CN105797783A - 一种低温原油催化剂及其制备方法 - Google Patents
一种低温原油催化剂及其制备方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 50
- 239000010779 crude oil Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims abstract description 38
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims abstract description 36
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims abstract description 22
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 claims abstract description 22
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 235000010288 sodium nitrite Nutrition 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 14
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 14
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical group O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 42
- 239000000243 solution Substances 0.000 claims description 36
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 24
- 238000005470 impregnation Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- 229910021529 ammonia Inorganic materials 0.000 claims description 12
- 239000003921 oil Substances 0.000 claims description 11
- 238000006477 desulfuration reaction Methods 0.000 claims description 9
- 230000023556 desulfurization Effects 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 6
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 6
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 description 10
- 230000003009 desulfurizing effect Effects 0.000 description 7
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 6
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000005553 drilling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 239000003129 oil well Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate group Chemical group S(=O)(=O)([O-])[O-] QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0201—Oxygen-containing compounds
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Abstract
本发明公开了一种低温原油催化剂,其特征是:低温原油催化剂包括催化剂溶液A和催化剂溶液B组成;催化剂溶液A以水作为溶剂,溶质为甲醛、甲基二乙醇胺、亚硝酸钠和二乙醇胺;其中,溶质的质量份数为甲醛10‑15份,甲基二乙醇胺6‑22份,二乙醇胺32‑34份,亚硝酸钠5份‑7份;催化剂溶液B由二氧化锆、二氧化锰、三氧化二铁、硝酸锰和硝酸铁组成,二氧化锆、二氧化锰、三氧化二铁、硝酸锰和硝酸铁的重量比为10:80:15:3:2;催化剂溶液B的制备方法包括以下步骤:步骤一、称取硝酸锰、硝酸铁和二氧化锆;步骤二、将称取的硝酸锰、硝酸铁加入去离子水中制成浸渍液A,经浸渍液A加热至90℃备用。
Description
技术领域
本发明涉及催化剂领域,尤其涉及的是一种低温原油催化剂及其制备方法。
背景技术
目前,H2S作为一种剧毒气体,对人体危害严重。就石油行业而言,H2S气体的分布非常广泛,对作业工人存在潜在的生命伤害等安全隐患。腐蚀输油官网和下游炼化设备,并在一定程度上污染了周围环境,同时给油田员工和居民带来一定的安全隐患。
相关实验研究表明,油井和集输***中硫化氢大部分是硫酸盐还原菌代谢所得。目前关于油田脱硫剂主要有干法脱硫和湿法脱硫。
虽然这些脱硫剂短时间内能将硫化氢浓度降低至10mg/m3,达到相关标准,但存在着硫容较低的缺陷。
对于高含硫化氢的原油生产过程,存在脱硫效果不佳等技术问题。
发明内容
本发明的目的在于克服现有技术的不足,提供了一种低温原油催化剂及其制备方法,该一种低温原油催化剂及其制备方法可方便的进行脱硫,脱硫效果好。
本发明是通过以下技术方案实现的:
一种低温原油催化剂,其特征是:低温原油催化剂包括催化剂溶液A和催化剂溶液B组成;
催化剂溶液A以水作为溶剂,溶质为甲醛、甲基二乙醇胺、亚硝酸钠和二乙醇胺;其中,溶质的质量份数为甲醛10-15份,甲基二乙醇胺6-22份,二乙醇胺32-34份,亚硝酸钠5份-7份;
催化剂溶液B由二氧化锆、二氧化锰、三氧化二铁、硝酸锰和硝酸铁组成,二氧化锆、二氧化锰、三氧化二铁、硝酸锰和硝酸铁的重量比为10:80:15:3:2;
催化剂溶液B的制备方法包括以下步骤:
步骤一、称取硝酸锰、硝酸铁和二氧化锆;
步骤二、将称取的硝酸锰、硝酸铁加入去离子水中制成浸渍液A,经浸渍液A加热至90℃备用;
步骤三、将二氧化锆加入去离子水中搅拌加热至90℃,制成浸渍液B;
步骤四、将浸渍液A加入浸渍液B中,搅拌混合0.5h,在3-5个大气压的高压条件下搅拌;
步骤五、向步骤四制得的混合物中加入氨水后升温至100℃,恒温持续搅拌24h;得催化剂溶液B。
催化剂溶液A制备方法,包括以下工艺步骤:
1)按亚硝酸钠60g-90g、水1000ml的比例,在25℃-60℃,压力在3-5个大气压的高压条件下,将亚硝酸钠溶于水中配制亚硝酸钠溶液;
2)按二乙醇胺8ml-24ml、甲基二乙醇胺200ml的比例,将二乙醇胺滴至甲基二乙醇胺中,然后放置于2-6℃条件下冷却48-72小时;
3)按质量分数为20%-30%的30ml甲醛溶液比例,将甲醛溶液加入冷却后混合溶液中;
4)将配置的上述亚硝酸钠溶液、甲基二乙醇胺、甲醛溶液和二乙醇胺溶液放置于摇床中,摇动60-80min;
5)在3-5个大气压的压强条件下,混合液静置24小时后,得到水溶性原油脱硫剂。
二乙醇胺滴至甲基二乙醇胺时,二乙醇胺在10min-15min内匀速滴入甲基二乙醇胺中。
甲醛溶液加入冷却后混合溶液时,甲醛在5min-10min内匀速滴入混合溶液中。
氨水的添加量为硝酸铁和硝酸锰分别搭配使用的氨水量之和,氨水的质量浓度为25%。
在使用时将,催化剂溶液A和催化剂溶液B混匀后按照质量比1:2的比例加入到原油脱硫中,现用现配。
本发明与现有技术相比,本发明的脱硫剂具有优良的瞬间脱硫性能,对油田集输***硫化氢抑制,实现油田环境保护和节能减排具有重要的意义。
经测算,本脱硫剂添加量为20ml,6分钟内可将5000ppm降低至6ppm,达到国家《SY-T5087-2005含硫化氢油气井安全钻井推荐作法》的要求。
具体实施方式
实施例,一种低温原油催化剂,低温原油催化剂包括催化剂溶液A和催化剂溶液B组成;催化剂溶液A以水作为溶剂,溶质为甲醛、甲基二乙醇胺、亚硝酸钠和二乙醇胺;其中,溶质的质量份数为甲醛10-15份,甲基二乙醇胺6-22份,二乙醇胺32-34份,亚硝酸钠5份-7份;催化剂溶液B由二氧化锆、二氧化锰、三氧化二铁、硝酸锰和硝酸铁组成,二氧化锆、二氧化锰、三氧化二铁、硝酸锰和硝酸铁的重量比为10:80:15:3:2。
催化剂溶液B的制备方法包括以下步骤:
步骤一、称取硝酸锰、硝酸铁和二氧化锆;
步骤二、将称取的硝酸锰、硝酸铁加入去离子水中制成浸渍液A,经浸渍液A加热至90℃备用;
步骤三、将二氧化锆加入去离子水中搅拌加热至90℃,制成浸渍液B;
步骤四、将浸渍液A加入浸渍液B中,搅拌混合0.5h,在3-5个大气压的高压条件下搅拌;
步骤五、向步骤四制得的混合物中加入氨水后升温至100℃,恒温持续搅拌24h;得催化剂溶液B。
催化剂溶液A制备方法,包括以下工艺步骤:
1)按亚硝酸钠60g-90g、水1000ml的比例,在25℃-60℃,压力在3-5个大气压的高压条件下,将亚硝酸钠溶于水中配制亚硝酸钠溶液;
2)按二乙醇胺8ml-24ml、甲基二乙醇胺200ml的比例,将二乙醇胺滴至甲基二乙醇胺中,然后放置于2-6℃条件下冷却48-72小时;
3)按质量分数为20%-30%的30ml甲醛溶液比例,将甲醛溶液加入冷却后混合溶液中;
4)将配置的上述亚硝酸钠溶液、甲基二乙醇胺、甲醛溶液和二乙醇胺溶液放置于摇床中,摇动60-80min;
5)在3-5个大气压的压强条件下,混合液静置24小时后,得到水溶性原油脱硫剂。
二乙醇胺滴至甲基二乙醇胺时,二乙醇胺在10min-15min内匀速滴入甲基二乙醇胺中。
甲醛溶液加入冷却后混合溶液时,甲醛在5min-10min内匀速滴入混合溶液中。
氨水的添加量为硝酸铁和硝酸锰分别搭配使用的氨水量之和,氨水的质量浓度为25%。
本发明与现有技术相比,本发明的脱硫剂具有优良的瞬间脱硫性能,对油田集输***硫化氢抑制,实现油田环境保护和节能减排具有重要的意义。
经测算,本脱硫剂的硫容为400mg/L,添加量为20ml,6分钟内可将5000ppm降低至6ppm,达到国家《SY-T5087-2005含硫化氢油气井安全钻井推荐作法》的要求。
处理前 | 时间 | 处理后 | |
传统脱硫剂 | 5000ppm | 30分钟 | 8ppm |
本发明脱硫剂 | 5000ppm | 6分钟 | 6ppm |
Claims (6)
1.一种低温原油催化剂,其特征是:低温原油催化剂包括催化剂溶液A和催化剂溶液B组成;
催化剂溶液A以水作为溶剂,溶质为甲醛、甲基二乙醇胺、亚硝酸钠和二乙醇胺;其中,溶质的质量份数为甲醛10-15份,甲基二乙醇胺6-22份,二乙醇胺32-34份,亚硝酸钠5份-7份;
催化剂溶液B由二氧化锆、二氧化锰、三氧化二铁、硝酸锰和硝酸铁组成,二氧化锆、二氧化锰、三氧化二铁、硝酸锰和硝酸铁的重量比为10:80:15:3:2。
2.如权利要求1所述的一种低温原油催化剂的制备方法,其特征是:
催化剂溶液A制备方法,包括以下工艺步骤:
1)按亚硝酸钠60g-90g、水1000ml的比例,在25℃-60℃,压力在3-5个大气压的高压条件下,将亚硝酸钠溶于水中配制亚硝酸钠溶液;
2)按二乙醇胺8ml-24ml、甲基二乙醇胺200ml的比例,将二乙醇胺滴至甲基二乙醇胺中,然后放置于2-6℃条件下冷却48-72小时;
3)按质量分数为20%-30%的30ml甲醛溶液比例,将甲醛溶液加入冷却后混合溶液中;
4)将配置的上述亚硝酸钠溶液、甲基二乙醇胺、甲醛溶液和二乙醇胺溶液放置于摇床中,摇动60-80min;
5)在3-5个大气压的压强条件下,混合液静置24小时后,得到催化剂溶液A;
催化剂溶液B的制备方法包括以下步骤:
步骤一、称取硝酸锰、硝酸铁和二氧化锆;
步骤二、将称取的硝酸锰、硝酸铁加入去离子水中制成浸渍液A,经浸渍液A加热至90℃备用;
步骤三、将二氧化锆加入去离子水中搅拌加热至90℃,制成浸渍液B;
步骤四、将浸渍液A加入浸渍液B中,搅拌混合0.5h,在3-5个大气压的高压条件下搅拌;
步骤五、向步骤四制得的混合物中加入氨水后升温至100℃,恒温持续搅拌24h;得催化剂溶液B。
3.如权利要求2所述的一种低温原油催化剂的制备方法,其特征是:
二乙醇胺滴至甲基二乙醇胺时,二乙醇胺在10min-15min内匀速滴入甲基二乙醇胺中。
4.如权利要求2所述的一种低温原油催化剂,其特征是:
甲醛溶液加入冷却后混合溶液时,甲醛在5min-10min内匀速滴入混合溶液中。
5.如权利要求2所述的一种低温原油催化剂,其特征是:氨水的添加量为硝酸铁和硝酸锰分别搭配使用的氨水量之和,氨水的质量浓度为25%。
6.如权利要求2所述的一种低温原油催化剂,其特征是:在使用时将,催化剂溶液A和催化剂溶液B混匀后按照质量比1:2的比例加入到原油脱硫中,现用现配。
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