CN112745353A - 一种油溶性钼酸配合物的制备方法 - Google Patents
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F11/00—Compounds containing elements of Groups 6 or 16 of the Periodic Table
- C07F11/005—Compounds containing elements of Groups 6 or 16 of the Periodic Table compounds without a metal-carbon linkage
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2213—At least two complexing oxygen atoms present in an at least bidentate or bridging ligand
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2231/00—Catalytic reactions performed with catalysts classified in B01J31/00
- B01J2231/60—Reduction reactions, e.g. hydrogenation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/02—Compositional aspects of complexes used, e.g. polynuclearity
- B01J2531/0213—Complexes without C-metal linkages
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/60—Complexes comprising metals of Group VI (VIA or VIB) as the central metal
- B01J2531/64—Molybdenum
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
本发明涉及石油化工技术领域,具体涉及一种油溶性钼酸配合物的制备方法,将钼化合物与二醇以有机胺为催化剂进行反应,制得油溶性钼酸配合物。本发明将钼化合物与二醇在有机胺催化剂作用下反应,制备新型油溶性钼酸配合物,此类配合物可用加氢催化剂。
Description
技术领域
本发明涉及石油化工技术领域,具体涉及一种油溶性钼酸配合物的制备方法。
背景技术
目前,随着常规石油资源日益减少和重油开采技术日臻成熟,原油的生产呈现重质化、劣质化的趋势。炼化企业面临大量国产劣质重油和进口劣质重油的轻质化问题。同时要兼顾环保指标要求,控制汽、柴油质量,满足生产清洁燃料的需要。浆态床加氢裂化技术能够加工高金属、高残炭、高硫的劣质重油原料,且转化率高、轻质油收率高,符合提高资源利用率发展趋势的优良工艺。
国外诸家公司均开展了重油浆态床加氢裂化技术的研究,主要有意大利ENI公司的EST工艺、委内瑞拉Intevep与法国Axens合作开发的HDHPLUS-SHP工艺、Chevron公司的VRSH工艺、KBR和BP公司合作开发的VCC工艺、UOP公司的Uniflex工艺和Headwater公司的(HCAT/HC3)工艺等。重油浆态床加氢裂化工艺开发的关键在于优质加氢催化剂的持续性进步,其中油溶性催化剂能有效溶于重质原料中,具有优异的加氢效果且能有效抑制生焦,是理想的催化剂。
因此,油溶性催化剂逐渐成为研究的热点,如何获得制备方法简单、活性高的油溶性催化剂是本领域亟需解决的技术问题。
发明内容
为了克服现有技术中存在的缺点和不足,本发明的目的在于提供一种油溶性钼酸配合物的制备方法。
本发明的目的通过下述技术方案实现:一种油溶性钼酸配合物的制备方法,将钼化合物与二醇以有机胺为催化剂进行反应,制得油溶性钼酸配合物。
本发明采用的钼化合物包括钼酸、钼酸铵、对钼酸铵、三氧化钼、钼酸酐和氯化钼中的至少一种。
本发明采用的二醇为含有2至18个碳原子的α-烷二醇和/或β-烷二醇。更为优选的,所述二醇包括乙二醇、1,2-丙二醇、1,3-丙二醇、1,2-戊二醇、2,3-丁二醇、1,2-己二醇、2-甲基-1,3-戊二醇、2-乙基-1,3-己二醇、1,2-辛二醇、1,3-辛二醇、1,2-十二二醇、2,4-二乙基辛烷-1,3-二醇和2,4,6-三乙基癸烷-1,3-二醇中的至少一种。在用二醇与钼化合物反应制备钼酸配合物时,通常需要大量过量的二醇,才能使钼化合物得到满意的利用。在大多数情况下,过量的二醇大约比化学计量量高出200%到250%。然后,必须通过萃取或高温低压蒸馏从产品中回收多余的二醇。很明显,回收或去除多余的二醇会大大增加工艺成本。因此,有必要提高二醇与钼酸的反应效率。
有机胺是二醇与钼化合物反应的非常有效的催化剂,本发明采用的有机胺为含有至少6个碳原子的烷基胺、芳胺、酰胺、叠氮和恶嗪中的至少一种,在大气压下沸点不超过约300℃,当使用这些催化剂时,反应可以继续进行到完成,只需要少量过量的二醇。具体的,本发明采用的有机胺包括二异辛胺、二苄基胺、三乙胺、二甲基甲酰胺、二甲基乙酰胺、二乙基甲酰胺、苯胺、甲苯胺、苯二胺、二甲基苯胺、N-烷基化、N-芳基化衍生物、吡啶、吡嗪、哌啶、N-乙基哌啶、吗啉和N-乙基吗啉中的至少一种。
二醇与钼化合物的反应优选在苯、甲苯、二甲苯等芳香烃溶剂中,在约80-160℃的温度范围内进行。反应在回流下进行方便,反应的水从回流中分离出来。优选二醇与钼化合物的摩尔比在1-1.5:1范围内。基于反应中使用的钼化合物,有机胺催化剂的浓度将在1~50wt%质量分数的范围内,优选范围为约10~40wt%质量分数。通过减压蒸馏将有机胺催化剂与溶剂一起从反应产物中除去。
本发明制得的油溶性钼酸配合物的结构式如式Ⅰ、式Ⅱ或式Ⅲ所示:
其中,R1、R2和R3是氢原子或烷基。
本发明的有益效果在于:本发明将钼化合物与二醇在有机胺催化剂作用下反应,制备新型油溶性钼酸配合物,此类配合物可用加氢催化剂。
具体实施方式
为了便于本领域技术人员的理解,下面结合实施例对本发明作进一步的说明,实施方式提及的内容并非对本发明的限定。
实施例1
将60g钼酸铵、124g 2-乙基1,3-己二醇、250mL二甲苯和25mL二甲基甲酰胺装入合适的反应器。反应物在回流下通过搅拌加热,水从回流塔顶分离。反应持续到产水率降低,通常需要5到9小时。然后冷却反应混合物,在抽吸下过滤,并添加到足够的中性矿物溶剂油中。然后在约160℃和约0.25mm压力下通过减压蒸馏除去溶剂和有机胺催化剂,得到油溶性钼酸配合物的浓缩物,其钼含量在5~15wt%之间。
实施例2
将钼酸铵与2-乙基-1,3-己二醇在二甲苯中的反应在许多单独的制剂中进行,其中在某些情况下不使用催化剂,在其他情况下使用本发明的催化剂。按照实施例1中概述的一般方式在回流下加热进行反应。在每种情况下,反应一直持续到水的形成速度下降。然后对每种情况下的产品进行过滤,并测定过滤残留物的量。
反应物的比例、所用的各种催化剂以及所得结果如下表所示。
从上表可以看出,每种催化剂都缩短了反应时间,并获得了更有效的反应物利用率。
上述实施例为本发明较佳的实现方案,除此之外,本发明还可以其它方式实现,在不脱离本发明构思的前提下任何显而易见的替换均在本发明的保护范围之内。
Claims (10)
1.一种油溶性钼酸配合物的制备方法,其特征在于:将钼化合物与二醇以有机胺为催化剂进行反应,制得油溶性钼酸配合物。
2.根据权利要求1所述的一种油溶性钼酸配合物的制备方法,其特征在于:所述钼化合物包括钼酸、钼酸铵、对钼酸铵、三氧化钼、钼酸酐和氯化钼中的至少一种。
3.根据权利要求1所述的一种油溶性钼酸配合物的制备方法,其特征在于:所述二醇为含有2至18个碳原子的α-烷二醇和/或β-烷二醇。
4.根据权利要求1所述的一种油溶性钼酸配合物的制备方法,其特征在于:所述二醇包括乙二醇、1,2-丙二醇、1,3-丙二醇、1,2-戊二醇、2,3-丁二醇、1,2-己二醇、2-甲基-1,3-戊二醇、2-乙基-1,3-己二醇、1,2-辛二醇、1,3-辛二醇、1,2-十二二醇、2,4-二乙基辛烷-1,3-二醇和2,4,6-三乙基癸烷-1,3-二醇中的至少一种。
5.根据权利要求1所述的一种油溶性钼酸配合物的制备方法,其特征在于:所述有机胺为含有至少6个碳原子的烷基胺、芳胺、酰胺、叠氮和恶嗪中的至少一种。
6.根据权利要求1所述的一种油溶性钼酸配合物的制备方法,其特征在于:所述有机胺包括二异辛胺、二苄基胺、三乙胺、二甲基甲酰胺、二甲基乙酰胺、二乙基甲酰胺、苯胺、甲苯胺、苯二胺、二甲基苯胺、N-烷基化、N-芳基化衍生物、吡啶、吡嗪、哌啶、N-乙基哌啶、吗啉和N-乙基吗啉中的至少一种。
7.根据权利要求1所述的一种油溶性钼酸配合物的制备方法,其特征在于:所述溶剂为苯、甲苯和二甲苯。
8.根据权利要求1所述的一种油溶性钼酸配合物的制备方法,其特征在于:所述反应温度为80-160℃。
9.根据权利要求1所述的一种油溶性钼酸配合物的制备方法,其特征在于:所述二醇与钼化合物的摩尔比在1-1.5:1,有机胺的浓度为1-50wt%质量分数。
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US3285942A (en) * | 1962-03-06 | 1966-11-15 | Exxon Research Engineering Co | Preparation of glycol molybdate complexes |
US4009122A (en) * | 1975-06-23 | 1977-02-22 | Olin Corporation | Novel glycol soluble molybdenum catalysts and method of preparation |
US4593012A (en) * | 1984-03-09 | 1986-06-03 | Atlantic Richfield Company | Production of hydrocarbon-soluble salts of molybdenum for epoxidation of olefins |
US4650886A (en) * | 1984-12-31 | 1987-03-17 | Texaco Inc. | Synthesis of ammonium molybdate/alkanol complexes |
CN107090004A (zh) * | 2017-05-31 | 2017-08-25 | 张卫东 | 一种有机钼润滑油脂添加剂及其制备方法 |
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US3285942A (en) * | 1962-03-06 | 1966-11-15 | Exxon Research Engineering Co | Preparation of glycol molybdate complexes |
US4009122A (en) * | 1975-06-23 | 1977-02-22 | Olin Corporation | Novel glycol soluble molybdenum catalysts and method of preparation |
US4593012A (en) * | 1984-03-09 | 1986-06-03 | Atlantic Richfield Company | Production of hydrocarbon-soluble salts of molybdenum for epoxidation of olefins |
US4650886A (en) * | 1984-12-31 | 1987-03-17 | Texaco Inc. | Synthesis of ammonium molybdate/alkanol complexes |
CN107090004A (zh) * | 2017-05-31 | 2017-08-25 | 张卫东 | 一种有机钼润滑油脂添加剂及其制备方法 |
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