CN101972638A - Deep denitrification method for fuel oil - Google Patents
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- CN101972638A CN101972638A CN 201010541223 CN201010541223A CN101972638A CN 101972638 A CN101972638 A CN 101972638A CN 201010541223 CN201010541223 CN 201010541223 CN 201010541223 A CN201010541223 A CN 201010541223A CN 101972638 A CN101972638 A CN 101972638A
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- 239000000295 fuel oil Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 29
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000003463 adsorbent Substances 0.000 claims abstract description 49
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 20
- 239000002253 acid Substances 0.000 claims abstract description 9
- 238000001179 sorption measurement Methods 0.000 claims abstract description 9
- 239000007789 gas Substances 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract 2
- 238000003756 stirring Methods 0.000 claims description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- DHRLEVQXOMLTIM-UHFFFAOYSA-N phosphoric acid;trioxomolybdenum Chemical compound O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.OP(O)(O)=O DHRLEVQXOMLTIM-UHFFFAOYSA-N 0.000 claims description 5
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 claims description 5
- 239000011964 heteropoly acid Substances 0.000 claims description 4
- 230000008929 regeneration Effects 0.000 claims description 4
- 238000011069 regeneration method Methods 0.000 claims description 4
- 238000009423 ventilation Methods 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 239000002594 sorbent Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 2
- CGFYHILWFSGVJS-UHFFFAOYSA-N silicic acid;trioxotungsten Chemical compound O[Si](O)(O)O.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 CGFYHILWFSGVJS-UHFFFAOYSA-N 0.000 claims description 2
- 239000007848 Bronsted acid Substances 0.000 claims 2
- 230000001476 alcoholic effect Effects 0.000 claims 2
- 239000011260 aqueous acid Substances 0.000 claims 2
- 238000002156 mixing Methods 0.000 claims 1
- 230000007420 reactivation Effects 0.000 claims 1
- 238000011084 recovery Methods 0.000 claims 1
- 150000004767 nitrides Chemical class 0.000 abstract description 7
- 238000001035 drying Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000012159 carrier gas Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000007654 immersion Methods 0.000 abstract 1
- 239000000446 fuel Substances 0.000 description 11
- 238000005984 hydrogenation reaction Methods 0.000 description 10
- 229910017464 nitrogen compound Inorganic materials 0.000 description 9
- 150000002830 nitrogen compounds Chemical class 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000002283 diesel fuel Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- UJOBWOGCFQCDNV-UHFFFAOYSA-N 9H-carbazole Chemical compound C1=CC=C2C3=CC=CC=C3NC2=C1 UJOBWOGCFQCDNV-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- SIKJAQJRHWYJAI-UHFFFAOYSA-N Indole Chemical compound C1=CC=C2NC=CC2=C1 SIKJAQJRHWYJAI-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- JBGWMRAMUROVND-UHFFFAOYSA-N 1-sulfanylidenethiophene Chemical class S=S1C=CC=C1 JBGWMRAMUROVND-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000008098 formaldehyde solution Substances 0.000 description 1
- PZOUSPYUWWUPPK-UHFFFAOYSA-N indole Natural products CC1=CC=CC2=C1C=CN2 PZOUSPYUWWUPPK-UHFFFAOYSA-N 0.000 description 1
- RKJUIXBNRJVNHR-UHFFFAOYSA-N indolenine Natural products C1=CC=C2CC=NC2=C1 RKJUIXBNRJVNHR-UHFFFAOYSA-N 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
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- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
Description
技术领域：Technical field:
本发明涉及燃油脱氮领域，具体地说涉及燃油的非加氢脱氮方法。The invention relates to the field of denitrification of fuel oil, in particular to a method for non-hydrogenation denitrogenation of fuel oil.
技术背景：technical background:
根据2010年2月6日第一次全国污染源普查公报的数据，2007年度全国机动车尾气排放的氮氧化物总量为549.65万吨，机动车尾气排放占总排放量的30%，机动车尾气排放已成为城市大气污染的主要来源之一。燃油中的氮化物主要包括碱性氮化物和非碱性氮化物。碱性氮化物主要包括吡啶、喹啉及其衍生物；非碱性氮化合物主要包括吡咯、吲哚、咔唑及其衍生物。随着石油馏分沸点的增加，氮化物含量迅速增加。燃油中的氮化物不但易使加氢催化剂中毒，而且氮化物的加氢反应活性低，加氢过程需要消耗大量的氢气。燃油中氮化物的存在还和燃油中的噻吩类硫化物产生竞争性吸附，抑制加氢脱硫的深度，对燃油的加氢脱硫深度有很大影响。此外氮化物的存在还影响燃油的安定性，并影响到加氢后燃油的收率。氮化物分子量越大，结构越复杂，加氢脱氮的反应速度越慢。氮化物在加氢过程中，可能生成比原氮化物分子量更大，结构与原氮化物很不相同的氮化物，而这类大分子的氮化物更不容易进行加氢脱氮反应。在加氢脱氮过程中随着脱氮率的提高，加氢脱氮的速度常数随燃油含氮量的减少而减小。因此，采用加氢的方法得到深度脱氮燃油非常困难。 According to the data in the Bulletin of the First National Survey of Pollution Sources on February 6, 2010, the total amount of nitrogen oxides emitted by motor vehicle exhaust in the country in 2007 was 5.4965 million tons, and motor vehicle exhaust emissions accounted for 30% of the total emissions. Emissions have become one of the main sources of urban air pollution. The nitrogen compounds in fuel mainly include basic nitrogen compounds and non-basic nitrogen compounds. Basic nitrogen compounds mainly include pyridine, quinoline and their derivatives; non-basic nitrogen compounds mainly include pyrrole, indole, carbazole and their derivatives. As the boiling point of petroleum fractions increases, the nitrogen content increases rapidly. The nitrogen compounds in the fuel not only easily poison the hydrogenation catalyst, but also have low hydrogenation reaction activity of the nitrogen compounds, and the hydrogenation process needs to consume a large amount of hydrogen. The existence of nitrogen compounds in fuel also produces competitive adsorption with thiophene sulfides in fuel, which inhibits the depth of hydrodesulfurization and has a great impact on the depth of hydrodesulfurization of fuel. In addition, the existence of nitrogen compounds also affects the stability of fuel oil and affects the yield of fuel oil after hydrogenation. The larger the molecular weight of the nitride, the more complex the structure, and the slower the reaction rate of hydrodenitrogenation. During the hydrogenation process, nitrides may generate nitrides with larger molecular weight than the original nitrides and very different structures from the original nitrides, and such macromolecular nitrides are less likely to undergo hydrodenitrogenation reactions. In the process of hydrodenitrogenation, with the increase of denitrification rate, the rate constant of hydrodenitrogenation decreases with the decrease of fuel nitrogen content. Therefore, it is very difficult to obtain deeply denitrified fuel by hydrogenation. the
深度加氢脱氮需要高温高压，设备投资和运行费用高，氢耗大，脱氮率低。我国石油工业氢源相对匮乏，使加氢工艺的应用受到一定限制。吸附剂法脱氮在常温常压下操作，不消耗氢气，脱氮后的副产物也被吸附于吸附剂的孔内，对燃油的品质几乎没有影响。Deep hydrodenitrogenation requires high temperature and high pressure, high equipment investment and operating costs, high hydrogen consumption, and low denitrogenation rate. The relative scarcity of hydrogen sources in my country's petroleum industry limits the application of hydrogenation processes. The denitrification by adsorbent method is operated at normal temperature and pressure, does not consume hydrogen, and the by-products after denitrification are also adsorbed in the pores of the adsorbent, which has almost no effect on the quality of fuel.
发明内容：Invention content:
本发明的目的是提供一种燃油深度脱氮方法，特别是车用燃油的深度非加氢脱氮方法。本发明为制备清洁燃油提供了一种新颖、高效、快速的深度脱氮方法，对节能减排和环境保护具有重要意义。The object of the present invention is to provide a deep denitrification method for fuel oil, especially a deep non-hydrogenation denitrification method for vehicle fuel. The invention provides a novel, efficient and rapid deep denitrification method for preparing clean fuel oil, and has great significance for energy saving, emission reduction and environmental protection.
本发明所述的燃油深度脱氮方法如下： The deep denitrification method of fuel oil described in the present invention is as follows:
燃油深度脱氮方法，过程如下：Fuel oil deep denitrification method, the process is as follows:
（1） 配制质子酸的水溶液或者醇溶液，加入吸附剂，搅拌，干燥至恒重。(1) Prepare the aqueous solution or alcohol solution of protonic acid, add adsorbent, stir, and dry to constant weight.
（2） 氮气或者空气通过甲醛水溶液，然后气体通过装有上述干燥后的吸附剂的吸附柱，吸附剂负载甲醛后停止通气。(2) Nitrogen or air passes through the formaldehyde solution, and then the gas passes through the adsorption column equipped with the above-mentioned dried adsorbent, and the adsorbent is loaded with formaldehyde and then the ventilation is stopped.
（3） 将上述脱氮吸附剂加入燃油中，搅拌反应后，过滤除去吸附剂得到深度脱氮燃油，回收的吸附剂再生使用。(3) Add the above-mentioned denitrification adsorbent into the fuel oil, stir and react, filter and remove the adsorbent to obtain deep denitrification fuel oil, and regenerate the recovered adsorbent for use.
步骤（1）所述质子酸的水溶液或者醇溶液的质量浓度为0.05%～35%；搅拌时间为10～30分钟，干燥温度为80℃～110℃。In step (1), the mass concentration of the protic acid aqueous solution or alcohol solution is 0.05% to 35%, the stirring time is 10 to 30 minutes, and the drying temperature is 80°C to 110°C.
步骤（3）所述搅拌反应温度为20℃～90℃，时间为0.5～6小时。In step (3), the stirring reaction temperature is 20° C. to 90° C., and the time is 0.5 to 6 hours.
所述的质子酸为杂多酸、磷酸或硫酸。The protonic acid is heteropolyacid, phosphoric acid or sulfuric acid.
所述的杂多酸是磷钼酸、磷钨酸、硅钨酸或硅钼酸。The heteropoly acid is phosphomolybdic acid, phosphotungstic acid, silicotungstic acid or silicomolybdic acid.
所述的吸附剂为孔径为2-50nm的介孔吸附剂，加入的吸附剂和质子酸的质量比为1:0.05～1:0.9。The adsorbent is a mesoporous adsorbent with a pore diameter of 2-50 nm, and the mass ratio of the added adsorbent to protonic acid is 1:0.05˜1:0.9.
步骤（2）所述氮气或者空气通过37%～40%的甲醛水溶液，然后此气体通过装有上述干燥后的吸附剂的吸附柱来负载甲醛，吸附剂负载甲醛的量和吸附剂的重量之比为0.05:1～0.6:1。The nitrogen or air in step (2) passes through 37% to 40% formaldehyde aqueous solution, and then the gas passes through the adsorption column equipped with the above-mentioned dried adsorbent to load formaldehyde, the amount of formaldehyde loaded on the adsorbent and the weight of the adsorbent The ratio is 0.05:1 to 0.6:1.
所述的燃油脱氮过程，吸附剂和燃油的质量比为1：10～1：90。In the fuel denitrification process, the mass ratio of the adsorbent to the fuel is 1:10-1:90.
所述的吸附剂的再生，是与燃油过滤分离后的吸附剂在300℃～400℃空气中加热2～4小时，然后脱氮吸附剂负载甲醛的量达到负载量后完成脱氮剂的再生。吸附剂负载的质子酸，其特征是为其含有可解离的质子，包括杂多酸、磷酸、硫酸。The regeneration of the adsorbent is to heat the adsorbent separated from the fuel oil in the air at 300° C. to 400° C. for 2 to 4 hours, and then complete the regeneration of the denitrification agent after the amount of formaldehyde loaded on the denitrification adsorbent reaches the load capacity. . Sorbent-loaded protic acids, characterized by containing dissociable protons, include heteropolyacids, phosphoric acid, sulfuric acid.
本发明的优点：Advantages of the present invention:
本发明的非加氢吸附脱氮过程不消耗氢气，脱氮反应速度快，吸附剂材料可以反复使用，对燃油品质无影响，具有投资少，操作成本低的特点。为制备清洁燃油提供了一种新颖、高效、快速的深度脱氮方法，对节能减排和环境保护具有重要意义。The non-hydrogenation adsorption denitrification process of the present invention does not consume hydrogen, the denitrification reaction speed is fast, the adsorbent material can be used repeatedly, has no influence on fuel oil quality, and has the characteristics of less investment and low operation cost. It provides a novel, efficient and rapid deep denitrification method for the preparation of clean fuel oil, which is of great significance to energy saving, emission reduction and environmental protection.
具体实施方式：Detailed ways:
实施例1Example 1
首先配制质量浓度8%的磷钼酸的水溶液10g，加入1.5g SBA-15吸附剂，搅拌10～30分钟后，含有吸附剂和磷钼酸的溶液在105℃下干燥至恒重。氮气先通过37%～40%的甲醛水溶液，然后通过装有上述干燥后的吸附剂的吸附柱，吸附0.4g甲醛后停止通气。将负载有磷钼酸和甲醛的吸附剂加入30g 0#柴油，70℃下搅拌60分钟后，燃油氮含量从273ppm降低至4ppm，得到深度脱氮柴油。First prepare 10g of aqueous solution of phosphomolybdic acid with a mass concentration of 8%, add 1.5g of SBA-15 adsorbent, stir for 10 to 30 minutes, and dry the solution containing adsorbent and phosphomolybdic acid at 105°C to constant weight. Nitrogen first passes through 37% to 40% formaldehyde aqueous solution, then passes through the adsorption column equipped with the above-mentioned dried adsorbent, absorbs 0.4g of formaldehyde, and then stops ventilation. The adsorbent loaded with phosphomolybdic acid and formaldehyde was added to 30g 0# diesel oil, and after stirring at 70°C for 60 minutes, the nitrogen content of the fuel oil decreased from 273ppm to 4ppm, and deep denitrification diesel oil was obtained.
实施例2Example 2
首先配制质量浓度3.5%的磷钨酸的水溶液20g，加入1g B型硅胶吸附剂，搅拌10～30分钟后，含有吸附剂和磷钨酸的溶液在105℃下干燥至恒重。氮气通过37%～40%的甲醛水溶液，然后气体通过装有上述干燥后的吸附剂的吸附柱，吸附0.3g甲醛后停止通气。将负载有磷钨酸和甲醛的吸附剂加入30g 0#柴油，80℃下搅拌30分钟后，燃油氮含量从273ppm降低至7.6ppm，得到深度脱氮柴油。First prepare 20g of phosphotungstic acid aqueous solution with a mass concentration of 3.5%, add 1g of B-type silica gel adsorbent, stir for 10-30 minutes, and dry the solution containing adsorbent and phosphotungstic acid at 105°C to constant weight. Nitrogen gas passes through 37% to 40% formaldehyde aqueous solution, and then the gas passes through the adsorption column equipped with the above-mentioned dried adsorbent, and stops ventilation after absorbing 0.3g of formaldehyde. The adsorbent loaded with phosphotungstic acid and formaldehyde was added to 30g 0# diesel oil, and after stirring at 80°C for 30 minutes, the nitrogen content of the fuel oil decreased from 273ppm to 7.6ppm, and deep denitrification diesel oil was obtained.
Claims (9)
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| CN102559252A (en) * | 2012-03-07 | 2012-07-11 | 抚顺石化北天集团众兴公司鸿远达精细化工厂 | Non-hydrodenitrogeneration method for catalytically cracked gasoline |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102559252A (en) * | 2012-03-07 | 2012-07-11 | 抚顺石化北天集团众兴公司鸿远达精细化工厂 | Non-hydrodenitrogeneration method for catalytically cracked gasoline |
| CN102559252B (en) * | 2012-03-07 | 2013-10-09 | 抚顺石化北天集团众兴公司鸿远达精细化工厂 | Non-hydrodenitrogeneration method for catalytically cracked gasoline |
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