KR20210074925A - Eco-Friendly Water-Soluble Cutting Oil Containing Biocompatible Antibacterial Agent (POM) - Google Patents
Eco-Friendly Water-Soluble Cutting Oil Containing Biocompatible Antibacterial Agent (POM) Download PDFInfo
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
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Abstract
Description
본 발명은 생체적합성 항균제(POM)를 함유한 친환경 수용성 절삭유에 관한 것으로, 보다 상세하게는 고체 파우더 상태의 생체적합성 항균제인 폴리옥소메탈레이트 1(polyoxometalate 1, POM 1), 폴리옥소메탈레이트 2(polyoxometalate 2, POM 2) 또는 폴리옥소메탈레이트 7(polyoxometalate 7, POM 7)을 물에 녹여 친환경 수용성 절삭유를 제조하여, 강한 산화력을 가져서 향균, 탈취 기능이 있으며, 독성이 없으며, 물과 유기 용매에 대한 높은 용해도와 열적인 안정성을 가지고 있으며, 자외선-근가시선에서의 강한 흡수성을 가지며, 다양한 산화제에 의해 재산화 항균성이 높고 인체에 무해한 생체적합성 항균제(POM)를 함유한 친환경 수용성 절삭유에 관한 것이다.The present invention relates to an eco-friendly water-soluble cutting oil containing a biocompatible antibacterial agent (POM), and more particularly, polyoxometalate 1 (POM 1), polyoxometalate 2 (polyoxometalate 1, POM 1), which are biocompatible antibacterial agents in a solid powder state ( By dissolving
일반적으로 절삭유는 절삭기계에서 금속의 가공을 돕기 위한 윤활유이며, 비수용성 절삭유, 수용성 절삭유로 대별된다. 본 발명은 수용성 절삭유에 적용되는 것으로, 상기 수용성 절삭유는 냉각작용이 우수하고, 비인화성, 화재위험이 없으며, 경제적으로 우수하며, 청정작용을 하며, 깨끗한 환경이 조성되는 장점이 있다. 그러나 상기 수용성 절삭유는 유해성분을 함유하기 쉽고, 부패/악취/성능저하의 우려가 있으며 첨가된 항균제성분이 독성을 가지기 쉬운 단점이 있다. 곧 수용성 절삭유의 문제점은 미생물 번식이 용이하여 부패 악취가 발생하기 쉽고 부패 방지를 위해 사용되는 항균제는 유해성분(아민계, 페놀류, 염화파라핀류 등)을 함유하고 있어서 항균제로 인한 피부염, 습진, 폐쇄성 폐증상(기침, 가래, 천식, 만성기관지염 등)이 발생하고 있다. 그러므로 이러한 수용성 절삭유를 개선하려는 기술이 개발되어 왔으며, 일례로서 종래기술인 등록특허공보 등록번호 10-0665790호에는 식물유 30~60 중량%, 포화 및 불포화 지방산 5~25 중량%, 이염기 지방산 0.1~5 중량%, 안식향산 나트륨 0.5~3 중량%, 아마이드계 방청제 1~10 중량%, 알코올계 용매 3~20 중량%, pH 조정제 0.1~1.5 중량%, 천연 계면활성제 3~7 중량%, 부식방지제 0.1~0.5 중량%, 산화방지제 0.1~1 중량%, 미생물 억제제 0.5~3 중량%를 증류수에 배합하여 조성된 것을 특징으로 하는 수용성 절삭유 조성물이 공개되어 있다.In general, cutting oil is a lubricating oil to help metal processing in a cutting machine, and is roughly divided into water-insoluble cutting oil and water-soluble cutting oil. The present invention is applied to water-soluble cutting oil, and the water-soluble cutting oil has an excellent cooling action, is non-flammable, has no fire risk, is economically excellent, has a clean action, and creates a clean environment. However, the water-soluble cutting oil tends to contain harmful components, there is a risk of decay/odor/performance degradation, and the added antibacterial agent component is likely to be toxic. The problem with water-soluble cutting oil is that it is easy to propagate microorganisms, so the smell of decay is easy to occur. Antibacterial agents used to prevent spoilage contain harmful ingredients (amines, phenols, chlorinated paraffins, etc.), so dermatitis, eczema, and occlusion caused by antibacterial agents. Pulmonary symptoms (cough, sputum, asthma, chronic bronchitis, etc.) are occurring. Therefore, technologies to improve such water-soluble cutting oil have been developed, and as an example, in the prior art Registration No. 10-0665790, vegetable oil 30-60 wt%, saturated and unsaturated fatty acid 5-25 wt%, dibasic fatty acid 0.1-5 wt% wt%, sodium benzoate 0.5-3 wt%, amide-based rust inhibitor 1-10 wt%, alcohol solvent 3-20 wt%, pH adjuster 0.1-1.5 wt%, natural surfactant 3-7 wt%, corrosion inhibitor 0.1- There is disclosed a water-soluble cutting oil composition comprising 0.5 wt% of an antioxidant, 0.1 to 1 wt% of an antioxidant, and 0.5 to 3 wt% of a microorganism inhibitor in distilled water.
또한, 등록특허공보 등록번호 10-1069392호에는 나노 은을 포함하는 수용성 절삭유 조성물로서,In addition, Patent Registration No. 10-1069392 discloses a water-soluble cutting oil composition containing nano silver,
상기 나노 은 입자는 평균 입경이 3 nm 내지 16 nm이고,The nano-silver particles have an average particle diameter of 3 nm to 16 nm,
나노 은의 농도는 20 ppm 내지 100 ppm이며,The concentration of nano silver is 20 ppm to 100 ppm,
나노 은의 불순물 농도는 0.003 내지 0.005 중량%인 수용성 항균 절삭유 조성물이 공개되어 있다.A water-soluble antibacterial cutting oil composition having an impurity concentration of 0.003 to 0.005 wt % of nano silver has been disclosed.
그러나 상기 종래기술들은 항균성이 낮아 변질되거나 인체에 유해한 물질이 발생될 우려가 있었다.However, the prior art has a low antibacterial property, there is a risk of deterioration or substances harmful to the human body.
따라서 본 발명은 상기와 같은 문제점을 해결하고자 안출된 것으로,유해물질을 배제하고, 고성능 생체적합성 항균제인 폴리옥소메탈레이트(polyoxometalate, POM)를 함유하는 친환경 수용성 절삭유 제조방법을 제공하고자 하는 것이다.Therefore, the present invention has been devised to solve the above problems, and it is an object of the present invention to provide an eco-friendly, water-soluble cutting oil manufacturing method that excludes harmful substances and contains polyoxometalate (POM), a high-performance biocompatible antibacterial agent.
본 발명은 폴리옥소메탈레이트(POM)를 함유한 친환경 수용성 절삭유에 관한 것으로,The present invention relates to an eco-friendly water-soluble cutting oil containing polyoxometalate (POM),
고체 파우더 상태의 생체적합성 항균제인 폴리옥소메탈레이트 1(polyoxometalate 1, POM 1), 폴리옥소메탈레이트 2(polyoxometalate 2, POM 2) 또는 폴리옥소메탈레이트 7(polyoxometalate 7, POM 7)을 물에 녹여 친환경 수용성 절삭유를 제조하는 것을 특징으로 한다.Dissolve polyoxometalate 1 (POM 1), polyoxometalate 2 (POM 2) or polyoxometalate 7 (POM 7), which are biocompatible antibacterial agents in a solid powder state, in water. It is characterized by manufacturing eco-friendly water-soluble cutting oil.
따라서 본 발명의 제조방법에 의해 제조된 친환경 수용성 절삭유는 강한 산화력을 가져서 향균, 탈취 기능이 있으며, 독성이 없으며, 물과 유기 용매에 대한 높은 용해도와 열적인 안정성을 가지고 있으며, 자외선-근가시선에서의 강한 흡수성을 가지며, 다양한 산화제에 의해 재산화 항균성이 높고 인체에 무해한 현저한 효과가 있다.Therefore, the eco-friendly water-soluble cutting oil produced by the manufacturing method of the present invention has strong oxidizing power, has antibacterial and deodorizing functions, is non-toxic, has high solubility in water and organic solvents and thermal stability, and is It has a strong absorbency of oxidizing agents, has high reoxidation and antibacterial properties by various oxidizing agents, and has a remarkable effect harmless to the human body.
도 1은 본 발명의 (a) Solid and (b) solution states of POM1, POM2, and POM7
도 2는 본 발명의 FT-IR spectra of POM1, POM2, and POM7 (KBr)
도 3은 본 발명의 UV-VIS spectra of POM1, POM2, and POM7 (H2O)
도 4는 본 발명의 XRD data of (a) POM1, (b) POM2, and (c) POM7
도 5는 본 발명의 POM1, POM2, POM7을 함유한 친환경 수용성 절삭유 시료에 대한 한국분석시험연구원(KATR)의 항균도 시험성적서
도 6은 본 발명의 POM1, POM2, POM7을 함유한 친환경 수용성 절삭유 시료에 대한 한국석유관리원(KPETRO)의 시험성적서1 is (a) Solid and (b) solution states of POM1, POM2, and POM7 of the present invention;
2 is an FT-IR spectra of POM1, POM2, and POM7 (KBr) of the present invention
3 is a UV-VIS spectra of POM1, POM2, and POM7 (H 2 O) of the present invention
4 is an XRD data of (a) POM1, (b) POM2, and (c) POM7 of the present invention.
5 is an antibacterial test report of the Korea Analytical Testing Research Institute (KATR) for an environmentally friendly water-soluble cutting oil sample containing POM1, POM2, and POM7 of the present invention;
6 is a test report of the Korea Petroleum Administration (KPETRO) for an eco-friendly water-soluble cutting oil sample containing POM1, POM2, and POM7 of the present invention.
본 발명은 폴리옥소메탈레이트(POM)를 함유한 친환경 수용성 절삭유에 관한 것으로,The present invention relates to an eco-friendly water-soluble cutting oil containing polyoxometalate (POM),
고체 파우더 상태의 생체적합성 항균제인 폴리옥소메탈레이트 1(polyoxometalate 1, POM 1), 폴리옥소메탈레이트 2(polyoxometalate 2, POM 2) 또는 폴리옥소메탈레이트 7(polyoxometalate 7, POM 7)을 물에 녹여 친환경 수용성 절삭유를 제조하는 것을 특징으로 한다.Dissolve polyoxometalate 1 (POM 1), polyoxometalate 2 (POM 2) or polyoxometalate 7 (POM 7), which are biocompatible antibacterial agents in a solid powder state, in water. It is characterized by manufacturing eco-friendly water-soluble cutting oil.
또한, 상기 폴리옥소메탈레이트 1(polyoxometalate 1, POM 1)은 [(NH4)6Mo7O24 ·4H2O] 인 것을 특징으로 한다.In addition, the polyoxometalate 1 (polyoxometalate 1, POM 1) is [(NH 4 ) 6 Mo 7 O 24 · 4H 2 O] It is characterized in that.
또한, 상기 폴리옥소메탈레이트 2(polyoxometalate 2, POM 2)는 NaVO3 을 물에 녹여 수용액을 제조하는 단계;In addition, the polyoxometalate 2 (
상기 수용액을 Na2MoO4 ·2H2O수용액에 가한 후 H3PO4를 넣어 혼합물 용액을 제조하는 단계;preparing a mixture solution by adding the aqueous solution to an aqueous solution of Na 2 MoO 4 · 2H 2 O and then adding H 3 PO 4 ;
상기 혼합물 용액을 가열하는 단계;heating the mixture solution;
상기 가열된 혼합물 용액을 식히는 단계;cooling the heated mixture solution;
상기 식힌 혼합물 용액에 KCl 70-80 g을 넣는 단계;adding 70-80 g of KCl to the cooled mixture solution;
생성된 침전물을 거른 후 황산수용액을 넣어 재결정하는 단계;Recrystallization by adding an aqueous sulfuric acid solution after filtering the resulting precipitate;
재결정을 거른 후 찬물로 씻고 공기중에서 건조시키는 단계;를 포함하여 제조되는 것을 특징으로 한다.After filtering recrystallization, washing with cold water and drying in air; characterized in that it is prepared including.
또한, 상기 폴리옥소메탈레이트 7(polyoxometalate 7, POM 7)은(NH4)6Mo7O24·4H2O를 물에 넣어 녹이는 단계; In addition, dissolving the polyoxometalate 7 (polyoxometalate 7, POM 7) silver (NH 4 ) 6 Mo 7 O 24· 4H 2 O in water;
H2O2를 넣는 단계;Putting H 2 O 2 ;
에탄올을 넣은 후 냉장고에 보관하여 결정을 얻는 단계; obtaining crystals by adding ethanol and storing in a refrigerator;
상기 결정을 거른 후 에탄올로 씻어 공기중에서 건조시키는 단계;를 포함하여 제조되는 것을 특징으로 한다.After filtering the crystals, washing with ethanol and drying in air; characterized in that it is prepared including.
본 발명을 첨부도면에 의해 상세히 설명하면 다음과 같다.The present invention will be described in detail with reference to the accompanying drawings as follows.
도 1은 본 발명의 (a) Solid and (b) solution states of POM1, POM2, and POM7, 도 2는 본 발명의 FT-IR spectra of POM1, POM2, and POM7 (KBr), 도 3은 본 발명의 UV-VIS spectra of POM1, POM2, and POM7 (H2O),도 4는 본 발명의 XRD data of (a) POM1, (b) POM2, and (c) POM7이다.Figure 1 is (a) Solid and (b) solution states of POM1, POM2, and POM7 of the present invention, Figure 2 is an FT-IR spectra of POM1, POM2, and POM7 (KBr) of the present invention, Figure 3 is the present invention UV-VIS spectra of POM1, POM2, and POM7 (H 2 O), Figure 4 is the XRD data of (a) POM1, (b) POM2, and (c) POM7 of the present invention.
본 발명의 수용성 절삭유는 주로 식물성 절삭유 성분이 포함되는 식물성 절삭유에 해당되며, 해당 절삭유는 통상 KS 분류로 1종 2호에 속하는 절삭유이다.The water-soluble cutting oil of the present invention mainly corresponds to vegetable cutting oil containing vegetable cutting oil components, and the cutting oil is usually a type 1
본 발명의 배합 성분은 POM이 수용성 절삭유의 전체의 중량비로 2% 이상이 함유되는 것을 특징으로 한다. 즉 여러 가지 첨가제 (광물성기유, 계면활성제, 지방산 혼합물)를 물에 혼합하되, POM이 수용성 절삭유의 전체의 중량비로 2% 이상이 함유되는 것이 바람직하다.The blending component of the present invention is characterized in that POM is contained in 2% or more of the total weight ratio of the water-soluble cutting oil. That is, various additives (mineral base oil, surfactant, fatty acid mixture) are mixed with water, but POM is preferably contained in 2% or more of the total weight ratio of the water-soluble cutting oil.
본발명의 성분인 폴리옥소메탈레이트(polyoxometalate, POM)은 주로 다중 음이온인 다원자 이온으로서 3개 이상의 전이금속 산소음이온이며, 산소원자에 의해 서로 연결되어 큰 3차원 구조를 가지며, 금속원자는 5, 6족 전이금속 (예: 바나듐(V), 니오븀(V), 탄탈륨(V), 몰리브데넘(VI), 텅스텐(VI) 등)이며, 높은 산화상태 (전자배치는 d0 또는 d1)의 특징을 가진다.Polyoxometalate (POM), a component of the present invention, is a polyatomic ion that is mainly a polyanion, and is three or more transition metal oxygenanions. They are connected to each other by oxygen atoms and have a large three-dimensional structure, and the metal atoms are 5 , a Group 6 transition metal (e.g., vanadium (V), niobium (V), tantalum (V), molybdenum (VI), tungsten (VI), etc.), and has a high oxidation state (electron configuration is d0 or d1). have characteristics.
본발명의 실시례로서,As an embodiment of the present invention,
POM1은 [(NH4)6Mo7O24 ·4H2O] 무색의 결정이며, 녹는점은 90 도에서 물 분자를 잃고, 190 도에서 타면서 녹는 특성이 있다.POM1 is [(NH 4 ) 6 Mo 7 O 24 · 4H 2 O] colorless crystal, and has a melting point of losing water molecules at 90°C and melting at 190°C while burning.
POM2는 [K5H4PMo6V6O40 ·15H2O] 이다.POM2 is [K 5 H 4 PMo 6 V 6 O 40 · 15H 2 O].
POM7는 [(NH4)8Mo10O22(O2)12 ·15H2O] 이다.POM7 is [(NH 4 ) 8 Mo 10 O 22 (O 2 ) 12 · 15H 2 O].
특히 본 발명의 POM2의 제조방법에 대해 설명하면, NaVO3 36.3 g(0.3 mol)을 뜨거운 물 250 ml에 녹였다. 이 용액을 Na2MoO4 ·H2O 41.1 g(0.3 mol)을 녹인 뜨거운 물 100 ml에 가한 후 85% H3PO4 25 ml를 넣었다. 이 혼합물을 95 ?C에서 1시간 동안 가열하였다. 혼합물 용액을 차갑게 식힌 후 KCl 70-80 g을 천천히 넣은 후 저어주었다. 생성된 침전물을 거른 후 80-100 ml의 0.25 M 황산수용액으로 80 ?C에서 재결정하였다. 흑적색의 결정을 거른 후 찬물로 씻고 공기중에서 건조시킨다. 녹는점은 120 도이다.In particular, describing the method for preparing POM2 of the present invention, 36.3 g (0.3 mol) of NaVO 3 was dissolved in 250 ml of hot water. This solution was added to 100 ml of hot water in which Na 2 MoO 4 · H 2 O 41.1 g (0.3 mol) was dissolved, and then 85% H 3 PO 4 25 ml was added. The mixture was heated at 95 °C for 1 h. After cooling the mixture solution, 70-80 g of KCl was slowly added thereto and stirred. After filtering the resulting precipitate, it was recrystallized at 80 °C with 80-100 ml of 0.25 M aqueous sulfuric acid solution. After filtering the black-red crystals, wash with cold water and dry in the air. The melting point is 120 degrees.
POM7의 제조방법은 (NH4)6Mo7O24 ·4H2O 10 g(8.1 mmol)을 물 40 ml에 넣어 60 ?C에서 녹인 후 실온으로 식혔다. 30% H2O2 40 ml를 넣었다. 에탄올 100 ml를 넣은 후 냉장고에 보관하여 노란색 결정을 얻어 거른 후 에탄올로 씻어 공기중에서 건조시켰다. 녹는점은 120-125 도이다.For the preparation of POM7, (NH 4 ) 6 Mo 7 O 24 · 4H 2 O 10 g (8.1 mmol) was dissolved in 40 ml of water at 60 °C, and then cooled to room temperature. 40 ml of 30% H 2 O 2 was added. After adding 100 ml of ethanol, it was stored in a refrigerator to obtain yellow crystals, filtered, washed with ethanol and dried in the air. The melting point is 120-125 degrees.
POM1, POM2, POM7은 고체 파우더 상태로 제조하며, 각각 물에 녹여 수용성 절삭유를 제조한다(도 1 참조).POM1, POM2, and POM7 are prepared in a solid powder state, and each dissolved in water to prepare a water-soluble cutting oil (see FIG. 1).
따라서 본발명의 제조방법에 의해 제조된 친환경 수용성 절삭유는 강한 산화력을 가져서 향균, 탈취 기능이 있으며, 독성이 없으며, 물과 유기 용매에 대한 높은 용해도와 열적인 안정성을 가지고 있으며, 자외선-근가시선에서의 강한 흡수성을 가지며, 다양한 산화제에 의해 재산화 항균성이 높고 인체에 무해한 현저한 효과가 있다.Therefore, the eco-friendly water-soluble cutting oil produced by the manufacturing method of the present invention has strong oxidizing power, has antibacterial and deodorizing functions, is non-toxic, has high solubility in water and organic solvents and thermal stability, and is It has a strong absorbency of oxidizing agents, has high reoxidation and antibacterial properties by various oxidizing agents, and has a remarkable effect harmless to the human body.
Claims (4)
상기 수용액을 Na2MoO4 ·2H2O수용액에 가한 후 H3PO4를 넣어 혼합물 용액을 제조하는 단계;
상기 혼합물 용액을 가열하는 단계;
상기 가열된 혼합물 용액을 식히는 단계;
상기 식힌 혼합물 용액에 KCl 70-80 g을 넣는 단계;
생성된 침전물을 거른 후 황산수용액을 넣어 재결정하는 단계;
재결정을 거른 후 찬물로 씻고 공기중에서 건조시키는 단계;를 포함하여 제조되는 것을 특징으로 하는 생체적합성 항균제(POM)를 함유한 친환경 수용성 절삭유The method of claim 1, wherein the polyoxometalate 2 (polyoxometalate 2, POM 2) is prepared by dissolving NaVO 3 in water to prepare an aqueous solution;
preparing a mixture solution by adding the aqueous solution to an aqueous solution of Na 2 MoO 4 · 2H 2 O and then adding H 3 PO 4 ;
heating the mixture solution;
cooling the heated mixture solution;
adding 70-80 g of KCl to the cooled mixture solution;
Recrystallization by adding an aqueous sulfuric acid solution after filtering the resulting precipitate;
After recrystallization, washing with cold water and drying in air; Eco-friendly water-soluble cutting oil containing biocompatible antibacterial agent (POM), characterized in that it is manufactured including
(NH4)6Mo7O24 ·4H2O를 물에 넣어 녹이는 단계;
H2O2를 넣는 단계;
에탄올을 넣은 후 냉장고에 보관하여 결정을 얻는 단계;
상기 결정을 거른 후 에탄올로 씻어 공기중에서 건조시키는 단계;를 포함하여 제조되는 것을 특징으로 하는 생체적합성 항균제(POM)를 함유한 친환경 수용성 절삭유According to claim 1, wherein the polyoxometalate 7 (polyoxometalate 7, POM 7) is
(NH 4 ) 6 Mo 7 O 24 · 4H 2 O dissolved in water;
Putting H 2 O 2 ;
obtaining crystals by adding ethanol and storing in a refrigerator;
After filtering the crystals, washing with ethanol and drying in air; Eco-friendly water-soluble cutting oil containing a biocompatible antibacterial agent (POM), characterized in that it is manufactured including
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