CN107469852A - 一种合成生物柴油碳基磁性固体碱催化剂及其制备方法 - Google Patents
一种合成生物柴油碳基磁性固体碱催化剂及其制备方法 Download PDFInfo
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- 239000007787 solid Substances 0.000 title claims abstract description 31
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 239000003225 biodiesel Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 14
- 238000001308 synthesis method Methods 0.000 title abstract description 4
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 11
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 4
- -1 alkali metal salt Chemical class 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229920000877 Melamine resin Polymers 0.000 claims description 5
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- 239000011698 potassium fluoride Substances 0.000 claims description 4
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 3
- 239000011775 sodium fluoride Substances 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000002955 isolation Methods 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 239000002585 base Substances 0.000 abstract description 20
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 abstract 2
- 239000003513 alkali Substances 0.000 abstract 1
- 229910052783 alkali metal Inorganic materials 0.000 abstract 1
- 230000036571 hydration Effects 0.000 abstract 1
- 238000006703 hydration reaction Methods 0.000 abstract 1
- 230000005415 magnetization Effects 0.000 abstract 1
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- 239000003549 soybean oil Substances 0.000 description 5
- 235000012424 soybean oil Nutrition 0.000 description 5
- 239000003921 oil Substances 0.000 description 3
- 235000019198 oils Nutrition 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 238000005815 base catalysis Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 230000001172 regenerating effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 235000019482 Palm oil Nutrition 0.000 description 1
- 235000019484 Rapeseed oil Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 235000012343 cottonseed oil Nutrition 0.000 description 1
- 239000002385 cottonseed oil Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000007974 melamines Chemical class 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 239000002540 palm oil Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J35/33—Electric or magnetic properties
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L1/00—Liquid carbonaceous fuels
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
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- C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
- C10L2290/12—Regeneration of a solvent, catalyst, adsorbent or any other component used to treat or prepare a fuel
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
本发明公开了一种合成生物柴油碳基磁性固体碱催化剂及其制备方法。催化剂的载体为磁性的C3N4,负载的活性组分是碱金属盐或者碱,制备方法为:通过FeCl3和水合肼反应,将C3N4赋予磁性,对磁性化之后的载体进一步进行负载活性组分,制得碳基磁性固体碱催化剂。本发明的优点在于,所制得的催化剂用于合成生物柴油的反应,催化活性好,可进行磁分离,稳定性好,降低生产成本,有良好的工业应用前景。
Description
技术领域
本发明涉及合成生物柴油碳基磁性固体碱催化剂的制备及应用,属于合成生物柴油技术领域。
背景技术
能源是社会经济发展和提高人民生活水平的重要基础。因此寻求更加安全、清洁、经济的能源,已经成为世界各国的共同追求。生物柴油的利用是从环境保护和资源战略的角度出发,发展替代燃料及可再生能源的重要途径。作为无污染的可再生能源,生物柴油性能可与传统的石化柴油媲美,尾气有害排放降低。因此,生物柴油的研究和应用是全球广泛关注的问题。
国内外生物柴油工业生产还是以传统均相酸碱催化为主,价格低廉,反应活性高,但存在产物分离困难、产生大量废水等弊端。对于传统酸碱所带来的问题,磁性催化剂因其催化活性高、环境友好、可重复利用、易实现与产物分离等优点得到人们广泛的关注。
为了解决上述问题,本发明提供一种碳基磁性固体碱催化剂及其制备方法,其催化制备生物柴油的工艺符合绿色化学的要求,有着良好的工业化前景。
发明内容
本发明的目的在于提供了一种合成生物柴油碳基磁性固体碱催化剂及其制备方法。以该方法所制得的催化剂具有活性高,可重复利用的特点。所述的碳基磁性固体碱催化剂的制备方法,其特征在于包括以下过程,
(1)将5~10g前驱体,放在带盖的坩埚里用马弗炉焙烧,5~8°/min升温到500~600℃保持2~8h,得到黄色的固体C3N4载体;
(2)将1~3g的载体C3N4超声分散在40~80mL的乙二醇溶液中,1~3g的FeCl3·6H2O加入到溶液中,搅拌10~30min,加入4~10mL的80%的一水合肼水溶液,继续搅拌20~50min,转移至150~200℃的烘箱中,水热8~14h,分别用去离子水和乙醇各洗涤3~6次,磁性分离,在60~80℃下,真空干燥20~36h,得到磁性载体C3N4;
(3)将5~50g的固体碱活性组分置于40~100mL的水中,搅拌溶解,分别加入1~3g的磁性载体C3N4,搅拌8~12h,过滤,干燥,得到碳基磁性固体碱催化剂。
上述合成C3N4的前驱体为三聚氰胺、二氰二胺、硫脲或尿素的任何一种。
上述合成固体碱活性组分为KF、KOH、K2CO3、NaF、NaOH或Na2CO3的任何一种。
上述制得的碳基磁性固体碱催化剂用于合成生物柴油的方法,其特征在于包括以下过程:
1)将油脂和短链醇以醇油摩尔比6~48:1加入高压反应釜,再加入碳基磁性固体碱催化剂,催化剂加入量为油脂质量的1.0~10.0%,在反应温度为50~70℃下,反应1~10h,即得到含有生物柴油的混合物;
2)对步骤1)混合物进行过滤,滤出的固体催化剂进行循环利用,所得滤液经减压蒸馏除去甲醇,再静置分层,分离出下层甘油,上层液体即为生物柴油。
上述合成生物柴油的工艺中,油脂是大豆油、菜籽油、棉籽油或棕榈油的任何一种,短链醇为甲醇、乙醇或丙醇的任何一种。
本发明的优点在于,催化剂活性高,可重复使用,是潜在的具竞争力的绿色路线。
下面通过具体实施例来对本发明加以进一步说明,但不限制本发明。
具体实施方式
【实施例1】
将5g三聚氰胺,放在带盖的坩埚里用马弗炉焙烧,5°/min升温到550℃保持6h,得到黄色的固体C3N4。将1g C3N4的超声分散在64mL的乙二醇溶液中,1g的FeCl3·6H2O加入到溶液中,搅拌10min,加入6mL的80%的一水合肼水溶液,继续搅拌30min,转移至200℃的烘箱中,水热10h,分别用去离子水和乙醇各洗涤4次,磁性分离,在60℃下,真空干燥24h,得到磁性的C3N4。将20g固体碱活性组分KF于50mL的水中,搅拌溶解,分别加入1g的磁性C3N4,吸附,搅拌10h,过滤,干燥,得到碳基磁性固体碱催化剂。
【实施例2】
在催化剂的制备条件与实施例1完全相同的情况下,只将合成C3N4的前驱体三聚氰胺改为尿素,制得碳基磁性固体碱催化剂。
【实施例3】
在催化剂的制备条件与实施例1完全相同的情况下,只将成C3N4的前驱体三聚氰胺改为二氰二胺,制得碳基磁性固体碱催化剂。
【实施例4】
在催化剂的制备条件与实施例1完全相同的情况下,只将合成固体碱活性组分KF改为NaF,制得碳基磁性固体碱催化剂。
【反应实施例5-8】
在150mL圆底烧瓶中,加入反应物18g大豆油及9g甲醇,加入1.5g碳基磁性固体碱催化剂,在反应温度为60℃,反应时间为4h。以大豆油转化率C、生物柴油收率Y为指标,所得催化剂的催化性能如表1所示。
表1碳基磁性固体碱催化剂合成生物柴油的反应结果
【反应实施例9】
碳基磁性固体碱催化剂的反复使用性能。
在150mL圆底烧瓶中,加入反应物18g大豆油及9g甲醇,分别使用催化剂制备的实施例1所制得催化剂各2g,在反应温度为60℃,反应时间为4h。反应后将碳基磁性固体碱催化剂过滤,60℃干燥4h,将该催化剂再循环使用,以大豆油转化率C、生物柴油收率Y为指标,催化剂的反应性能如表2所示。
表2碳基磁性固体碱催化剂的重复利用性能
Claims (3)
1.一种合成生物柴油碳基磁性固体碱催化剂的制备方法,其特征在于包括以下过程,
(1)将5~10g前驱体,放在带盖的坩埚里用马弗炉焙烧,5~8°/min升温到500~600℃保持2~8h,得到黄色的固体C3N4载体;
(2)将1~3g的载体C3N4超声分散在40~80mL的乙二醇溶液中,1~3g的FeCl3·6H2O加入到溶液中,搅拌10~30min,加入4~10mL的80%的一水合肼水溶液,继续搅拌20~50min,转移至150~200℃的烘箱中,水热8~14h,分别用去离子水和乙醇各洗涤3~6次,磁性分离,在60~80℃下,真空干燥20~36h,得到磁性载体C3N4;
(3)将5~50g的固体碱活性组分置于40~100mL的水中,搅拌溶解,分别加入1~3g的磁性载体C3N4,搅拌8~12h,过滤,干燥,得到碳基磁性固体碱催化剂。
2.按权利要求1所述的合成生物柴油碳基磁性固体碱催化剂的制备方法,其特征在于,上述前驱体为三聚氰胺、二氰二胺、硫脲或尿素的任何一种。
3.按权利要求1所述的合成生物柴油碳基磁性固体碱催化剂的制备方法,其特征在于,上述固体碱活性组分为KF、KOH、K2CO3、NaF、NaOH或Na2CO3的任何一种。
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