CN1084099A - 以催化裂化回炼油溶剂抽出物重质芳烃为原料的短侧链稠环芳烃混合磺酸盐型表面活性剂 - Google Patents
以催化裂化回炼油溶剂抽出物重质芳烃为原料的短侧链稠环芳烃混合磺酸盐型表面活性剂 Download PDFInfo
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Abstract
本发明公开了一种带有碳原子数为1~3的短
侧链、芳环数为3~5的稠环芳烃混合磺酸盐型表面
活性剂,它是以催化裂化回炼油经溶剂抽提得到的重
质芳烃为原料,经过磺化、中和制得。该产品亲水亲
油平衡值为8~16,具有良好的乳化性、分散性和驱
油能力,尤其适用于油-水体系乳化油的乳化剂、三
次采油的化学剂以及水煤浆燃料的分散剂等。
Description
本发明涉及一种以催化裂化回炼油的溶剂抽出物重质芳烃为原料制备的短侧链稠环芳烃混合磺酸盐型表面活性剂。
当代燃料工业、石油开采工业对表面活性剂提出了更高的要求,除了要有良好的使用性能外,还需要能提供大量质优价廉、配伍性能好的表面活性剂。
在现有技术中,石油磺酸盐基本上是由烷基芳基磺酸盐组成的,例如美国专利US 4144266描述了一种直接磺化原油来生产石油磺酸盐的方法,美国专利US 4847018描述了一种分段磺化原油获得高当量磺酸盐的方法,美国专利US 3970690和美国专利US 4541965描述了分别从高温和低温下进行石油馏份蒸汽裂解的残留物获得分散剂的方法。英国专利UK 2159536中描述了一种从焦油、特别是矿物煤的磺化产品中获得的分散剂。中国专利CN 1053443描述了一种从石油沥青制备磺化分散剂的方法。
在现有技术中,催化裂化回炼油中的重质芳烃尚无较好的利用途径,多数作沥青、燃料油等使用。一些用常减压减二、减三线油品磺化后生成少量长烷基侧链稠环芳烃混合磺酸盐视为酸渣废弃,随污水排放。催化裂化回炼油经过溶剂抽提后的重质芳烃含有90%(wt)以上带有1~3个碳原子短侧链、3~5个芳环的稠环芳烃。在现有技术中一般认为短侧链稠环芳烃磺酸盐作表面活性剂性能差,无利用价值,至今未见以重质芳烃为原料制备短侧链稠环芳烃磺酸盐型表面活性剂的报道。
本发明的目的,是公开一种以催化裂化回炼油溶剂抽提得到的重质芳烃为原料用浓硫酸或气相三氧化硫磺化制备的短侧链稠环芳烃混合磺酸盐型表面活性剂,解决了“催化裂化-芳烃抽提组合工艺”溶剂抽出物混合重质芳烃利用问题,并为燃料工业、石油开采工业等工业部门提供了性能优良的表面活性剂。
催化裂化回炼油经溶剂抽提得到的重质芳烃外观为一粘稠性液体,平均分子量为200~350,沸程为280~480℃、密度(20℃)为1.0020~1.1200,粘度为8~65mm2/s(50℃),胶质、沥青质为3.5~7.0%(wt),其中含有混合芳烃80~90%(wt)以上,饱和烃5~10%(wt),胶质和沥青质5~10%(wt),以及少量有机硫、有机氮化合物。混合芳烃中,三环至五环稠环芳烃占80~90%(wt),其余为少量的五环以上的稠环芳烃及芳杂环芳烃,稠环芳烃的芳环上带有1~3个碳原子的短侧链。
本发明将全馏份或部分馏份的未经处理的重质芳烃原料,与磺化剂98%(wt)以上的浓硫酸或者浓度为2~5%(wt)的气相三氧化硫接触反应,反应温度控制在50~150℃,重质芳烃与磺化剂的比例为1∶0.3~1∶3之间,反应时间1~3小时,获得一种褐色胶团状物质,然后用碱金属、或碱土金属、或胺的氢氧化物的水溶液中和,中和后PH值为7~9,所得产物经“亚甲基蓝法”定性鉴定为磺酸盐产品。经溶剂萃取和化学分析,其化学组成包含单磺酸盐20~40%(wt),多磺酸盐60~80%(wt),硫酸钠2~5%(wt)。
本发明克服了短侧链稠环芳烃磺酸盐作表面活性剂性能差,无利用价值的技术偏见。
本发明利用重质芳烃为原料制得的短侧链稠环芳烃混合磺酸盐表面活性剂无需分离即可使用,且具有意料不到的显著效果。
例如用全馏份重质芳烃为原料制得的短侧链稠环芳烃混合磺酸盐型表面活性剂作乳化剂,与柴油、渣油等油品和水经机械搅拌混合,得到一种多重乳状液型乳化油,乳化油最小水珠直径为1~2u,占水珠总量60%(wt)以上,最大水珠直径仅为6~8u。乳化油用离心机在4000转/分钟转速下进行离心分离1小时后,无任何分离现象,加热至70℃,并于70℃下长期静置,100小时内乳化油不会破乳,常温下乳化油稳定期为三年。
在实验室评价了本发明以全馏份重质芳烃为原料制备的短侧链稠环芳烃混合磺酸盐型表面活性剂作为三次采油化学剂的应用效果。评价的系统由新疆油田原油和岩芯等组成,其中矿化度高达7000ppm。用旋转液滴仪测得本发明产品作化学剂的原油-水界面张力为3×10-2~6×10-2毫牛顿/米,而用高纯度的长侧链烷基单苯环的石油磺酸盐表面活性剂作化学剂,测得的界面张力为3.53×10-2毫牛顿/米,在相同浓度和相同实验环境下,两种表面活性剂降低界面张力的能力相当。但是实验室驱油实验表明,在相同使用浓度下,本发明的短侧链稠环芳烃混合磺酸盐型表面活性剂剥离残留油的能力比长侧链烷基单苯环石油磺酸盐表面活性剂更强。
用本发明产品作水煤桨等流化剂和稳定剂也显示出较好的效果。将中间馏份的重质芳烃在高烃酸比下制备的磺酸盐表面活性剂,按常规方法制备浓度为62%~70%(wt)的水煤桨的粘度和稳定性均优于高效分散剂萘磺酸甲醛缩合物(NNO)制备的水煤桨,且析水率大大降低,无任何板结状沉淀。实验室评价数据见表1。
附图1为重质芳烃色质联用图谱。
亚甲基蓝法:在5ml 1%(wt)试样的水溶液中,加入亚甲基蓝溶液(将12g硫酸慢慢注入50ml水中并加亚甲基蓝0.03g和无水硫酸钠50g,溶解和加入水稀释至1升为止)10ml和氯仿5ml,将混合物摇荡2~3秒后,静止分层。氯仿层显蓝色证明有阴离子表面活性剂。
以下用具体实施例进一步说明本发明,但应当认为本发明决不限于这些实施例:
实施例1
将200g芳烃含量为90%(wt)的全馏份重质芳烃加入500ml四口烧瓶中,该烧瓶装有搅拌装置、回流冷凝管和温度计,用电热碗加热和控制反应温度,将130g 98%(wt)以上的浓硫酸加到反应瓶中。反应分别在100℃和120℃维持30分钟,得到一种褐色胶团状物质,然后用20%(wt)氢氧化钠水溶液中和,获得一粘稠状水溶性磺酸盐,用“亚甲基蓝法”定性鉴定为阴离子磺酸盐型表面活性剂,经溶剂萃取、化学分析,其中含磺酸盐50%(wt),水46%(wt),硫酸钠3%(wt)。
用上述产品0.8g加到20g水中搅拌混合,然后将水溶液加到80g的柴油、渣油混合物中,用玻璃棒、胶体磨搅拌得到一种均匀的多重乳状液型乳化油。取10g乳化油至离心分离机的试管中,离心机转速为4000转/分,旋转分离30分钟后无任何分离现象。将装有80g乳化油一广口瓶放入70℃的恒温水浴中,100小时内无任何分离现象。
实施例2
将200g馏程为350~450℃、芳烃含量为90%(wt)以上的重质芳烃加到三口烧瓶中,该反应器装有搅拌装置、温度计和回流冷凝管。将200g 98%(wt)的浓硫酸分三次加入到反应瓶中。反应温度从20℃起不断提高,保持反应物为流体状态,反应终止温度为140℃,总反应时间为1.5小时。反应结束后除掉未反应液体饱和烃,然后用15%(wt)的氢氧化钠水溶液中和磺酸,得到一高粘度水溶性磺酸盐,将此水溶性产物在真空干燥,得到450g固体产物。
将上述固体产品0.5g溶于30g的水中,然后加入68g煤粉,用搅拌装置强力搅拌,得到类似于重油的水煤桨,用粘度计测得该水煤桨的粘度为2000厘泊,为牛顿型流体,放置七天后,水煤桨表面无明显析水现象发生,底部仅有少量疏松状沉淀。
实施例3
将200g全馏份重质芳烃加到装有回流冷凝管、搅拌器和温度计的500ml四口烧瓶中,将550g 120%(wt)的发烟硫酸装入500ml反应瓶中,用氮气作携带剂,仔细调节流量使气相三氧化硫浓度为3%(V),将反应瓶用耐酸胶管与装有重质芳烃的反应瓶相联接,控制反应温度为50℃,待发烟硫酸重量降为450g时,停止反应。用15%(wt)的氢氧化钠水溶液中和反应物,得一褐色液体。
模拟新疆油田地质条件评价了上述产品,温度为45℃,矿化水按新疆油田地层水平组成配制。其矿化度为7000ppm,用3‰(wt)浓度的上述产品配制的原油-水体系,用旋转液滴仪测得界面张力为5.3×10-2毫牛顿/米。
表1
性能 | 1#产品 | NNO | 3#产品 | NNO |
指标 | 62%(wt) | 62%(wt) | 70%(wt) | 70%(wt) |
粘度 厘泊 | 300 | 500 | 2000 | 3600 |
析水率% | 4 | 6 | 3 | 4 |
稳定性 | 7天后有少 | 7天后有板 | 较好 | 一般 |
量软沉淀 | 结状沉淀 |
Claims (3)
1、一种短侧链稠环芳烃混合磺酸盐型表面活性剂,其特征在于是带有碳原子数为1~3的短侧链、芳环数为3~5的稠环芳烃的单磺酸盐和多磺酸盐的混合物,其亲水亲油平衡值为8~16,
2、根据权利要求1所述的表面活性剂,其特征在于以催化裂化回炼油的溶剂抽出物重质芳烃为原料,用98%(wt)以上浓硫酸或者气相三氧化硫为磺化剂,经过磺化、中和制得,重质芳烃与磺化剂的重量比为1∶0.3~1∶3,反应温度为50~150℃,反应时间为1~3小时,中和剂为碱金属、或碱土金属、或胺的氢氧化物,中和后的PH值为7~9,
3、根据权利要求2所述的重质芳烃,是带有碳原子数为1~3的短侧链、芳环数为3~5的含量为80~90%(wt)以上的稠环芳烃混合物,其平均分子量为200~350,沸程为280~480℃,密度(20℃)为1.0020~1.1200,粘度(50℃)为8~65mm2/s,胶质、沥青质为3.5~7.0%(wt)。
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101543744B (zh) * | 2009-04-03 | 2011-08-31 | 北京弘扬紫东环保科技有限公司 | 一种多组分复合水煤浆分散剂及其应用 |
CN102604670A (zh) * | 2012-02-10 | 2012-07-25 | 胜利油田中胜环保有限公司 | 油田驱油用石油磺酸盐原料的制备方法 |
CN102643216A (zh) * | 2012-04-01 | 2012-08-22 | 中国石油化工股份有限公司 | 一种抽出油烷基化产物磺化法制备表面活性剂方法 |
CN102839026A (zh) * | 2012-09-17 | 2012-12-26 | 宋晓轩 | 用高含杂环芳香烃组份生产水煤浆添加剂的方法 |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
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IT1227903B (it) * | 1988-12-23 | 1991-05-14 | Eniricerche S P A Snamprogetti | Procedimento per la preparazione di disperdenti solfonati |
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1993
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101543744B (zh) * | 2009-04-03 | 2011-08-31 | 北京弘扬紫东环保科技有限公司 | 一种多组分复合水煤浆分散剂及其应用 |
CN102604670A (zh) * | 2012-02-10 | 2012-07-25 | 胜利油田中胜环保有限公司 | 油田驱油用石油磺酸盐原料的制备方法 |
CN102643216A (zh) * | 2012-04-01 | 2012-08-22 | 中国石油化工股份有限公司 | 一种抽出油烷基化产物磺化法制备表面活性剂方法 |
CN102839026A (zh) * | 2012-09-17 | 2012-12-26 | 宋晓轩 | 用高含杂环芳香烃组份生产水煤浆添加剂的方法 |
CN102839026B (zh) * | 2012-09-17 | 2014-07-09 | 宋晓轩 | 用高含杂环芳香烃组份生产水煤浆添加剂的方法 |
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CN1038657C (zh) | 1998-06-10 |
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