KR101056580B1 - Detergent Composition and Cleaning Method of Heat Exchanger Using Coal Sorbent Oil - Google Patents
Detergent Composition and Cleaning Method of Heat Exchanger Using Coal Sorbent Oil Download PDFInfo
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- KR101056580B1 KR101056580B1 KR1020040110154A KR20040110154A KR101056580B1 KR 101056580 B1 KR101056580 B1 KR 101056580B1 KR 1020040110154 A KR1020040110154 A KR 1020040110154A KR 20040110154 A KR20040110154 A KR 20040110154A KR 101056580 B1 KR101056580 B1 KR 101056580B1
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- heat exchanger
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- absorbent
- oil
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- 238000004140 cleaning Methods 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000003599 detergent Substances 0.000 title claims abstract description 20
- 239000003245 coal Substances 0.000 title claims abstract description 5
- 239000002594 sorbent Substances 0.000 title description 2
- 239000002250 absorbent Substances 0.000 claims abstract description 58
- 230000002745 absorbent Effects 0.000 claims abstract description 58
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 54
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000010802 sludge Substances 0.000 claims abstract description 26
- 238000011084 recovery Methods 0.000 claims abstract description 10
- 239000002283 diesel fuel Substances 0.000 claims abstract description 9
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims description 42
- 235000019445 benzyl alcohol Nutrition 0.000 claims description 14
- 238000004821 distillation Methods 0.000 claims description 13
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 12
- 238000009835 boiling Methods 0.000 claims description 11
- IANQTJSKSUMEQM-UHFFFAOYSA-N 1-benzofuran Chemical compound C1=CC=C2OC=CC2=C1 IANQTJSKSUMEQM-UHFFFAOYSA-N 0.000 claims description 10
- 238000010521 absorption reaction Methods 0.000 claims description 10
- 239000000571 coke Substances 0.000 claims description 7
- 235000010290 biphenyl Nutrition 0.000 claims description 6
- 239000004305 biphenyl Substances 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 230000009969 flowable effect Effects 0.000 claims 1
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 4
- 238000004090 dissolution Methods 0.000 description 21
- 230000000694 effects Effects 0.000 description 16
- 230000001965 increasing effect Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- SIKJAQJRHWYJAI-UHFFFAOYSA-N Indole Chemical compound C1=CC=C2NC=CC2=C1 SIKJAQJRHWYJAI-UHFFFAOYSA-N 0.000 description 4
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000032683 aging Effects 0.000 description 3
- -1 aromatic organic compounds Chemical class 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 230000000087 stabilizing effect Effects 0.000 description 3
- QNLZIZAQLLYXTC-UHFFFAOYSA-N 1,2-dimethylnaphthalene Chemical compound C1=CC=CC2=C(C)C(C)=CC=C21 QNLZIZAQLLYXTC-UHFFFAOYSA-N 0.000 description 2
- QPUYECUOLPXSFR-UHFFFAOYSA-N 1-methylnaphthalene Chemical compound C1=CC=C2C(C)=CC=CC2=C1 QPUYECUOLPXSFR-UHFFFAOYSA-N 0.000 description 2
- YBYIRNPNPLQARY-UHFFFAOYSA-N 1H-indene Chemical compound C1=CC=C2CC=CC2=C1 YBYIRNPNPLQARY-UHFFFAOYSA-N 0.000 description 2
- QIMMUPPBPVKWKM-UHFFFAOYSA-N 2-methylnaphthalene Chemical compound C1=CC=CC2=CC(C)=CC=C21 QIMMUPPBPVKWKM-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000004939 coking Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- PQNFLJBBNBOBRQ-UHFFFAOYSA-N indane Chemical compound C1=CC=C2CCCC2=C1 PQNFLJBBNBOBRQ-UHFFFAOYSA-N 0.000 description 2
- PZOUSPYUWWUPPK-UHFFFAOYSA-N indole Natural products CC1=CC=CC2=C1C=CN2 PZOUSPYUWWUPPK-UHFFFAOYSA-N 0.000 description 2
- RKJUIXBNRJVNHR-UHFFFAOYSA-N indolenine Natural products C1=CC=C2CC=NC2=C1 RKJUIXBNRJVNHR-UHFFFAOYSA-N 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- XYTKCJHHXQVFCK-UHFFFAOYSA-N 1,3,8-trimethylnaphthalene Chemical compound CC1=CC=CC2=CC(C)=CC(C)=C21 XYTKCJHHXQVFCK-UHFFFAOYSA-N 0.000 description 1
- ZMXIYERNXPIYFR-UHFFFAOYSA-N 1-ethylnaphthalene Chemical compound C1=CC=C2C(CC)=CC=CC2=C1 ZMXIYERNXPIYFR-UHFFFAOYSA-N 0.000 description 1
- 239000004792 Prolene Substances 0.000 description 1
- CWRYPZZKDGJXCA-UHFFFAOYSA-N acenaphthene Chemical compound C1=CC(CC2)=C3C2=CC=CC3=C1 CWRYPZZKDGJXCA-UHFFFAOYSA-N 0.000 description 1
- 230000001464 adherent effect Effects 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- RFRXIWQYSOIBDI-UHFFFAOYSA-N benzarone Chemical compound CCC=1OC2=CC=CC=C2C=1C(=O)C1=CC=C(O)C=C1 RFRXIWQYSOIBDI-UHFFFAOYSA-N 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- RJTJVVYSTUQWNI-UHFFFAOYSA-N beta-ethyl naphthalene Natural products C1=CC=CC2=CC(CC)=CC=C21 RJTJVVYSTUQWNI-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 239000003623 enhancer Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000008137 solubility enhancer Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/261—Alcohols; Phenols
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3263—Amides or imides
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3281—Heterocyclic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
- C11D2111/20—Industrial or commercial equipment, e.g. reactors, tubes or engines
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/40—Specific cleaning or washing processes
- C11D2111/44—Multi-step processes
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Detergent Compositions (AREA)
Abstract
본 발명은 경유회수설비 열교환기의 세정제 조성물 및 세정방법, 보다 상세하게는 (a) 흡수세정제 20~40 부피%; (b) 디메틸포름아마이드(Dimethyl formamide) 15-35 부피%; (c) 노말 메틸 2-파이롤리돈 (N-methyl 2-pyrrolidone; NMP) 10-30 부피%; 및 (d) 벤질알콜 5-10부피%를 포함하여 이루어지는 세정제 조성물, 및 석탄계 흡수유를 이용하는 열교환기 전, 후단을 연결하여 상기 세정제 조성물을 고압하에 강제 순환시키는 단계를 포함하여 이루어지는 열교환기의 세정방법에 관한 것이다. The present invention is a detergent composition and cleaning method of the diesel oil recovery equipment heat exchanger, and more specifically, (a) 20 to 40% by volume of absorbent cleaner; (b) 15-35% by volume of dimethyl formamide; (c) 10-30% by volume normal methyl 2-pyrrolidone (N-methyl 2-pyrrolidone; NMP); And (d) a detergent composition comprising 5-10% by volume of benzyl alcohol, and a step of connecting the front and rear ends of the heat exchanger using coal-based absorbent oil to force circulation of the detergent composition under high pressure. It is about a method.
본 발명의 세정제 조성물 및 세정방법에 의하면 흡수유에서 발생되는 슬러지가 열교환기에 부착함으로 인한 열교환 효율의 감소 및 열교환기 배관 등의 폐쇄를 해결하여 처리 시간의 절감 및 운전 효율을 제고할 수 있다. According to the cleaning composition and the cleaning method of the present invention, by reducing the heat exchange efficiency and the closing of the heat exchanger pipe due to the sludge generated in the absorbent oil attached to the heat exchanger, it is possible to reduce the processing time and improve the operating efficiency.
세정제 조성물, 열교환기, 경유회수설비, 슬러지, 노말 메틸 2-파이롤리돈, 디메틸포름아마이드, 벤질알콜, 흡수유Cleaner composition, heat exchanger, diesel recovery equipment, sludge, normal methyl 2-pyrrolidone, dimethylformamide, benzyl alcohol, absorbent oil
Description
도 1은 흡수유 열교환기 전후 공정을 보완한 본 발명의 세정 공정도에 관한 개략도이다.1 is a schematic view of a cleaning process diagram of the present invention to supplement the process before and after absorption oil heat exchanger.
도 2는 용해비율 vs. 디메틸포름아마이드의 첨가비율(a), 용해비율 vs. 노말 메틸 2-파이롤리돈의 첨가비율(b), 용해비율 vs. 벤질알콜의 첨가비율(c)에 대한 결과를 도시한 도면이다.2 is the dissolution ratio vs. Addition ratio (a), dissolution ratio vs. of dimethylformamide Addition ratio (b), dissolution ratio of normal methyl 2-pyrrolidone. The figure which shows the result with respect to the addition ratio (c) of benzyl alcohol.
도 3은 흡수세정제의 첨가비율에 따른 용해비율의 변화를 도시한 도면이다.
3 is a view showing a change in the dissolution rate according to the addition ratio of the absorption detergent.
본 발명은 경유회수설비의 열교환기의 세정제 조성물, 및 그를 이용하는 세정방법에 관한 것이다. 보다 상세하게는, 제철공정에서 다종의 석탄을 배합하여 코크스를 제조하는 건류공정에서 코크오븐가스 (coke oven gas: 이하 COG라고 한 다) 중에 일부 휘발성 유기물질인 벤젠, 톨루엔, 크실렌(Benzen, Tolune, Xylene: 이하 BTX라고 한다) 등의 방향족 유기화합물을 회수하는 경유회수설비 중의 흡수유 사용으로 인한 열교환기의 내부 부착물질을 세정하기 위한 세정제 조성물과 세정방법에 관한 것이다. The present invention relates to a cleaning composition of a heat exchanger of a diesel oil recovery facility, and a cleaning method using the same. More specifically, some volatile organic substances such as benzene, toluene, and xylene (Benzen, Tolune) in the coke oven gas (cog oven gas) are used in the coking oven (coke oven gas) process in which coking is made by mixing various types of coal in the steelmaking process. The present invention relates to a cleaning composition and a cleaning method for cleaning internal adherents of a heat exchanger due to the use of absorbent oil in a diesel oil recovery facility for recovering aromatic organic compounds such as Xylene (hereinafter referred to as BTX).
통상 경유회수설비 내에서는 흡수유에 의해서 흡수된 BTX를 증류 분리 시키는 가열공정과 냉각하여 흡수효과를 증대시키는 공정에서 열교환이 일어나는 온도의 변화에 의해서 흡수유의 변성이 일어나고, COG중의 불순물인 H2S, HCN, COS, CS2등의 가스 성분으로 인한 흡수유의 노화 현상이 일어난다. 이렇게 변성 노화된 흡수유 내에 생성된 슬러지가 열교환기 내에 부착하게 되어 배관 폐쇄를 일으키고, 이로 인해 열교환기 내부 면적이 감소하여 열효율이 떨어지게 된다. 따라서, 이런 문제를 해소하기 위하여 세정작업이 행해지고 있는데, 일반적으로 세정작업은 스팀과 알칼리세정제를 사용하고 있으나, 세정 시간이 길고 비용이 과다하며, 세정후의 오염 발생이 심한 문제가 존재하였다. In the diesel oil recovery system, in the heating process of distilling and separating the BTX absorbed by the absorbent oil and the process of cooling to increase the absorption effect, the change of the temperature of the absorbent oil occurs due to the change of the temperature at which the heat exchange takes place, and impurities such as H2S, HCN, Aging of absorbent oil occurs due to gas components such as COS and CS2. The sludge generated in the modified aging absorbent oil adheres to the heat exchanger, causing the pipe to be closed, thereby reducing the internal area of the heat exchanger, thereby reducing thermal efficiency. Therefore, in order to solve such a problem, a cleaning operation is performed. In general, the cleaning operation uses steam and an alkaline cleaner, but the cleaning time is long, the cost is excessive, and there is a problem of serious contamination after cleaning.
본 발명자들은 이런 문제점을 해소하고자 흡수유의 화학적 물리적 변성에 의해 발생된 슬러지의 용해성을 증대시킬수 있는 세정제를 개발하기 위해 흡수유의 기본성질에 대한 연구를 진행하였다. 본 발명자들의 연구결과에 따르면 흡수유의 성분으로는 벤조퓨란, 인덴, 인단, 나프탈렌, 큐놀린, 메틸나프탈렌, 에틸나프탈렌, 인돌, 디메틸나트탈렌, 에세나프탈렌, 트리메틸나프탈렌, 프로렌 등의 수십종이 존재하며, 이들 성분들로 인해 공정상에서 흡수유의 열화진행이 빨라져서 슬러지의 생성이 과대해지며, 결과적으로 경유회수설비의 열교환기 및 기타 장치에서 배관의 폐쇄 등을 일으키게 된다는 것을 알게 되었다. In order to solve this problem, the present inventors have conducted research on the basic properties of absorbent oil in order to develop a cleaner capable of increasing the solubility of sludge caused by chemical and physical modification of the absorbent oil. According to the results of the present inventors, dozens of sorbents such as benzofuran, indene, indane, naphthalene, quinoline, methylnaphthalene, ethylnaphthalene, indole, dimethylnaphthalene, ethenaphthalene, trimethylnaphthalene, and prolene are present. It has been found that these components accelerate the deterioration of the absorbent oil in the process, resulting in excessive sludge production and, consequently, the closing of pipes in heat exchangers and other devices of diesel oil recovery facilities.
따라서, 본 발명의 목적은 흡수유에서 발생되는 슬러지가 열교환기에 부착함으로 인한 열교환 효율의 감소 및 열교환기 배관 등의 폐쇄를 해결하여 처리 시간의 절감 및 운전 효율을 제고할 수 있는 신규한 세정제 조성물 및 세정방법을 제공하고자 하는 것이다. Accordingly, an object of the present invention is to solve the reduction of heat exchange efficiency and the closing of heat exchanger piping due to the sludge generated in the absorbent oil adheres to the heat exchanger, a novel cleaning composition which can reduce the processing time and improve the operating efficiency and It is to provide a cleaning method.
이하에서, 본 발명을 상세히 설명하고자 한다.Hereinafter, the present invention will be described in detail.
본 발명은 경유회수설비 열교환기의 세정제 조성물 및 세정방법에 관한 것이다.The present invention relates to a cleaning composition and a cleaning method of a diesel oil recovery facility heat exchanger.
보다 구체적으로, 본 발명의 세정제 조성물은 More specifically, the cleaning composition of the present invention
(a) 흡수세정제 20~40 부피%; (a) 20-40% by volume of absorbent cleaner;
(b) 디메틸포름아마이드(Dimethyl formamide) 15-35 부피%; (b) 15-35% by volume of dimethyl formamide;
(c) 노말 메틸 2-파이롤리돈 (N-methyl 2-pyrrolidone; NMP) 10-30 부피%; 및 (c) 10-30% by volume normal methyl 2-pyrrolidone (N-methyl 2-pyrrolidone; NMP); And
(d) 벤질알콜 5-10부피% (d) 5-10% by volume benzyl alcohol
를 포함하여 이루어진다.It is made, including.
상기에서, (a) 흡수세정제는 코크스를 제조하는 과정에서 발생된 타르를 증류탑에서 벤조퓨란 비등점인 173 ℃ 이상에서 증류하여 라이트오일을 제거하고, 미증물을 다시 증류탑에서 바이페닐 비등점 255℃에서 증류하여, 이 증류물을 냉각기 를 통하여 냉각시켜 제조되는 것을 특징으로 한다.In the above, (a) the absorbent cleaner is distilled tar generated in the process of preparing the coke at 173 ℃ or more of the benzofuran boiling point in the distillation column to remove the light oil, and distillate the distillate at the biphenyl boiling point 255 ℃ again in the distillation column It is characterized in that the distillate is produced by cooling through a cooler.
열교환기의 세정제 조성물을 제조하기 위해서는, 흡수유에 함유된 방향족의 동질성 물질을 흡수하는 조성물로 효과를 높이기 위해서 흡수세정제를 사용하여야 한다. 본 발명자들의 연구결과에 따르면, 벤조퓨란의 비등점 이상의 조성물이 효과적인 것으로 나타났으며, 비등점이 바이페닐 이상의 물질은 흡수효과는 있지만 세정효과가 미미하므로 역시 슬러지화되어 흡수유 슬러지 부착물을 제거하는 데는 그다지 효과적이 못한 것으로 나타났다. In order to prepare the cleaning composition of the heat exchanger, an absorbent cleaner should be used in order to enhance the effect of the composition absorbing aromatic homogeneous substances contained in the absorbent oil. According to the results of the present inventors, the composition above the boiling point of benzofuran was found to be effective, and the substance having a boiling point of biphenyl or higher has an absorption effect but a slight cleaning effect, so it is also sludged to remove absorbed oil sludge deposits. It was found to be ineffective.
즉, 본 발명의 흡수세정제는 코크스를 제조하는 과정에서 발생된 타르를 증류탑에서 벤조퓨란의 비등점인 173℃ 이상에서 증류하여 라이트오일을 제거하고, 미증물을 다시 증류탑에서 바이페닐 비등점 255℃에서 증류하여, 이 증류물을 냉각기를 통하여 냉각시켜 제조된 것을 사용한다.That is, the absorbent cleaner of the present invention distills the tar generated in the process of producing coke at 173 ℃ or more boiling point of benzofuran in the distillation column to remove the light oil, and distillation of the fines at the biphenyl boiling point of 255 ℃ again in the distillation column The distillate is cooled and cooled by a cooler.
이 흡수세정제 자체로도 열교환기 배관 등에 부착된 물질을 제거하기 위한 세정의 효과는 가지고 있으나, 디메틸포름아마이드, 노말 메틸 2-파이롤리돈, 및 벤질알콜이 적정비율로 첨가된다면 그 효과는 더욱 증대된다는 것이 본 발명자들의 연구에 의해 밝혀졌다.This absorbent cleaner itself has the effect of cleaning to remove substances adhering to heat exchanger pipes, but the effect is further increased if dimethylformamide, normal methyl 2-pyrrolidone, and benzyl alcohol are added at an appropriate ratio. It has been found by the study of the inventors.
노말 메틸 2-파이롤리돈은 흡수유 내에 존재하는 고형성분, 즉 나프탈렌, 2-메틸나프탈렌, 인돌, 바이페닐, 아세나프텐, 프로렌 등의 성분의 용해성을 증진시켜서 슬러지의 발생을 억제하며, 배관에 부착되는 성질을 개선하는 효과를 지닌다. 또한, 첨가성분 중의 하나인 디메틸포름아마이드는 흡수세정제 조성물 내에서 안정적인 조성을 유지하도록 하는 안정화조제로 기여한다. 추가로, 벤질알콜의 경우는 고형성분의 슬러지의 용해성을 증진시키는 효과를 동반하고 있다. Normal methyl 2-pyrrolidone suppresses the formation of sludge by enhancing the solubility of the solid components present in the absorbent oil, that is, components such as naphthalene, 2-methylnaphthalene, indole, biphenyl, acenaphthene, and proren. Has the effect of improving the adhesion properties. In addition, dimethylformamide, which is one of the additive ingredients, contributes to the stabilizing aid to maintain a stable composition in the absorbent detergent composition. In addition, benzyl alcohol is accompanied by the effect of improving the solubility of the sludge of the solid component.
본 발명의 세정제 조성물은 제조된 흡수세정제와 노말 메틸 2-파이롤리돈, 디메틸포름아마이드와 벤질 알코올이 흡수세정제 20-40 부피%, 디메틸포름아마이드 15-35 부피%, 노말 메틸 2-파이롤리돈(NMP) 10-30 부피% 및 벤질알콜 5-10 부피%의 조성으로 존재하는 것이 바람직하다. The cleaning composition of the present invention comprises 20-40% by volume of the absorbent detergent prepared with normal methyl 2-pyrrolidone, dimethylformamide and benzyl alcohol, 15-35% by volume of dimethylformamide, and normal methyl 2-pyrrolidone. (NMP) preferably at a composition of 10-30% by volume and 5-10% by volume benzyl alcohol.
세정제 조성물 중에 흡수세정제가 20 부피% 미만으로 존재하면 세정효과의 저하를 초래하며, 40 부피%를 넘는 경우는 세정효과를 높이는 용해성 증진제로 사용되는 노말 메틸 2-파이롤리돈과 안정화조제인 디메틸포름아마이드와 벤질알콜의 함량이 줄어들게 된다. 따라서, 본 발명에서는 흡수세정제가 20-40 부피%로 존재하는 것이 바람직하다. The presence of less than 20% by volume of the absorbent detergent in the cleaning composition leads to a deterioration of the cleaning effect, and in excess of 40% by volume, normal methyl 2-pyrrolidone used as a solubility enhancer to enhance the cleaning effect and dimethylform, a stabilizing aid The amide and benzyl alcohol content will be reduced. Therefore, in the present invention, it is preferable that the absorbent cleaner is present at 20-40% by volume.
또한 노말 메틸 2-파이롤리돈은 세정제 조성물 중에 10-30 부피%로 존재하는 것이 바람직하다. 만약 이것이 10부피% 미만으로 있을 경우는 고형성분을 용해하는 성능이 저하되며, 30 부피%를 넘는 경우는 흡수세정제의 양이 줄어들어서 세정의 효과가 저하된다. It is also preferred that normal methyl 2-pyrrolidone is present in the detergent composition at 10-30% by volume. If it is less than 10% by volume, the performance of dissolving the solid component is degraded, and if it exceeds 30% by volume, the amount of the absorbent detergent is reduced to reduce the effectiveness of the cleaning.
추가로, 디메틸포름아마이드는 세정제 조성물 중에 15-35부피%로 존재하는 것이 바람직하다. 디메틸포름아마이드가 15부피% 미만일 경우 안정화조제로서의 성능이 그다지 발휘되지 못하며, 35부피%를 넘는 경우는 사용할 필요가 없는 것으로 나타났다. 또한 벤질알콜은 벤질의 환형고리형상이 흡수세정제와 안정하게 혼합되어 안정화제로서의 역할을 함으로써 세정효과를 증가시키는 것이 가능하며, 세정제 조성물 중에는 5-10 부피%로 혼합되는 것이 바람직하다. 5부피% 미만에서는 안정화 효과가 미미하고, 10부피%를 넘는 경우는 안정된 상태 이상으로 첨가하게 되는 것이 되므로 이 이상 첨가할 필요가 없으며 또 그 이상 첨가 시에는 세정효과를 증진시키는 성분이 적게 함유되어 세정효과가 저하되는 문제가 존재한다.In addition, dimethylformamide is preferably present in the detergent composition at 15-35% by volume. When dimethylformamide is less than 15% by volume, the performance as a stabilizing aid is not exhibited very much, and when it exceeds 35% by volume it is not necessary to use. In addition, benzyl alcohol is capable of increasing the cleaning effect by the cyclic ring shape of benzyl is stably mixed with the absorption detergent to act as a stabilizer, it is preferable to be mixed at 5-10% by volume in the cleaning composition. If it is less than 5% by volume, the stabilization effect is insignificant, and if it exceeds 10% by volume, it will be added in a stable state or more. Therefore, it is not necessary to add more than this. There is a problem that the cleaning effect is lowered.
본 발명은 또한, 본 발명의 세정제 조성물을 이용하는 경유회수설비 열교환기의 세정방법에 관한 것이다.The present invention also relates to a cleaning method of a diesel oil recovery facility heat exchanger using the cleaning composition of the present invention.
보다 상세하게는, 본 발명의 경유회수설비 열교환기의 세정방법은 석탄계 흡수유를 이용하는 열교환기 전, 후단을 연결시켜 펌프를 사용하여 상기 세정제 조성물을 고압하에 강제 순환시키는 단계를 포함하여 이루어짐을 특징으로 한다.More specifically, the cleaning method of the diesel oil recovery equipment heat exchanger of the present invention comprises the step of forcibly circulating the detergent composition under a high pressure using a pump by connecting before and after the heat exchanger using coal-based absorbent oil. It is done.
상기 단계에서 압력은 5kgf/cm2 이상의 고압인 것이 세정의 효과를 증가시킬 수 있어 바람직하며, 압력이 낮으면 세정시간이 길어지는 단점이 있다. In this step, the pressure is preferably 5kgf / cm 2 or more to increase the effect of cleaning, and the low pressure has a disadvantage that the cleaning time is long.
본 발명의 세정방법은 열교환기 입구에 원심분리기를 설치하고, 원심분리에 의한 유동성 흡수유는 공정에 피드백시키고, 점도성의 슬러지 함유 흡수유는 탈피치탑에서 증류시키고 피치화된 물질은 제거후 응축기에서 응축시켜 흡수유에 피드백시키는 공정을 더 포함할 수 있다. In the cleaning method of the present invention, a centrifuge is installed at the inlet of the heat exchanger, the fluid absorbent oil by centrifugation is fed back to the process, the viscous sludge-containing absorbent oil is distilled in the de-pitching column, and the pitched material is removed in the condenser. The method may further include condensing and feeding back the absorbent oil.
열교환기에 부착된 슬러지의 세정작업 이외에, 열교환기에 부착성이 큰 흡수유의 노화성분의 슬러지를 원심분리하여 증류 탈피치탑에서 운전하여 제거하고, 증발 흡수유는 응축시켜 피드백시켜 사용하는 공정을 더 추가하면 흡수유 내에 생성된 슬러지로 인해 열교환기 배관 폐쇄 등의 문제가 더욱 원활히 해결될 수 있어 처리 시간의 절감 및 운전 효율이 더욱 높아지게 된다. In addition to the cleaning of the sludge attached to the heat exchanger, the sludge of the aging component of the absorbent oil having high adhesion to the heat exchanger is centrifuged and removed by operation in a distillation depitch column. Due to the sludge generated in the absorbent oil, problems such as heat exchanger pipe closing can be more smoothly solved, thereby reducing processing time and increasing operating efficiency.
즉, COG를 정제하기 위해서 흡수유를 사용하는 공정에서 열교환기 입구에 기 존에 설치되지 않는 원심분리기를 설치하여 미세하게 생성된 슬러지를 분리하는 과정에서 완전히 슬러지만 분리하기는 어려운 점이 있어서, 슬러지를 원심분리방식으로 슬러지가 함유된 점도가 높은 상태와 슬러지 함유 상태가 적은 유동성이 큰 상태로 분리하며, 점도성이 많은 분리된 슬러지 함유 흡수유는 탈피치탑에서 피치성분을 증류시켜서 제거하는 공정으로 보내며, 증류된 물질은 응축기에서 응축시며 사용중인 흡수유에 포함시켜서 운전을 진행한다. 또한 유동성의 흡수유는 바로 공정에 포함시키는 공정을 거친다. That is, in the process of using absorbent oil to purify COG, the sludge is completely sludge in the process of separating finely produced sludge by installing a centrifuge not existing in the heat exchanger inlet. Centrifugation method separates the sludge-containing sludge into a high fluidity state with a low sludge-containing state, and the separated sludge-containing absorbent oil with a high viscosity is a process of distilling the pitch component in a de-pitching column. The distilled material is condensed in the condenser and included in the absorbent oil in use for operation. In addition, the fluid absorbent oil goes through the process of being included in the process.
본 발명에서 흡수유 열교환기 전후 공정을 보완한 본 발명의 세정공정도를 제 1도에 나타냈다. In the present invention, the cleaning process diagram of the present invention complementing the process before and after the absorption oil heat exchanger is shown in FIG.
이하 본 발명의 실시예를 통하여 설명한다.
Hereinafter will be described through an embodiment of the present invention.
실험예 1Experimental Example 1
본 실험예는 코크스 제조시 발생되는 코울타르 기존 증류공정인 200℃와 300℃사이에서 증류한 흡수유 시료와, 원료 코크스를 제조하는 과정에서 발생된 타르를 증류탑에서 벤조퓨란 비등점173℃ 이상에서 증류하여 라이트오일을 제거하고, 미증물을 다시 증류탑에서 바이페닐 비등점 255℃에서 증류하여, 이 증류물을 냉각기를 통하여 냉각하여 제조한 흡수세정제를 비교하기 위한 시험으로 열교환기에 부착된 슬러지의 용해시험을 실시하였다. 25℃의 온도에서 슬러지 50g에 일반 흡수유와 흡수세정제를 각각 200cc씩 채취하여 혼합한 후 에지테이터로 100RPM 으로 10분간 혼합하고, 각각 필터링한 후에 슬러지의 중량을 측정하고, 초기중량대비 용해비 율을 계산하였다. 그 결과를 표 1에 나타내었다.This Experimental Example is a sample of absorbent oil distilled between 200 ° C and 300 ° C, which is a coartar existing distillation process produced from coke, and the tar generated in the process of preparing raw material coke is distilled at a benzofuran boiling point of 173 ° C or higher in a distillation column. The light oil was removed, and the distillate was distilled again in a distillation column at a biphenyl boiling point of 255 ° C., and the distillate was cooled through a cooler to compare the absorbent detergent prepared. Was carried out. 50 g of sludge at a temperature of 25 ° C, 200cc of normal absorbent oil and absorbent cleaner were collected and mixed, and then mixed with 100rpm for 10 minutes with edge data, and after each filtering, the weight of the sludge was measured and the ratio of dissolution to initial weight was measured. Was calculated. The results are shown in Table 1.
상기 표1에서 보는 바와 같이, 기존공정의 흡수유와 본 발명의 흡수세정제 모두는 채취된 슬러지의 용해성이 있어 세정효과를 가지는 것으로 나타났지만, 본 발명의 흡수세정제는 95% 이상인 98.7%를 나타냈으며, 기존의 흡수유는 87.5%의 값을 나타내고 있다. 공정에 사용하기 위해서는 세정효과가 90% 이상은 되어야 하므로, 본 발명의 흡수세정제가 배관에 부착되는 슬러지 제거에 더 적합함을 알 수 있다.
As shown in Table 1, both the absorbent oil of the conventional process and the absorbent cleaner of the present invention were found to have a cleaning effect due to the solubility of the collected sludge, but the absorbent cleaner of the present invention exhibited 98.7% of 95% or more. The existing absorbent oil shows a value of 87.5%. Since the cleaning effect should be 90% or more for use in the process, it can be seen that the absorbent cleaner of the present invention is more suitable for removing sludge adhered to the pipe.
실험예 2Experimental Example 2
본 실험예에서는 실험예 1과 같은 방법으로 시험을 실시하고, 용해시간을 3분으로 단축하여 시험을 하였다. 본 발명의 흡수세정제에 첨가제인 용해증진제로 노말 메틸2-파이롤리돈과, 디메틸포름아마이드 및 벤질알콜의 첨가량을 결정하기 위해서, In this Experimental Example, the test was carried out in the same manner as in Experimental Example 1, and the dissolution time was shortened to 3 minutes. In order to determine the addition amount of normal methyl 2-pyrrolidone, dimethylformamide and benzyl alcohol as a dissolution enhancer which is an additive to the absorption detergent of the present invention,
A) 흡수세정제에 디메틸포름아마이드를 각각 10, 15, 20, 25, 30, 35, 40부피%로 첨가하고 각각의 시료에 대해서 실험예 1과 같은 방법으로 시험하여 용해비율을 측정하였다. A) Dimethylformamide was added to the absorbent detergent at 10, 15, 20, 25, 30, 35 and 40% by volume, respectively, and the dissolution ratio was measured by testing in the same manner as in Experiment 1 for each sample.
B) 흡수세정제에 노말 메틸2-파이롤리돈을 각각 5, 10, 20, 30, 40 부피%로 첨가하고 각각의 시료에 대해서 실험예 1과 같은 방법으로 시험하여 용해비율을 측정하였다.B) 5, 10, 20, 30, 40% by volume of normal methyl 2-pyrrolidone was added to the absorbent cleaner, and the dissolution ratio was measured by testing in the same manner as in Experimental Example 1 for each sample.
C) 흡수세정제에 벤질알콜을 각각 2.5, 5, 7.5, 10.0, 12.5 부피%로 첨가하고 각각의 시료에 대해서 실험예 1과 같은 방법으로 시험하여 용해비율을 측정하였다.C) Benzyl alcohol was added at 2.5, 5, 7.5, 10.0, and 12.5% by volume to the absorbent cleaner, and the dissolution ratio was measured by testing in the same manner as in Experimental Example 1 for each sample.
각각의 시험결과를 제 2도에 나타내었다. 제 2도의 (a)에서 있어서 디메틸포름아마이드의 바람직한 첨가량은 용해비율이 90% 이상을 만족시키는 범위에서 선택하였다. 디메틸포름아마이드가 15부피% 미만에서는 용해비율이 85%로 저조한 상태였으며, 첨가량이 40부피%로 증가하여도 감소하는 경향을 나타내었다. 결론적으로, 첨가량이 15-35부피%가 바람직한 범위로 선정되었다. Each test result is shown in FIG. In (a) of FIG. 2, the preferable addition amount of dimethylformamide was selected in the range whose dissolution ratio satisfy |
제 2도의 (b)에서 있어서 역시 노말 메틸 2-파이롤리돈의 바람직한 첨가량은 용해비율이 90%이상이 되는 조건을 만족시키는 범위에서 선택하였다. 노말 메틸 2-파이롤리돈의 함량이 5부피%에서는 용해비율이 83%로 저조한 상태이며, 그 함량이 40부피%로 증가하여도 용해비율이 감소하는 경향을 나타내었다. 결론적으로 본 발명에서 노말 메틸2-파이롤리돈의 첨가량은 10-30부피%가 바람직한 범위로 선정되었다 In (b) of FIG. 2, the preferable addition amount of normal methyl 2-pyrrolidone was also selected in the range which satisfy | fills the conditions for which dissolution rate becomes 90% or more. When the content of normal methyl 2-pyrrolidone was 5% by volume, the dissolution ratio was low at 83%, and even when the content was increased to 40% by volume, the dissolution ratio tended to decrease. In conclusion, in the present invention, the amount of normal methyl 2-pyrrolidone added was selected to be in the range of 10-30% by volume.
마지막으로, 제 2도의 (c)에서 있어서 벤질알콜의 바람직한 첨가량은 용해비율이 90%이상이 되는 조건을 만족시키는 범위에서 선택하였다. 벤질알콜의 함량이 2.5부피%에서는 용해비율이 83%로 저조한 상태이며, 첨가량이 12.5부피%로 증가하 여도 용해비율이 감소하는 경향을 나타내었다. 결론적으로, 본 발명에서 벤질알콜의 첨가량은 5-10부피%가 바람직한 범위로 선정되었다.
Finally, in (c) of FIG. 2, the preferable addition amount of benzyl alcohol was selected in the range which satisfy | fills the conditions for which a melt ratio becomes 90% or more. In the case of benzyl alcohol content of 2.5% by volume, the dissolution rate was low at 83%, and the dissolution rate was decreased even when the addition amount was increased to 12.5% by volume. In conclusion, in the present invention, the amount of benzyl alcohol added was 5-10% by volume.
실험예 3Experimental Example 3
흡수유세정제의 비율을 결정하기 위해서, 흡수세정제의 비율을 변화시키면서 디메틸포름아마이드와 노말 메틸 2-파이롤리돈 및 벤질알콜의 비율을 조절하여 시험을 실시하였다. 흡수세정제 첨가비율의 결정을 위해서 나머지 3성분을 효과 있는 중앙값기준으로 혼합비를 일정하게 하여 혼합 조제된 시료에 흡수세정제의 비율을 10-50부피%까지 변화시키면서 실험예 2와 같은 방법으로 시험을 진행하였다. 3 성분, 즉 디메틸포름아마이드: 노말 메틸 2-파이롤리돈: 벤질알콜의 혼합비는 25: 30: 7.5 (부피비)이다. In order to determine the ratio of the absorbent cleaner, the test was conducted by adjusting the ratio of dimethylformamide, normal methyl 2-pyrrolidone and benzyl alcohol while changing the ratio of the absorbent cleaner. In order to determine the rate of absorption detergent, the mixing ratio of the remaining three components was made constant based on the effective median value, and the test was conducted in the same manner as in Experimental Example 2 while changing the ratio of the absorption detergent to 10-50% by volume. It was. The mixing ratio of the three components, dimethylformamide: normal methyl 2-pyrrolidone: benzyl alcohol, is 25: 30: 7.5 (volume ratio).
흡수세정제의 비율 vs. 용해비율의 결과를 제 3도에 나타내었다. 용해비율이 95% 이상인 것을 만족스러운 기준으로 삼았을 때 흡수세정제가 10부피% 및 50부피%에서는 용해비율이 95% 미만으로 만족스럽지 못하며, 20-40부피%에서는 95% 이상의 조건을 만족하였다. Percentage of absorbent cleaner vs. The results of the dissolution ratio are shown in FIG. When satisfactory standards were set for the dissolution ratio of 95% or more, the dissolution rate was not satisfactory at less than 95% at 10% by volume and 50% by volume, and at least 95% at 20-40% by volume.
상술한 바와 같이 본 발명의 세정제 조성물 및 세정방법에 따르면 흡수유에서 발생되는 슬러지가 열교환기에 부착함으로 인한 열교환 효율의 감소 및 열교환기 배관 등의 폐쇄를 해결하여 처리 시간의 절감 및 운전 효율을 제고할 수 있다. As described above, according to the cleaning composition and the cleaning method of the present invention, the sludge generated in the absorbent oil adheres to the heat exchanger, thereby reducing the heat exchange efficiency and closing the heat exchanger pipe, thereby reducing processing time and improving operation efficiency. Can be.
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| JPH1068000A (en) | 1996-08-29 | 1998-03-10 | Hakuto Co Ltd | Cleaning composition for coating material pipe and cleaning of the same |
| KR0168486B1 (en) * | 1993-05-17 | 1999-01-15 | 야마다 시게아키 | Detergent, method and apparatus for cleaning |
| KR20030052379A (en) * | 2001-12-21 | 2003-06-27 | 주식회사 포스코 | Preparing method of absorption oil for refining of coke oven gas having improved yield and the absorption oil thereof |
| JP2004155821A (en) * | 2002-11-01 | 2004-06-03 | Tosoh Corp | Cleaning agent |
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| KR0168486B1 (en) * | 1993-05-17 | 1999-01-15 | 야마다 시게아키 | Detergent, method and apparatus for cleaning |
| JPH1068000A (en) | 1996-08-29 | 1998-03-10 | Hakuto Co Ltd | Cleaning composition for coating material pipe and cleaning of the same |
| KR20030052379A (en) * | 2001-12-21 | 2003-06-27 | 주식회사 포스코 | Preparing method of absorption oil for refining of coke oven gas having improved yield and the absorption oil thereof |
| JP2004155821A (en) * | 2002-11-01 | 2004-06-03 | Tosoh Corp | Cleaning agent |
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