1톤 사용 시에 CO2를 2.2톤 감면받음으로써 국가경쟁력에도 이바지한다. 식물유 메틸 에스테르는 Methyl Oleate와 Methyl Linoleate가 주성분으로 저점도이며(40 , 1.9∼6.0cSt), 윤활성이 뛰어나 석유계 탄화수소 윤활기유 대신 사용할 경우 가공성이나 세정성 등에서 우수한 성능을 나타낸다.Vegetable oil methyl ester and biodiesel are less toxic and biodegradable, so when they are spilled into the soil, soil contamination is less than that of hydrocarbon-based lubricants. It also contributes to national competitiveness by reducing 2.2 tonnes of CO2 when one tonne of vegetable oil methyl ester is used as a way of responding to the climate change agreement (Life Cycle CO2). Vegetable oil methyl ester is composed of Methyl Oleate and Methyl Linoleate as the main components, and has low viscosity (40, 1.9∼6.0 cSt). It has excellent lubricity and shows excellent performance in processability and detergency when used in place of petroleum hydrocarbon lubricant base oil.

CH3-(CH2)14-COO-CH3 : Methyl PalmitateCH3- (CH2) 14-COO-CH3: Methyl Palmitate

CH3-(CH2)6-CH2-CH=CH-CH2-(CH2)6-COO-CH3 : Methyl OleateCH3- (CH2) 6-CH2-CH = CH-CH2- (CH2) 6-COO-CH3: Methyl Oleate

CH3-(CH2)3-CH2-CH=CH-CH2-CH=CH-CH2-(CH2)6-COO-CH3 : Methyl LinoleateCH3- (CH2) 3-CH2-CH = CH-CH2-CH = CH-CH2- (CH2) 6-COO-CH3: Methyl Linoleate

식물유 메틸 에스테르는 식물성유지로부터 합성된 메틸 에스테르로서 제조공정은 다음과 같다.Vegetable oil methyl ester is a methyl ester synthesized from vegetable oil and the manufacturing process is as follows.

Figure 112007500343354-pat00017
Figure 112007500343354-pat00017

여기서, R, R', R"은 알킬기로 포화 또는 불포화 탄화수소를 뜻한다.Here, R, R 'and R "refer to saturated or unsaturated hydrocarbons with alkyl groups.

〈바이오디젤을 제조하는 채종유 및 대두유의 지방산 조성〉<Fatty acid composition of rapeseed oil and soybean oil to manufacture biodiesel>

Figure 112007500343354-pat00018
Figure 112007500343354-pat00018

〈그리스 제조에 사용되는 지방산의 화학적 구조〉<Chemical Structure of Fatty Acids Used in Greek Preparation>

Figure 112007500343354-pat00019
Figure 112007500343354-pat00019

〈식물유 및 합성에스테르계 기유의 생분해성 비교, CEC-L-33-A-93법〉<Biodegradability comparison of vegetable oil and synthetic ester base oil, CEC-L-33-A-93 method>

Figure 112007500343354-pat00020
Figure 112007500343354-pat00020

식물유 메틸 에스테르의 조성성분과 조성비율은 식물유의 지방산 성분 및 조 성비율에 따라 다르다. 하기 표에 나와있는 지방산의 메틸 에스테르가 식물유 메틸에스테르의 조성성분이다.The compositional components and composition ratios of the vegetable oil methyl esters depend on the fatty acid component and composition ratio of the vegetable oil. The methyl esters of fatty acids shown in the following table are the components of vegetable oil methyl esters.

〈수용성 금속가공유에 사용될 수 있고 식물유 메틸에스테르 제조에 사용될 수 있는 지방산의 화학적 구조〉<Chemical structure of fatty acids that can be used for water-soluble metal covalent and used to prepare vegetable oil methyl esters>

Figure 112007500343354-pat00021
Figure 112007500343354-pat00021

본 발명에 사용할 수 있는 식물유 메틸에스테르를 합성 할 수 있는 식물성오일은 하기 표에 나와 있다.Vegetable oils which can synthesize vegetable oil methyl esters that can be used in the present invention are shown in the following table.

〈바이오 디젤을 제조할 수 있는 식물성오일의 지방산 조성〉<Fatty acid composition of vegetable oils that can produce biodiesel>

Figure 112007500343354-pat00022
Figure 112007500343354-pat00022

바이오디젤은 경유에 섞어서 사용할 수도 있고 100％ 바이오디젤 만으로 사용할 수 있는데, 경유 95％에 5％의 바이오디젤을 섞은 것을 BD5 라고 부르며 바이오디젤이 20％ 포함된 것은 BD20 이라고 말한다. 바이오디젤은 폐자원의 재활용이나 온실가스인 CO2를 저감 시키는 효과가 있으며, 대기오염 물질의 배출이 적은 편이어서 국내외에서 미래의 에너지원으로 관심받고 있다. 현재 세계에서는 바이오디젤을 시범으로 사용하거나 시범사업을 통하여 보급을 늘려가고 있는 단계이다. 먼저 유럽은 대체에너지 사용에 적극성을 갖고 있어 바이오디젤에 대한 제도가 정착단계에 이르고 있다. 일반 경유의 규격을 만족하는 범위 내에서 사용을 공식적으로 인정하고 있는데, 2004년 1월 발효된 유럽 경유 규격(EN590)에 따르면 바이오디젤 5％까지를 일반 경유로 인정하고 있다. (단, EN14214 규격 만족 필요) 미국에서는 1992년에 국립 바이오디젤 보드를 설립한 이후로 1998년부터 국회 및 EPA에서 BD20을 디젤 차량 연료로 승인하였고 2001년에는 부시 대통령이 바이오디젤을 포함한 신 재생에너지의 보급 확대를 천명한바 있습니다. 정부차원에서 적극적으로 도입을 발표함에 따라 바이오디젤의 보급실적이 매년 증가하고 있으며 육군, 공군, 에너지성, NASA를 비롯하여 주정부의 관용차량 및 버스 등에 사용되고 있다. 우리나라에 서는 2002년 5월 산업자원부의 바이오디젤 시범보급사업 추진에 관한 고시에 근거하여 2년간의 시범운행을 하였으며 올해 다시 1년을 연장하는 등 바이오디젤에 대한 시장반응 및 문제점에 대한 검토를 하고 있는 상황이다. 바이오디젤의 가장 큰 장점은 자동차에서 뿜어져 나오는 매연을 저감 시킬 수 있다는 점이다. 바이오디젤이 온실가스인 CO2를 배출하지 않는 것은 아니지만, 공정의 전 주기(생산부터 소비까지 전체적인 관점에서 보는 것)에서 볼 때 CO2의 산출량이 아주 낮으며 황산화물(SOx)과 입자상물질(PM)도 다소 적게 배출한다. 식물자원에서 생산되므로 국내에서 자체 생산할 수 있어 에너지 안보차원에서도 장점이 있으며, 폐식용유 등 폐자원의 활용으로 환경오염 저감의 효과가 있다. 또한 인프라 측면에서도 디젤 엔진이나 주유소 유통망을 사용할 수 있어서 추가적인 소요 비용이 없다는 점도 장점으로 꼽히고 있다. 그러나 이러한 장점에도 불구하고 기존의 경유나 휘발유를 대체하기에는 여러 가지 문제점을 가지고 있다. 자동차 배출가스의 유해물질 저감을 위해서는 바이오디젤의 배합비율이 높아져야 하는데 바이오디젤은 엔진을 부식 시키는 특성이 있어서 엔진의 고장을 유발할 수 있으며, 오래 저장하는 경우 변질되는 문제가 있다.Biodiesel can be mixed with light oil or used as 100% biodiesel only. A mixture of 95% diesel and 5% biodiesel is called BD5 and 20% biodiesel is called BD20. Biodiesel has the effect of reducing the recycling of waste resources and CO2, which is a greenhouse gas, and because of the low emission of air pollutants, it is drawing attention as a future energy source at home and abroad. At present, the world is using biodiesel as a demonstration or increasing its supply through pilot projects. First of all, Europe is active in using alternative energy, and the biodiesel system is settled. It is formally recognized for use as long as it meets the specifications of general diesel. The European Diesel Standard (EN590), which entered into force in January 2004, recognizes up to 5% biodiesel as general diesel. In the United States, since the establishment of the National Biodiesel Board in 1992, the National Assembly and EPA have approved the BD20 as a diesel vehicle fuel since 1998. In 2001, President Bush began renewable energy, including biodiesel. We have expanded our spread. As the government announces the introduction actively, biodiesel's supply is increasing every year, and it is used in the army, air force, energy ministry, NASA, state vehicles and buses. In Korea, in May 2002, the Ministry of Commerce, Industry and Energy conducted a two-year pilot operation based on the notification of the Ministry of Commerce, Industry and Energy's promotion of biodiesel pilot projects. It is a situation. The biggest advantage of biodiesel is that it can reduce the smoke emitted from cars. While biodiesel does not emit CO2, a greenhouse gas, CO2 yields are very low throughout the life cycle of the process (from an overall point of view, from production to consumption), sulfur oxides (SOx) and particulate matter (PM). Somewhat less emissions. Since it is produced from plant resources, it can be produced in-house in Korea, which has advantages in terms of energy security. It also has the effect of reducing environmental pollution by utilizing waste resources such as waste cooking oil. In terms of infrastructure, diesel engines and gas station distribution networks can be used, which means that there is no additional cost. However, despite these advantages, there are various problems to replace the existing diesel or gasoline. In order to reduce harmful substances in automobile exhaust gas, the biodiesel compounding ratio should be increased. Biodiesel has a characteristic of corroding the engine, which may cause engine failure, and deteriorates when stored for a long time.

이런 이유로 식물유 메틸에스테르를 자동차 연료유로 사용하기 위해서는 좀 더 높은 순도의 제품을 필요로 하기 때문에 메틸에스테르 반응 후 별도의 감압증류 공정을 거친다. 감압 증류조건은 2∼3torr, max 240 정도로 수행을 한다. 감압증류 후 증류물은 바이오디젤 연료유로 사용되어지고, 약 1∼5％ 정도의 증류잔류물이 부가적으로 생성된다. 이러한 바이오디젤 생산 시 생성되는 증류잔류물도 식물유의 반응물로 에스테르 구조를 가지고 있으며 친환경 윤활기유로 사용이 가능하다.For this reason, vegetable oil methyl ester requires a higher purity product to be used as an automobile fuel oil, and thus undergoes a separate vacuum distillation process after the methyl ester reaction. Distillation under reduced pressure is carried out at 2 to 3 torr, about 240 max. After distillation under reduced pressure, the distillate is used as biodiesel fuel oil, and about 1 to 5% of distillation residue is additionally produced. Distillation residues produced during the production of biodiesel also have ester structure as reactants of vegetable oil, and can be used as eco-friendly lubricant base oil.

본 발명은 대두유 및 채종유를 원료로 하여 바이오디젤을 생산할 때 발생되는 증류잔류물을 기유로 사용하고, 기타 증주제 및 첨가제를 배합하여 조성되는 그리스 조성물을 제공하는 것이다.The present invention provides a grease composition comprising a distillation residue generated when biodiesel is produced using soybean oil and rapeseed oil as a base oil, and a combination of other thickeners and additives.

증주제로는 리튬비누계, 디우레아계, 알루미늄복합 비누계, 벤토나이트계 등이 있으며, 첨가제로는 유동점강하제, 윤활첨가제, 구조안정제, 산화방지제, 금속부식 방지제 등을 사용하며 환경에 미치는 영향이 적은 첨가제만을 사용하였고, 향후 사용이 규제될 수 있는 첨가제 성분인 Nitrite, Formaldehyde 및 그 유도체 등은 사용하지 않았고, 석유계 탄화수소 등은 제외한 것이다.Thickeners include lithium soap-based, diurea-based, aluminum complex soap-based, bentonite-based, and additives such as pour point depressants, lubricating additives, structural stabilizers, antioxidants, and metal corrosion inhibitors. Only additives were used. Nitrite, Formaldehyde and its derivatives, which are additive ingredients that could be regulated in the future, were not used. Petroleum hydrocarbons are excluded.

본 발명은 기계, 설비 등 산업용 윤활그리스에 관한 것으로서, 더욱 상세하게는 바이오디젤을 생산할 때 발생되는 증류잔류물 10∼95 중량％와 증주제 3∼30중량％ 및 첨가제 3∼50중량％를 배합하여 조성되는 그리스 조성물에 관한 것이다.The present invention relates to industrial lubricating grease, such as machinery and equipment, and more particularly, by mixing 10 to 95% by weight of distillation residues, 3 to 30% by weight of thickener and 3 to 50% by weight of additives A grease composition to be formulated.

본 발명에서 바이오디젤의 증류잔류물은 대두유와 유채유에서 생성되는 바이오디젤의 증류잔류물이다.In the present invention, the distillation residue of biodiesel is a distillation residue of biodiesel produced from soybean oil and rapeseed oil.

본 발명에서 사용되는 증주제는 리튬비누, 알루미늄비누, 디우레아(Di-Urea), 벤톤(entone), 실리카겔(Silica Gel)의 5종으로 구분되며 이들 그룹 중에서 선택되는 하나 이상의 것이다.The thickener used in the present invention is classified into five kinds of lithium soap, aluminum soap, diurea (Di-Urea), benton (entone), and silica gel (Silica Gel) and at least one selected from these groups.

리튬 및 알루미늄비누는 리튬 및 알루미늄 금속과 12-Hydroxy Stearic Acid, Stearic Acid, Boric Acid, Benzoic Acid, H2O 등과의 비누화 반응 후 생성되는 비누를 포함한다.Lithium and aluminum soaps include soaps produced after saponification of lithium and aluminum metals with 12-Hydroxy Stearic Acid, Stearic Acid, Boric Acid, Benzoic Acid, H2O and the like.

디우레아계 증주제는 톨릴렌디이소시아네이트 화합물, 디페닐메탄디이소시아네이트, 나프탈렌, 디이소시아네이트등의 디이소시아네이트 화합물로 이루어진 군과 벤질아민, 톨루이딘, 콜로로아닐린등의 모노아민, 테트라데실아민, 펜타데실아민, 헥사데실아민, 헵타데실아민, 옥타데실아민, 노닐데실아민, 에이코실아민 등의 군과의 반응물인 Di-Urea 반응물을 포함한다.The diurea thickener is composed of diisocyanate compounds such as tolylene diisocyanate compound, diphenylmethane diisocyanate, naphthalene, diisocyanate, monoamines such as benzylamine, toluidine, and coloaniline, tetradecylamine, pentadecylamine, Di-Urea reactants, which are reactants with groups such as hexadecylamine, heptadecylamine, octadecylamine, nonyldecylamine, eicosylamine, and the like.

벤톤계 증주제는 Bentonite와 Self Activator로서 알코올 또는 물을 포함한다.Bentonic thickeners include alcohol or water as Bentonite and Self Activator.

실리카겔계 증주제는 Fumed Silica 로서 Hydorphobil(친수성)과 Hydrophilic(소수성)계의 Silica를 포함한다.Silica gel-based thickeners are Fumed Silica and include Hydorphobil (hydrophilic) and Hydrophilic (hydrophobic) Silica.

본 발명에서 사용하는 첨가제는 유동점강하제, 윤활첨가제, 금속부식 방지제, 산화방지제, 구조안정제, 증점제를 포함한다. 본 발명에서 사용하는 첨가제는 유동점강하제, 윤활첨가제, 금속부식 방지제, 산화방지제, 구조안정제, 증점제로 이루어진 그룹 중에서 선택되는 하나 이상인 것이다. 본 발명에서 사용하는 첨가제로서 유동점강하제는 폴리메타크릴레이트, 아로마틱계 합성기유 및 이들의 유도체를 포함한다. 윤활첨가제는 디티오카바메이트, 아릴포스페이트계, 인산에스테르의 금속염, 및 황화물 및 이들의 유도체를 포함한다. 금속부식방지제는 벤조트리아졸, 톨리트리아졸, 머캅토벤조티아졸 및 이들의 유도체를 포함한다. 산화방지제는 테트라부틸메틸페놀, 퀴놀린계 화합물 및 이들의 유도체를 포함한다. 구조안정제는 에 틸렌 프로필렌과 같은 공중합체 및 이들의 유도체를 포함한다. 증점제는 폴리부텐 및 폴리이소부틸렌 등의 유도체를 포함한다.The additive used in the present invention includes a pour point lowering agent, a lubricating additive, a metal corrosion inhibitor, an antioxidant, a structural stabilizer, and a thickener. The additive used in the present invention is at least one selected from the group consisting of a flow point lowering agent, a lubricant additive, a metal corrosion inhibitor, an antioxidant, a structural stabilizer, and a thickener. Pour point depressants as additives used in the present invention include polymethacrylates, aromatic synthetic base oils and derivatives thereof. Lubricant additives include dithiocarbamate, arylphosphate-based, metal salts of phosphate esters, and sulfides and derivatives thereof. Anticorrosive agents include benzotriazole, tolytriazole, mercaptobenzothiazole and derivatives thereof. Antioxidants include tetrabutylmethylphenol, quinoline compounds and derivatives thereof. Structural stabilizers include copolymers such as ethylene propylene and derivatives thereof. Thickeners include derivatives such as polybutene and polyisobutylene.

[실시예]EXAMPLE

바이오디젤 증류잔류물을 기유로 사용하여 4개의 증주제 별로 그리스를 제조한 후 물성치와 성능을 측정하였다.The biodiesel distillation residue was used as base oil to prepare grease for each of the four thickeners, and then the physical properties and performance were measured.

실시예 1 (리튬계 증주제)Example 1 (lithium thickener)

바이오디젤 생산 시 생성되는 증류잔류물, 리튬 비누(수산화 리튬과 12-Hydroxy Stearic Acid, Stearic Acid, Azelaic Acid, Boric Acid 등의 지방산과 비누화 반응물), 유동점 향상제, 윤활첨가제, 금속부식 방지제, 산화방지제, 구조안정제, 증점제를 첨가하여 리튬비누계 그리스조성물을 제조하였다.Distillation residues produced during biodiesel production, lithium soaps (fatty acid and saponification reactions of lithium hydroxide and 12-Hydroxy Stearic Acid, Stearic Acid, Azelaic Acid, Boric Acid, etc.), Pour point enhancers, lubricant additives, metal corrosion inhibitors, antioxidants A lithium soap-based grease composition was prepared by adding a structural stabilizer and a thickener.

표 1. 리튬비누계 그리스 조성 및 물성Table 1. Lithium soap-based grease composition and physical properties

Figure 112007500343354-pat00010
Figure 112007500343354-pat00010

실시예 2(디우레아 계 증주제 )Example 2 (Diurea type thickener)

바이오디젤을 생산할 때 생성되는 증류잔류물, 디우레아증주제(Di-urea, 톨릴렌디이소시아네이트 화합물, 디페닐메탄디이소시아네이트, 나프탈렌디이소시아네이트등의 디이소시아네이트 화합물, 벤질아민, 톨루이딘, 콜로로아닐린등의 모노아인, 테트라데실아민, 펜타데실아민, 헥사데실아민, 헵타데실아민, 옥타데실아민, 노닐데실아민, 에이코실아민 등의 방향족아민), 유동점 강하제, 윤활첨가제, 금속부식 방지제, 산화방지제, 구조안정제를 첨가하여 디우레아 그리스 조성물을 제조하였다.Distillation residue produced when producing biodiesel, diurea thickener (Di-urea, tolylene diisocyanate compound, diisocyanate compound such as diphenylmethane diisocyanate, naphthalene diisocyanate, benzylamine, toluidine, coloaniline, etc.) Amine, tetradecylamine, pentadecylamine, hexadecylamine, heptadecylamine, octadecylamine, nonyldecylamine, aromatic amines such as eicosylamine), pour point depressant, lubricant additive, metal corrosion inhibitor, antioxidant, structural stabilizer Diurea grease composition was prepared by addition.

표 2. 디우레아 그리스 조성 및 물성Table 2. Diurea Grease Composition and Properties

Figure 112007500343354-pat00023
Figure 112007500343354-pat00023

실시예 3(알루미늄 계 증주제)Example 3 (aluminum thickener)

바이오디젤을 생산할 때 생성되는 증류잔류물, 알루미늄 복합 증주제(알루미늄 금속 화합물과 지방산 Benzoic, Palmitic, Palmitoleic, Stearic, Oleic, Linoleic Acid), 유동점 강하제, 윤활첨가제, 금속부식 방지제, 산화방지제, 구조안정제를 첨가하여 알루미늄 복합 그리스 조성물을 제조하였다.Distillation residues produced during biodiesel production, aluminum complex thickeners (aluminum metal compounds and fatty acids Benzoic, Palmitic, Palmitoleic, Stearic, Oleic, Linoleic Acid), Pour point depressants, lubricant additives, metal corrosion inhibitors, antioxidants, structural stabilizers Was added to prepare an aluminum composite grease composition.

표 3. 알루미늄 계 그리스 조성물 및 물성Table 3. Aluminum Grease Composition and Physical Properties

Figure 112007500343354-pat00024
Figure 112007500343354-pat00024

실시예 4 (벤톤 계 증주제)Example 4 (benton system thickener)

바이오디젤 생산 시 생성되는 증류잔류물, Bentone증주제, 유동점강하제, 윤활첨가제, 금속부식 방지제, 산화방지제, 구조안정제를 첨가하여 Betone 그리스 조성물을 제조하였다.A Betone grease composition was prepared by adding distillation residue, Bentone thickener, pour point lowering agent, lubricating additive, metal corrosion inhibitor, antioxidant, and structural stabilizer.

표 4. Bentone계 그리스 조성물 및 물성Table 4. Bentone Grease Compositions and Properties

Figure 112007500343354-pat00014
Figure 112007500343354-pat00014

실시예 5 (실리카 겔 계 증주제)Example 5 (silica gel type thickener)

바이오디젤을 생산할 때 생성되는 증류잔류물, Silica Gel 증주제, 유동점강하제, 윤활첨가제, 금속부식 방지제, 산화방지제, 구조안정제를 첨가하여 Silica 그리스를 제조하였다.Silica grease was prepared by adding distillation residue, Silica Gel thickener, pour point depressant, lubricant additive, metal corrosion inhibitor, antioxidant, and structural stabilizer.

표 5. Silica Gel을 증주제로 이용하는 그리스 조성물 및 물성Table 5. Grease Composition and Physical Properties Using Silica Gel as Thickener

Figure 112007500343354-pat00025
Figure 112007500343354-pat00025

본 발명은 그리스 조성물의 유효성분으로서 바이오디젤을 생산할 때 생성되는 증류잔류물을 그리스의 기유로 활용하여 기존의 석유계 기유사용에 비해서 윤활성이 우수하고 식물유계 및 합성에스테르를 기유로 사용하는 제품에 비해서는 저렴한 가격에 동등수준의 환경친화적인 그리스를 공급할 수있게 되었으며 바이오디젤 증류잔류물의 자원재활용 등 효과를 얻을 수 있는 것이다.The present invention utilizes the distillation residue produced when producing biodiesel as an active ingredient of the grease composition as a base oil of grease, and has excellent lubricity compared to the use of conventional petroleum base oils. On the other hand, it is possible to supply eco-friendly grease of the same level at a low price and to obtain the effect of recycling the biodiesel distillate residue.

Claims (8)

바이오디젤을 생산할 때 생성되는 증류잔류물 50∼95 중량％와 증주제 3∼30 중량％ 및 첨가제 3∼20 중량％를 배합하여 제조되는 것을 특징으로 하는 그리스 조성물A grease composition, which is prepared by combining 50 to 95% by weight of distillation residue, 3 to 30% by weight of thickener and 3 to 20% by weight of additives produced when producing biodiesel. 제 1항에 있어서, 상기 증류잔류물은 대두유 또는 채종유를 원료로 하여 바이오디젤을 생산할 때 생성되는 증류잔류물로서 기유 동점도(40 ,cSt)가 20∼400의 범위인 것을 특징으로 하는 그리스 조성물The grease composition according to claim 1, wherein the distillation residue is a distillation residue produced when biodiesel is produced using soybean oil or rapeseed oil as a raw material, and the base oil kinematic viscosity (40, cSt) is in a range of 20 to 400. 제1항에 있어서, 상기 증주제 는 리튬비누 계, 디우레아 계, 알루미늄 복합비누 계, Bentone 증주제 또는 실리카 겔 계중 선택되는 하나 이상인 것을 특징으로 하는 그리스 조성물The grease composition according to claim 1, wherein the thickener is at least one selected from lithium soap based, diurea based, aluminum complex soap based, Bentone thickener or silica gel based. 제 3 항에 있어서, 상기 리튬비누 계 증주제는 수산화리튬 금속화합물과 12-Hydroxy Stearic , Stearic, Boric, Azelaic, Sebacic Acid 중에서 선택되는 하나 이상인 것을 특징으로 하는 그리스 조성물The grease composition according to claim 3, wherein the lithium soap-based thickener is at least one selected from lithium hydroxide metal compound and 12-Hydroxy Stearic, Stearic, Boric, Azelaic, Sebacic Acid. 제 3 항에 있어서, 상기 디우레아 계는 디이소시아네이트 화합물과 벤질아민, 톨루이딘, 콜로로아닐린등의 모노아민, 테트라데실아민, 펜타데실아민, 헥사데 실아민, 헵타데실아민, 옥타데실아민, 노닐데실아민, 에이코실아민 등의 방향족아민 중에서 선택되는 하나 이상인 것을 특징으로 하는 그리스 조성물4. The diurea-based compound according to claim 3, wherein the diurea-based compound is a diisocyanate compound, a monoamine such as benzylamine, toluidine, and coloaniline, tetradecylamine, pentadecylamine, hexadecylamine, heptadecylamine, octadecylamine, and nonyl. A grease composition characterized by at least one selected from aromatic amines such as decylamine and eicosylamine. 제 3 항에 있어서, 상기 알루미늄복합비누 계 증주제는 알루미늄 금속 화합물과 Benzoic, Stearic, Palmitic, Palmitoleic, Oleic Acid중에서 선택되는 하나 이상인 것을 특징으로 하는 그리스 조성물4. The grease composition of claim 3, wherein the aluminum complex soap thickener is at least one selected from an aluminum metal compound and Benzoic, Stearic, Palmitic, Palmitoleic, and Oleic Acid. 제 3 항에 있어서, 실리카 겔 계 증주제는 Fumed Silica 로서 소수성(Hydrophobic)과 친수성(Hydrophilic)을 포함하여 기유에 분산하여 그리스 증주제로 사용되어지는 것을 특징으로 하는 그리스 조성물.The grease composition according to claim 3, wherein the silica gel-based thickener is Fumed Silica and is used as a grease thickener by dispersing it in a base oil including hydrophobic and hydrophilic. 제 1 항에 있어서, 상기 첨가제는 폴리메타크릴레이트, 아로마틱계 합성기유 및 이들의 유도체를 포함한 유동점강하제와 디티오카바메이트, 아릴포스페이트계, 인산에스테르의 금속염, 황화물 및 이들의 유도체를 포함한 윤활첨가제와 벤조트리아졸, 톨리트리아졸, 머캅토벤조티아졸 및 이들의 유도체를 포함한 금속부식방지제와 테트라부틸메틸페놀, 퀴놀린 화합물 및 이들의 유도체를 포함한 산화방지제 및 에틸렌 프로필렌과 같은 공중합체 및 이들의 유도체를 포함한 구조안정제 중 하나 이상인 것을 특징으로 하는 그리스 조성물The additive according to claim 1, wherein the additive is a lubricating agent including a polymethacrylate, an aromatic synthetic base oil and a derivative thereof and a lubricating agent including a dithiocarbamate, an aryl phosphate, a metal salt of a phosphate ester, a sulfide and a derivative thereof. And metal corrosion inhibitors including benzotriazole, tolytriazole, mercaptobenzothiazole and derivatives thereof, antioxidants including tetrabutylmethylphenol, quinoline compounds and derivatives thereof and copolymers such as ethylene propylene and the like A grease composition, characterized in that at least one of the structural stabilizers including derivatives
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