CN112812816A - 一种油浆粘度改性剂及其制备方法 - Google Patents
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Abstract
本发明涉及一种油浆粘度改性剂，该油浆粘度改性剂同时含有氨基、羧基和酰胺键的强极性化合物。本发明还提供了上述油浆粘度改性剂的制备方法，包括步骤：1)将多元胺溶于二甲苯中，分批加入二元酸，在80℃～120℃下回流搅拌2～4h，形成羧酸铵盐；2)在140℃～180℃下进行减压蒸馏4～8h，羧酸铵盐脱水形成酰胺键，最终得到黄色粘稠产物。本发明油浆粘度改性剂能降低油浆粘度，使油浆中的催化剂粉末更容易沉降，与油浆沉降剂结合使用，可使高粘度油浆的脱灰率达到95％以上，灰分含量降低到0.02％以下。
Description
技术领域
本发明涉及石油炼制加工技术领域，具体涉及一种降低催化裂化外甩油浆粘度的改性剂及其制备方法。
背景技术
随着我国船用燃料油出口退税政策的实施，国内炼厂积极响应生产需求，大力发展低硫船用燃料油。催化裂化外甩油浆作为其中一种重要的原料，成为炼厂新的经济增长点。然而，油浆中往往含有0.2～0.9％的催化剂粉末，严重限制了油浆的后续使用。为此，需采取措施降低油浆中固体颗粒含量。国内炼厂中通常采用化学助剂法，然而，不同炼厂的油浆因理化性能差异，沉降剂的效果也不尽相同。尤其是对于高粘度的油浆，胶质、沥青质含量高，沉降剂分子和固体颗粒在油浆中的运动受阻，使沉降剂难以与催化剂粉末结合，结合后难以依靠重力作用沉降，最终导致其固含量难以降低。为此，需采取必要措施，降低油浆粘度，以促进固体颗粒脱除。
通过提高温度和加轻质燃料油可以明显降低油浆的粘度，然而，提高温度往往伴随着上下游工艺的变化和能耗的增加；加轻质燃料油则会增加成本，降低油浆再利用的经济性，若回收则需增加新设备，提高运行成本。因此，通过加入油浆粘度改性剂的方式，调节油浆粘度，是最为经济、便捷的处理方式。
调节油浆粘度的关键在于提高胶质、沥青质在油浆中的分散性能。
专利US5948237A介绍了一种肌氨酸盐类衍生物能够抑制沥青质沉降，促进其在重油中分散。
专利US7122112B2设计开发了一种带有羧基和酰胺键的烃类化合物，不仅能够分散沥青质，还能提高原油的抗乳化性、降低体系粘度、减少沉积物形成、减少表面粘附和腐蚀。
专利CN1297981A中介绍了采用四乙烯五胺和脂肪二聚酸做絮凝剂，在80-100℃下沉降16-48h，辅助离心分离的方法，可将油浆灰分降至50ppm以下。
专利CN201810327207.8中通过加入丙烯酸高碳酸酯作为降粘剂来提高脱灰效果。
上述专利说明关于重油或原油沥青质分散和降低粘度的研究较多，并且证明带有氨基和羧基的化合物通过与沥青质的氢键作用能起到积极的作用。在油浆沉降剂的开发过程中，也有引入氨基、羧基或其他降粘剂来增强脱灰效果的报道。然而，对于催化裂化外甩油浆粘度改性剂的研发仍处于初级阶段，普遍存在加剂量大、对于高粘度油浆效果不明显的问题，进而导致油浆灰分难以脱除。
发明内容
本发明的目的在于弥补现有油浆沉降剂的不足，设计合成一种油浆粘度改性剂，将多元胺与二元酸通过酰胺键连接，形成同时含有氨基、羧基和酰胺键的强极性化合物，以提高对胶质、沥青质的分散性来降低油浆粘度，从而提高油浆沉降剂对催化裂化油浆中催化剂粉末的脱除效果。
本发明提供的一种油浆粘度改性剂，其中所述的油浆粘度改性剂具有如下结构式：
式中，R1为烷基链或含有仲氨结构的烷基链，R2为C2～C10的烷基链。
本发明还提供了上述油浆粘度改性剂的一种制备方法，包括如下步骤：
1)将多元胺溶于二甲苯中，分批加入二元酸，在80℃～120℃下回流搅拌2～4h，形成羧酸铵盐；
2)在140℃～180℃下进行减压蒸馏4～8h，羧酸铵盐脱水形成酰胺键，脱除的水分与溶剂二甲苯一起通过减压蒸馏脱离反应体系，最终得到黄色粘稠产物。
在上述制备方法中，所述的多元胺优选为C2～C12的脂肪族二胺或多烯多胺，更优选为多元胺为乙二胺、己二胺、二乙烯三胺或三乙烯四胺。
在上述制备方法中，所述的二元酸为C2～C10的脂肪族二元酸。
在上述制备方法中，所述步骤1)中，多元胺与二元酸的摩尔比优选为1:1。
本发明的油浆粘度改性剂优点在于：(1)将氨基、羧基和酰胺键结合在一个分子上，能与沥青质形成强烈的氢键作用，从而起到分散沥青质、降低油浆粘度的作用；(2)合成所用的原料为常见的化工原料，反应过程较为简单，因此生产成本不高；(3)仅包含碳、氢、氧、氮四种元素，不包含硫、金属等对油品有影响的元素。
具体实施方式
下面结合具体的实施例来说明本发明内容。需要说明的是，下文所提实施例所述内容为说明性内容，并不以任何形式限制本发明，不能据此来限定本发明的保护范围。
实施例1：油浆粘度改性剂A的制备
将12.0g(0.2mol)乙二胺分散于50mL二甲苯中，分五批加入40.5g(0.2mol)癸二酸，在100℃下反应3h后，将温度升至160℃，减压蒸馏6h，得到黄色粘稠的膏状物。
实施例2：油浆粘度改性剂B的制备
将23.2g(0.2mol)己二胺分散于80mL二甲苯中，分四批加入29.2g(0.2mol)己二酸，在120℃下反应2h后，将温度升至180℃，减压蒸馏4h，得到黄色粘稠产物。
实施例3：油浆粘度改性剂C的制备
将37.9g(0.2mol)四乙烯五胺分散于60mL二甲苯中，分三批加入23.6g(0.2mol)丁二酸，在80℃下反应4h后，将温度升至140℃，减压蒸馏8h，得到黄色粘稠的膏状物。
实施例4：实施例1～3中制备的三种油浆粘度改性剂性能评价。
(1)实验原料
本实施例中使用的油浆为某炼厂所提供的重油催化裂化外甩油浆，50℃运动粘度为367.32mm2/S，胶质、沥青质含量为12.13％，灰分含量为0.3304％。
本实施例中使用油浆沉降剂为中海油天津化工研究设计院有限公司自主研发的产品。
(2)实验方法
在加热条件下，将本发明所述的油浆粘度改性剂分散于高闪点溶剂油和异辛醇的混合溶剂中，配制成质量分数为30％的油浆粘度改性剂溶液，降至室温备用。
取1kg油浆预热至100℃，加入100mg上述油浆粘度改性剂溶液和400mg油浆沉降剂，混合均匀后，在100℃下静置沉降24h，然后取上层澄清油浆，按照国标《GB/T 508-85石油产品灰分测定法》规定的方法测灰分含量。将只加油浆粘度改性剂、只加油浆沉降剂和不加任何助剂的油浆采用相同方法处理，作为对照试验。
(3)实验结果
油浆粘度改性剂对油浆脱灰效果影响的评价结果如表1所示。
表1油浆粘度改性剂对油浆脱灰效果的影响
从表1中数据可以看出，该油浆由于粘度大，高温下沉降处理几乎不沉降，即使加入油浆沉降剂，效果并不明显。而加入本发明所制备的油浆粘度改性剂后，超过15％的灰分可以自然沉降，而当油浆粘度改性剂与油浆沉降剂进行复配后，脱灰率可达到95％，处理后油浆灰分含量在0.02％以下，能满足大多数油浆的后续使用需求。
Claims (5)
1.一种油浆粘度改性剂，其特征在于，所述的油浆粘度改性剂为多元胺与二元酸的反应产物，化学结构式如下：
式中，R1为烷基链或含有仲氨结构的烷基链，R2为C2～C10的烷基链。
2.一种权利要求1所述的油浆粘度改性剂的制备方法，其特征在于，包括如下步骤：
1)将多元胺溶于二甲苯中，分批加入二元酸，在80℃～120℃下回流搅拌2～4h，形成羧酸铵盐；多元胺与二元酸的摩尔比为1:1；
2)在140℃～180℃下进行减压蒸馏4～8h脱除的水分与溶剂二甲苯，羧酸铵盐脱水形成酰胺键，最终得到黄色粘稠产物。
3.根据权利要求2所述的制备方法，其特征在于，所述的多元胺是C2～C12的脂肪族二胺或多烯多胺。
4.根据权利要求3所述的制备方法，其特征在于，所述的多元胺为乙二胺、己二胺、二乙烯三胺或三乙烯四胺。
5.根据权利要求3所述的制备方法，其特征在于，所述的二元酸为C2～C10的脂肪族二元酸。
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| CN117363374B (zh) * | 2023-11-24 | 2025-10-28 | 中海油天津化工研究设计院有限公司 | 用于碱催化体系油浆的脱灰剂及其应用、油浆中固体颗粒的脱除方法 |
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