本文選題：重質(zhì)環(huán)烷酸 + 催化氧化�。� 參考：《中國石油大學(xué)(華東)》2015年碩士論文

【摘要】：工業(yè)酸洗除銹、油井酸化引起金屬腐蝕,加入緩蝕劑可以有效的減緩金屬腐蝕。咪唑啉類緩蝕劑是一種環(huán)保、高效、低毒的緩蝕劑。環(huán)烷酸是制備環(huán)烷基咪唑啉緩蝕劑的優(yōu)良原料。我國克拉瑪依煉油廠每年副產(chǎn)1萬噸左右的重質(zhì)環(huán)烷酸,來源廣、價格低廉,但是酸值低、粘度大、分子量大,應(yīng)用受限。本論文采取兩種措施:催化氧化和制備咪唑啉型緩蝕劑,來提高重質(zhì)環(huán)烷酸的工業(yè)附加值。首先,以氧氣為氧化劑,探究了催化劑種類及用量、氧化溫度、壓力、時間等因素的影響,并且采取二次補(bǔ)氧、加入添加劑來進(jìn)一步提高氧化深度。當(dāng)以環(huán)烷酸鹽為催化劑時,通過氧化,環(huán)烷酸酸值從95mgKOH/g升高到136mgKOH/g,環(huán)烷酸的粘度(60℃)從1480mpa·s降低到582mpa·s。通過紅外光譜分析、元素分析、LC-MS分析技術(shù)對氧化前后環(huán)烷酸的結(jié)構(gòu)進(jìn)行詳細(xì)的闡述。然后,分別以油酸、輕質(zhì)環(huán)烷酸、重質(zhì)環(huán)烷酸、氧化后環(huán)烷酸、混合酸為原料和二乙烯三胺反應(yīng),氯化芐為季銨化試劑合成了OM-1、OM-2、OM-3、OM-4、OM-5五種咪唑啉季銨鹽緩蝕劑。通過紅外光譜和核磁共振氫譜分析了咪唑啉季銨鹽緩蝕劑的結(jié)構(gòu)。采用靜態(tài)掛片失重法評價了緩蝕劑的緩蝕率,探索了腐蝕溫度、緩蝕劑加入量、腐蝕介質(zhì)的濃度等因素對A3鋼片腐蝕速率的影響。結(jié)果表明,OM-1緩蝕劑在5%鹽酸腐蝕介質(zhì)中,緩蝕率達(dá)到99.2%,符合標(biāo)準(zhǔn)DL/T523-1993中規(guī)定的酸洗緩蝕劑的評價指標(biāo);重質(zhì)環(huán)烷酸先經(jīng)過氧化再進(jìn)一步合成的咪唑啉緩蝕劑,其緩蝕效率優(yōu)于重質(zhì)環(huán)烷酸咪唑啉緩蝕劑,與輕質(zhì)環(huán)烷酸咪唑啉緩蝕劑效果相當(dāng),緩蝕率為93.3%。最后,通過改進(jìn)緩蝕劑的合成方法,可以省去減壓蒸餾過程,實現(xiàn)一鍋法制備咪唑啉緩蝕劑。結(jié)果表明,以氧化后重質(zhì)環(huán)烷酸為原料合成的緩蝕劑,產(chǎn)品在15%的鹽酸溶液中,60℃,4h的條件下,緩蝕劑加入量為0.3%時,對N80鋼片的緩蝕率為99.5%,符合標(biāo)準(zhǔn)SY/T5405-1996酸化用一級緩蝕劑的質(zhì)量標(biāo)準(zhǔn)。紅外光譜和核磁共振波譜分析表明該緩蝕劑是咪唑啉季銨鹽和另外一種有機(jī)化合物的混合物。其本身是一種良好的油田酸化緩蝕劑,兩者協(xié)同作用,抑制酸化壓裂過程對金屬的腐蝕。
[Abstract]:The corrosion of metal corrosion is caused by the acid cleaning of industrial acid washing and the acidification of oil wells. The imidazoline inhibitor is a kind of environmentally friendly, efficient and low toxic corrosion inhibitor. Naphthenic acid is a good raw material for the preparation of naphthenic Imidazoline Corrosion inhibitor. The Karamay refinery in China has a by-product of heavy naphthenic acid, which has a by-product of about 10 thousand tons per year. It has low acid value, low acid value, large viscosity, large molecular weight and limited application. This paper adopts two measures: catalytic oxidation and imidazoline type inhibitor to improve the industrial added value of heavy naphthenic acid. First, oxygen is used as oxidant to explore the influence of the catalyst species and dosage, oxidation temperature, pressure, time and other factors. Two times of oxygen supplement, adding additives to further improve the oxidation depth. When naphthenic acid is used as the catalyst, the value of naphthenic acid is increased from 95mgKOH/g to 136mgKOH/g by oxidation. The viscosity of naphthenic acid (60 degrees C) is reduced from 1480mpa. S to 582mpa. S. through infrared spectrum analysis, element analysis, and LC-MS analysis technique for naphthenic acid before and after oxidation. The structure of OM-1, OM-2, OM-3, OM-4, OM-5 and five kinds of imidazoline quaternary ammonium salts were synthesized with oleic acid, naphthenic acid, heavy naphthenic acid, naphthenic acid after oxidation, mixed acid as raw material and two ethylene three amine, and benzyl chloride as quaternating reagent. The structure of quaternary ammonium salt corrosion inhibitor. The corrosion inhibition rate of corrosion inhibitor was evaluated by static hanging weight loss method. The effect of corrosion temperature, corrosion inhibitor addition and corrosion medium concentration on the corrosion rate of A3 steel sheet was explored. The results showed that the corrosion inhibition rate of OM-1 corrosion inhibitor in 5% hydrochloric acid medium was 99.2%, which accorded with the standard of standard DL/T523-1993. The evaluation index of the acid washing inhibitor, the imidazoline inhibitor which is first oxidized and then synthesized by heavy naphthenic acid, is superior to heavy naphthenic acid imidazoline inhibitor, which is equivalent to the light naphthenic imidazoline inhibitor, and the corrosion inhibition rate is 93.3%. last. By improving the synthesis method of corrosion inhibitor, the decompression distillation can be saved. An imidazoline corrosion inhibitor was prepared by one pot method. The results showed that the corrosion inhibitor of heavy naphthenic acid after oxidation was prepared in 15% hydrochloric acid, 60 C and 4h, when the corrosion inhibitor was added to 0.3%, the corrosion inhibition rate of N80 steel was 99.5%, which was in line with the standard of standard SY/T5405-1996 acidification. Spectral and nuclear magnetic resonance spectroscopy analysis shows that the inhibitor is a mixture of imidazoline quaternary ammonium salt and another organic compound. It is a good acid corrosion inhibitor in oil field. Both of them synergistically and inhibit the corrosion of metal in the process of acidification and fracturing.
【學(xué)位授予單位】：中國石油大學(xué)(華東)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2015
【分類號】：TG174.42;TQ235

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