KR102326485B1 - 냉간 필거용 내면 윤활제 조성물 - Google Patents

냉간 필거용 내면 윤활제 조성물 Download PDF

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KR102326485B1
KR102326485B1 KR1020200012549A KR20200012549A KR102326485B1 KR 102326485 B1 KR102326485 B1 KR 102326485B1 KR 1020200012549 A KR1020200012549 A KR 1020200012549A KR 20200012549 A KR20200012549 A KR 20200012549A KR 102326485 B1 KR102326485 B1 KR 102326485B1
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cold pilger
lubricating composition
decomposition
enhancer
improving agent
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KR1020200012549A
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KR20210099226A (ko
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박민영
한상진
박기범
차정우
이덕희
김경태
여평모
장정진
최상순
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한전원자력연료 주식회사
주식회사 에스에이치엘
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Priority to KR1020200012549A priority Critical patent/KR102326485B1/ko
Priority to US17/118,953 priority patent/US11492568B2/en
Priority to EP20215383.9A priority patent/EP3858956B1/en
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    • C—CHEMISTRY; METALLURGY
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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

본 발명은 지르코늄 합금 피복관의 냉간 필거용 윤활제 조성물에 관한 것으로, 특히 윤활성과 내부패성이 우수한 지르코늄 합금 피복관의 냉간 필거용 내면 윤활 조성물에 관한 것이다.

Description

냉간 필거용 내면 윤활제 조성물{The composition of inner lubricant for cold pilgering}
본 발명은 지르코늄 합금 피복관의 냉간 필거용 내면 윤활제 조성물에 관한 것으로, 특히 윤활성, 극압성 및 내마모성이 우수한 지르코늄 합금 피복관의 냉간 필거용 내면 윤활제 조성물에 관한 것이다.
핵연료집합체에서 피복관은 UO2 소결체를 노심의 냉각수와 분리하여 보호하는 역할을 하며, UO2 소결체에서 생성된 방사성 핵분열생성물이 냉각수로 방출되는 것을 방지하고 아울러 냉각수와 UO2 소결체를 분리하여 서로간의 화학반응을 방지한다. 피복관의 재질로는 고온의 냉각수에 대해 내부식성이 좋고 중성자흡수율이 낮은 지르코늄(Zirconium) 합금이 사용된다.
일반적인 피복관의 제조 공정은 지르코늄 원광으로부터 하프늄(Hf)을 제거한 후, 여러 합금 원소들을 첨가하여 주괴를 제조하며, 주괴로부터 열간 압출(Hot Extrusion)을 통해 TREX(Tube Reduced Extrusion)를 제조하고 TREX를 필거링(Pilgering) 이라는 냉간 가공과 열처리 공정의 반복을 통하여 두께와 직경을 감소시켜 최종적으로 지르코늄 합금 피복관을 제작하게 된다.
원자력발전소 내에 핵연료 피복관 및 구조재로 많이 사용되는 지르코늄합금 튜브의　치수성형시 사용되는 냉각윤활제는 일반산업용 스테인레스강관 또는 동합금관 제조와는 구별되는 냉간필거링이라는 특수한 공법을 사용한다.　지르코늄합금의 금속결정학적 집합조직 제어를 위해서는 각 필거단계별 단면적 감소율을 약 70%이상 가해야 함에 따라, 금형 및 심봉, 튜브에는 높은 하중이 가해지며 이에 따라 내마모성 및 극압성 등의 특성이 요구된다.
여기서 냉간 필거링을 함에 있어서 금형(Dies) 및 심봉(Mandrel)과 튜브 사이에 유막형성을 통한 윤활 및 마찰로 인한 열의 냉각을 위하여 전용 윤활유를 사용한다. 다만 기존의 윤활제는 피복관에 도포하더라도 마찰로 인한 내면 표면결함 발생 및 금형수명 저하 등 충분한 효과를 발휘하지 못하여 최종 원자력연료용 피복관 표면품질에 악영향을 미치고, 박테리아나 곰팡이류로 인한 부패로 악취가 발생하는 문제점이 있었다.
본 발명의 목적은 지르코늄 합금 피복관의 냉간 필거용 윤활제 조성물에 관한 것으로, 더욱 상세하게는 윤활성 및 내부패성이 향상된 지르코늄 합금 피복관의 냉간 필거용 내면 윤활유를 제공하는 것이다.
본 발명은 상술한 문제점을 해결하기 위해, 기유(base oil), 윤활 향상제, 내마모성 향상제(anti wear agent) 및 내부패성 향상제를 포함하고, 상기 윤활 향상제는 식물성 왁스(vegetable wax)이고 1.0 내지 1.4중량% 포함하는 것을 특징으로 하는 냉간 필거용 윤활 조성물을 제공한다.
바람직하게는 상기 식물성 왁스는 brazil wax일 수 있다.
바람직하게는 상기 내마모성 향상제를 1.4 내지 1.8 중량% 포함할 수 있다.
바람직하게는 상기 내부패성 향상제를 0.8 내지 1.2 중량% 포함할 수 있다.
바람직하게는 상기 내마모성 향상제는 벤젠 설포닉산(Benzene sulfonic acid), C10 내지 16의 알킬기, 칼슘염, 황산(sulfonic acid), C16 내지 C24의 알킬유도체 중 어느 하나 이상을 포함할 수 있다.
바람직하게는 상기 내부패성 향상제는 1,2-벤지소치아졸리-3-논(1,2-Benzisothiazolin-3-one), 포타슘 하이드록사이드(potassium hydroxide), 소듐 하이드록사이드(Sodium Hydroxide), 에틸렌 글리콜(Ethylene Glycol), 및 디하이드로젠 옥사이드(Dihydrogen Oxide) 중 어느 하나 이상을 포함할 수 있다.
본 발명은 내부패성이 뛰어나 부패로 인한 성능 저하 없이 장기간 사용, 보관이 가능하고, 윤활성능이 뛰어난 냉간 필거용 윤활 조성물을 제공한다.
도 1은 윤활유의 윤활성을 측정하기 위한 Micro Tapping Torque Test Machine의 사진이다.
도 2는 윤활유의 윤활성을 Micro Tapping Torque Test Machine을 이용한 측정결과를 나타낸 자료이다.
도 3는 윤활유의 극압성 및 내마모성을 측정하는는 4-ball test machine 사진이다.
도 4은 비교예 및 실시예에 의한 윤활유를 4-ball test 결과를 나타낸 사진이다.
도 5는 비교예 및 실시예에 의한 윤활유를 박테리아/펀지 측정 결과를 나타낸 사진이다
도 6의 좌측 그래프는 비교예 및 실시예에 의한 윤활유의 시간경과에 따른 pH변화를 나타낸다.
도 6의 우측 사진은 비교예 및 실시예에 의한 윤활유의 시간경과에 따른 pH변화를 나타낸 표이다.
이하 본 발명을 실시예를 통해 자세히 설명한다. 그러나 이는 예시적인 것에 불과하고 본 발명이 이러한 실시예에 의해 제한되는 것은 아니다.
비교예 1 및 실시예 1 내지 8 - 윤활 향상제
(단위 : 중량%)
비교예 실시예
1 1 2 3 4 5 6 7 8
물 78.4 78.0 77.8 77.6 77.4 77.2 77.0 76.8 76.6
Base oil 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0
지방산 6 6 6 6 6 6 6 6 6
pH 향상제 0.7 0.7 0.7 0.7 0.7 0.7 0.7 0.7 0.7
점성 조절제 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2
윤활 향상제 A1 0 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8
내마모성 향상제 A2 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2
내부패성
향상제		 A3 0.8 0.8 0.8 0.8 0.8 0.8 0.8 0.8 0.8
기타 첨가제 A4 8.7 8.7 8.7 8.7 8.7 8.7 8.7 8.7 8.7
A1 : Brazil wax
A2 : Benzen sulfonic acid, C10-16-alkyl derives 및 calcium salts의 혼합물
A3 : 1,2-벤지소치아졸리-3-논(1,2-Benzisothiazolin-3-one), 포타슘 하이드록사이드(potassium hydroxide), 소듐 하이드록사이드(Sodium Hydroxide), 에틸렌 글리콜(Ethylene Glycol), 및 디하이드로젠 옥사이드(Dihydrogen Oxide)의 혼합물
A4 : 부식방지제, 동물성 천연유지, 동물성 지방산 Ester 및 기타 첨가제
비교예 2 및 실시예 9 내지 15 - 내마모성 향상제
(단위 : 중량%)
비교예 실시예
2 9 10 11 12 13 14 15
물 78.8 77.8 77.6 77.4 77.2 77.0 76.8 76.6
Base oil 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0
지방산 6 6 6 6 6 6 6 6
pH 향상제 0.7 0.7 0.7 0.7 0.7 0.7 0.7 0.7
점성 조절제 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2
윤활 향상제 A1 1.4 1.4 1.4 1.4 1.4 1.4 1.4 1.4
내마모성
향상제		 A2 0 1.0 1.2 1.4 1.6 1.8 2.0 2.2
내부패성
향상제		 A3 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2
기타 첨가제 A4 7.7 7.7 7.7 7.7 7.7 7.7 7.7 7.7
비교예 3 및 실시예 16 내지 22 - 내부패성 향상제
(단위 : 중량%)
비교예 실시예
3 16 17 18 19 20 21 22
물 78.2 77.8 77.6 77.4 77.2 77.0 76.8 76.6
Base oil 3 3 3 3 3 3 3 3
지방산 6 6 6 6 6 6 6 6
pH 향상제 0.7 0.7 0.7 0.7 0.7 0.7 0.7 0.7
점성 조절제 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2
윤활 향상제 A1 1.4 1.4 1.4 1.4 1.4 1.4 1.4 1.4
내마모성 향상제 A2 1.8 1.8 1.8 1.8 1.8 1.8 1.8 1.8
내부패성
향상제		 A3 0 0.4 0.6 0.8 1.0 1.2 1.4 1.6
기타 첨가제 A4 7.7 7.7 7.7 7.7 7.7 7.7 7.7 7.7
실험예 1 - 윤활성 및 극압성 측정
윤활성 및 극압성 측정을 위해 Micro-tapping Torque Machine를 이용하여 S45C, 600rpm, 400N/m, 5.5mm 조건에서 수행하였다. Column max의 값이 작을수록 기기와의 마찰 및 저항이 작아지는 것을 뜻하며, 윤활성 및 극압성이 향상되는 것을 확인할 수 있다. Column Mean%는 한가지 제품을 100으로 지정하여 데이터의 평균을 나타낸 값으로 100 초과시 상대적으로 윤활성 및 극압성이 떨어지는 것을 확인할 수 있다. 비교예 및 실시예를 이용하여 해당 실험을 수행하였고, 그 결과를 아래 표에 나타내었다.
비교예1 실시예1 실시예2 실시예3 실시예4 실시예5 실시예6 실시예7 실시예8
Column MAX(Y축) 253.0 249.0 231.0 197.0 202.0 210.0 97.0 220.0 226.0
Column Mean% 112.6 109.3 104.8 91.4 95.0 96.6 100.0
(기준)		 101.3 104.3
비교예과 실시예의 비교를 통하여 식물성 왁스를 첨가하는 경우 극압성 및 윤활성이 증가하는 것을 확인할 수 있다. 이에 더하여 실시예 1내지 8간 비교를 통해 식물성왁스를 0.8 이상을 포함하는 경우 극압성 및 윤활성이 크게 향상되고, 1.2 이상 포함시 극압성 및 윤활성이 크게 저하 되는 것을 확인할 수 있다.
실험예 2 - 내마모성 측정
내마모성을 측정하기 위해 4-Ball Test를 이용하여 온도 75˚C, 1200 rpm, 50kg으로 30분간 수행하였고, 그 결과를 아래에 나타내었다.
비교예2 실시예9 실시예
10		 실시예
11		 실시예
12		 실시예
13		 실시예
14		 실시예
15
마모흔 측정값(mm) 0.78 0.65 0.63 0.55 0.55 0.56 0.61 0.61
마모흔(mm) 이 작을수록 마모도가 적다는 것이다. 위 표의 비교예 및 실시예의 비교를 통해 내마모성 향상제 첨가 시 내마모도가 증가할 수 있음을 확인할 수 있다. 또한 습윤 첨가제가 1.4중량% 첨가시 마모도가 크게 감소하였고, 1.8 중량% 이상 첨가되었을 때 마모도가 다시 증가하는 것을 확인할 수 있다.
실험예 3 - 내부패성 측정
비교예 3 및 실시예 16 내지 22에 대한 박테리아/펀지를 이용한 내부패성 실험결과를 도 5 및 도 6에 나타냈다. 박테리아/펀지 KIT에 정량의 사용유 (1ml)를 넣고 spreader를 이용하여 유제를 퍼트리고, 셰이킹 인큐베이터에 넣어 35℃ 하에서 균을 배양하였다. 48시간이 지난 후 박테리아/펀지 발생여부를 측정하였고, 점의 개수를 통해 내부패성을 평가하였다. 도 5를 참고하면 내부패성 향상제를 사용할 시 pH가 안정되는 것을 확인할 수 있다. 특히 1.2중량% 이상을 첨가하더라도 pH의 변화에 영향을 주지 못하는 것을 확인할 수 있다.
도 6를 참고하면, 내부패성 향상제를 0.8중량% 이상 첨가 시 박테리아 및 펀지가 발생하지 않았음을 확인할 수 있다.

Claims (6)

  1. 냉간 필거용 윤활 조성물에 있어서,
    기유(base oil); 및
    윤활 향상제;
    내마모성 향상제(anti wear agent); 및
    내부패성 향상제를 포함하고,
    상기 윤활 향상제는 식물성 왁스(vegetable wax)이고 1.0 내지 1.4중량% 포함하고,
    상기 냉간 필거용 윤활 조성물은 지르코늄 합금 피복관에 사용되는 것을 특징으로 하는 냉간 필거용 윤활 조성물.
  2. 제1항에 있어서,
    상기 식물성 왁스는 브라질란 왁스(Brazilan wax)인 것을 특징으로 하는 냉간 필거용 윤활 조성물.
  3. 제1항에 있어서,
    상기 내마모성 향상제를 1.4 내지 1.8 중량% 포함하는 것을 특징으로 하는 냉간 필거용 윤활 조성물.
  4. 제1항에 있어서,
    상기 내부패성 향상제를 0.8 내지 1.2 중량% 포함하는 것을 특징으로 하는 냉간 필거용 윤활 조성물.
  5. 제1항에 있어서,
    상기 내마모성 향상제는 벤젠 설포닉산(Benzene sulfonic acid), C10 내지 16의 알킬기, 칼슘염, 황산(sulfonic acid), C16 내지 C24의 알킬유도체 중 어느 하나 이상을 포함하는 것을 특징으로 하는 냉간 필거용 윤활 조성물.
  6. 제1항에 있어서,
    내부패성 향상제는 1,2-벤지소치아졸리-3-논(1,2-Benzisothiazolin-3-one), 포타슘 하이드록사이드(potassium hydroxide), 소듐 하이드록사이드(Sodium Hydroxide), 에틸렌 글리콜(Ethylene Glycol), 및 디하이드로젠 옥사이드(Dihydrogen Oxide) 중 어느 하나 이상을 포함하는 것을 특징으로 하는 냉간 필거용 윤활 조성물.
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