CN107899549A - 一种改性柚子皮纤维吸油材料的制备方法 - Google Patents
一种改性柚子皮纤维吸油材料的制备方法 Download PDFInfo
- Publication number
- CN107899549A CN107899549A CN201711161857.1A CN201711161857A CN107899549A CN 107899549 A CN107899549 A CN 107899549A CN 201711161857 A CN201711161857 A CN 201711161857A CN 107899549 A CN107899549 A CN 107899549A
- Authority
- CN
- China
- Prior art keywords
- pomelo peel
- oil absorption
- absorption material
- preparation
- oil
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000463 material Substances 0.000 title claims abstract description 45
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 240000000560 Citrus x paradisi Species 0.000 title abstract 3
- 239000000835 fiber Substances 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 244000276331 Citrus maxima Species 0.000 claims description 78
- 235000001759 Citrus maxima Nutrition 0.000 claims description 32
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000005422 blasting Methods 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 20
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 19
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 18
- 238000004880 explosion Methods 0.000 claims description 14
- 229960000583 acetic acid Drugs 0.000 claims description 12
- 239000012065 filter cake Substances 0.000 claims description 12
- 239000012362 glacial acetic acid Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 10
- 238000007605 air drying Methods 0.000 claims description 10
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 9
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 claims description 8
- 229960002218 sodium chlorite Drugs 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 239000001913 cellulose Substances 0.000 abstract description 9
- 229920002678 cellulose Polymers 0.000 abstract description 9
- 229920005610 lignin Polymers 0.000 abstract description 4
- 229920002488 Hemicellulose Polymers 0.000 abstract description 2
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 abstract description 2
- 238000003851 corona treatment Methods 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract description 2
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- 210000000630 fibrocyte Anatomy 0.000 abstract description 2
- 230000002209 hydrophobic effect Effects 0.000 abstract description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- 239000012783 reinforcing fiber Substances 0.000 abstract description 2
- 125000004185 ester group Chemical group 0.000 abstract 2
- 230000004048 modification Effects 0.000 abstract 1
- 238000012986 modification Methods 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 60
- 210000004027 cell Anatomy 0.000 description 5
- 239000002270 dispersing agent Substances 0.000 description 5
- 239000003463 adsorbent Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000003305 oil spill Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- 150000001408 amides Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000004965 Silica aerogel Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 150000002148 esters Chemical group 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- KRQUFUKTQHISJB-YYADALCUSA-N 2-[(E)-N-[2-(4-chlorophenoxy)propoxy]-C-propylcarbonimidoyl]-3-hydroxy-5-(thian-3-yl)cyclohex-2-en-1-one Chemical compound CCC\C(=N/OCC(C)OC1=CC=C(Cl)C=C1)C1=C(O)CC(CC1=O)C1CCCSC1 KRQUFUKTQHISJB-YYADALCUSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 206010021143 Hypoxia Diseases 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000007954 hypoxia Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/485—Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Fats And Perfumes (AREA)
Abstract
本发明涉及一种改性柚子皮纤维吸油材料的制备方法,属于吸附材料技术领域。本发明采用柚子皮为吸油主体,利用高温高压蒸汽使纤维细胞内的冷凝水迅速蒸发膨胀,打破木质素包裹作用和纤维素结晶结构,显著增加材料的孔隙率,再用等离子体处理,激活纤维表面更多的活性位点,再进一步进行酯交换改性,纤维素上小分子量的羟基被大体积的乙酰基取代,削弱了分子间、分子内的氢键作用力,同时增大了空间位阻,一定程度的破坏了纤维素的结晶区结构,而且牢固包围结晶纤维素的半纤维素和木质素的凝聚态结构膨胀,从而导致酯交换改性后材料的孔隙率增大,增加纤维素本身的疏水亲油性,强化纤维素材料本身的空间结构,强化吸油性能。
Description
技术领域
本发明涉及一种改性柚子皮纤维吸油材料的制备方法,属于吸附材料技术领域。
背景技术
现在石油泄漏已经成为摧毁生态系统最严重事故之一。据有关报道统计,近几十年泄漏的石油等污染物已经使得近1000种海洋生物走向了灭绝。泄漏的石油烃类污染物漂浮在海面形成油膜,使得水中溶氧大大降低,海洋生物因此缺氧死亡。此外,石油中的镍、钒、有毒有机物以及石油分解过程中产生的一些有害物质分散在海洋中,不仅污染水体,严重影响当地渔业和旅游业的发展,而且会间接危害人类健康。由于海洋环境的复杂性,泄漏的石油会随着海水流动不断被稀释、扩散,与此同时伴随有沉降、乳化、生物降解等作用,但是这些对于溢油的处理来说微乎其微。
目前常见的海上溢油处理方法可分为三种:1、使用溢油分散剂将油类乳化分散成细小油滴以促进溢油的自然降解;2、原位燃烧浮油使其自然消失;3、使用吸附剂选择性吸收水中的油相。溢油分散剂是其中的一种吸附剂,它是由表面活性剂、有机溶剂、稳定剂等多种物质组成的混合物。使用溢油分散剂可以有效减少溢油污染,但是分散剂本身有一定毒性,大量分散剂的使用危害到海洋生物的生存。原位燃烧法处理费用低、操作简单、效果好,但是由于浮油的不完全燃烧会产生二次污染,不仅造成资源浪费且对生态环境造成不良影响。在这些方法中,使用吸附剂选择性移除油相是最有效、经济效率好、对环境友好的方法,原因在于该方法不仅能有效回收溢油且不会产生二次污染。
目前已出现一系列的吸附材料,从有机合成吸附剂如聚丙烯、聚苯乙烯到无机矿物材料包括有机质粘土、无机硅气凝胶和膨胀石墨等。但是,有机吸附材料的吸油能力有限,而硅气凝胶和膨胀石墨这类吸附材料生产成本过高从而限制了它们的广泛应用。同时,这些材料都不能生物降解。
因此,开发一种理想的具有较高的吸油倍数高,保油性能好,油水选择性强,浮力好,成本低,能够多次重复循环利用并且可生物降解的吸油材料显得尤为重要。
发明内容
本发明所要解决的技术问题:针对现有吸油材料吸油倍数低,保油性能差且不能生物降解的问题,提供了一种改性柚子皮纤维吸油材料的制备方法。
为解决上述技术问题,本发明采用的技术方案是:
(1)将柚子皮剥除外表皮后收集白色絮状物,水洗风干后粉碎,过40目筛,得预处理柚子皮;
(2)将预处理柚子皮装入蒸汽爆破罐中蒸汽爆破,用热水浸泡清洗后风干,得蒸汽爆破处理柚子皮;
(3)将蒸汽爆破处理柚子皮加入亚氯酸钠溶液中搅拌反应30~50min,用冰醋酸调节pH至4.0~4.5后过滤得滤饼,将滤饼加入氢氧化钠溶液中反应30~40min,再用冰醋酸调节pH至中性,过滤水洗后干燥,得柚子皮纤维;
(4)将柚子皮纤维置于低温等离子体处理箱中反应室的下电极进行辉光放电,得预处理柚子皮纤维;
(5)将预处理柚子皮纤维分散在N,N-二甲基甲酰胺中,再加入乙酸乙烯酯、碳酸钾,加热至60~80℃保温反应4~6h,冷却至室温后离心分离得沉淀,沉淀醇洗水洗后干燥,得改性柚子皮纤维吸油材料。
步骤(2)所述蒸汽爆破过程为向蒸汽爆破罐中通入1.5~2.5MPa温度为220~250℃水蒸汽,保持3~4min后瞬间打开蒸汽爆破罐阀门,泄压至常压后取出。
步骤(3)所述亚氯酸钠溶液的质量分数为5%,用量为蒸汽爆破处理柚子皮质量的16~24倍,所述氢氧化钠溶液的质量分数为5%,用量为蒸汽爆破处理柚子皮质量的16~24倍。
步骤(3)所述搅拌反应温度为70~75℃,所述反应温度为80~90℃。
步骤(4)所述辉光放电过程是控制功率为40~50W,压强为25~30Pa,进行辉光放电180~200s。
步骤(5)所述预处理柚子皮纤维、N,N-二甲基甲酰胺、乙酸乙烯酯、碳酸钾的重量份为50~60份预处理柚子皮纤维,50~60份N,N-二甲基甲酰胺,10~12份乙酸乙烯酯,75~90份碳酸钾。
本发明与其他方法相比,有益技术效果是:
(1)本发明采用具有大量沟槽,比表面积较大,具有松散网络结构的柚子皮为吸油主体,利用高温高压蒸汽通过扩散作用,渗透并浸润植物纤维的细胞壁,再突然降低压力,使纤维细胞内的冷凝水迅速蒸发膨胀,打破木质素包裹作用和纤维素结晶结构,显著增加材料的孔隙率,再用等离子体处理,激活纤维表面更多的活性位点,再进一步进行酯交换改性,纤维素上小分子量的羟基被大体积的乙酰基取代,削弱了分子间、分子内的氢键作用力,同时增大了空间位阻,一定程度的破坏了纤维素的结晶区结构,而且牢固包围结晶纤维素的半纤维素和木质素的凝聚态结构膨胀,从而导致酯交换改性后材料的孔隙率增大,增加纤维素本身的疏水亲油性,强化纤维素材料本身的空间结构,强化吸油性能;
(2)本发明制备的吸油材料吸附原油时,粒径对吸附除油基本无影响,2~5min就能达到吸附平衡,吸附速率快,低温条件有利于除油,且在各种酸碱条件下,中性吸油效果较好,吸油倍率波动较小,吸油量都相对较高。
具体实施方式
将柚子皮剥除外表皮后收集白色絮状物,用去离子水洗涤2~3次后自然风干,并装入粉碎机中粉碎,过40目筛,得预处理柚子皮,取300~500g预处理柚子皮装入蒸汽爆破罐中,并向蒸汽爆破罐中通入1.5~2.5MPa温度为220~250℃水蒸汽,保持3~4min后瞬间打开蒸汽爆破罐阀门,泄压至常压后取出,再浸泡在2~3L温度为80~85℃去离子水中40~50min,取出自然风干,得蒸汽爆破处理柚子皮,取100~120g蒸汽爆破处理柚子皮,加入2.0~2.4kg质量分数为5%亚氯酸钠溶液中,在70~75℃下以300~400r/min搅拌反应30~50min,并用冰醋酸调节pH至4.0~4.5,过滤得滤饼,将滤饼加入2.0~2.4kg质量分数为5%氢氧化钠溶液中,在80~90℃下继续搅拌反应30~40min,再用冰醋酸调节pH至中性,过滤得滤渣,用去离子水洗涤滤渣2~3次后置于烘箱中,在80~90℃下干燥至恒重,得柚子皮纤维,将柚子皮纤维置于低温等离子体处理箱中反应室的下电极,控制功率为40~50W,压强为25~30Pa,进行辉光放电180~200s,取出,得预处理柚子皮纤维,取50~60g预处理柚子皮纤维,加入50~60gN,N-二甲基甲酰胺中,以300~400r/min搅拌20~30min,再加入10~12g乙酸乙烯酯,75~90g碳酸钾,加热至60~80℃保温反应4~6h,冷却至室温后离心分离得沉淀,用无水乙醇洗涤沉淀2~3次再用去离子水洗涤2~3次,并转入干燥箱中,在90~100℃下干燥至恒重,得改性柚子皮纤维吸油材料。
实例1
将柚子皮剥除外表皮后收集白色絮状物,用去离子水洗涤2次后自然风干,并装入粉碎机中粉碎,过40目筛,得预处理柚子皮,取300g预处理柚子皮装入蒸汽爆破罐中,并向蒸汽爆破罐中通入1.5MPa温度为220℃水蒸汽,保持3min后瞬间打开蒸汽爆破罐阀门,泄压至常压后取出,再浸泡在2L温度为80℃去离子水中40min,取出自然风干,得蒸汽爆破处理柚子皮,取100g蒸汽爆破处理柚子皮,加入2.0kg质量分数为5%亚氯酸钠溶液中,在70℃下以300r/min搅拌反应30min,并用冰醋酸调节pH至4.0,过滤得滤饼,将滤饼加入2.0kg质量分数为5%氢氧化钠溶液中,在80℃下继续搅拌反应30min,再用冰醋酸调节pH至中性,过滤得滤渣,用去离子水洗涤滤渣2次后置于烘箱中,在80℃下干燥至恒重,得柚子皮纤维,将柚子皮纤维置于低温等离子体处理箱中反应室的下电极,控制功率为40W,压强为25Pa,进行辉光放电180s,取出,得预处理柚子皮纤维,取50g预处理柚子皮纤维,加入50gN,N-二甲基甲酰胺中,以300r/min搅拌20min,再加入10g乙酸乙烯酯,75g碳酸钾,加热至60℃保温反应4h,冷却至室温后离心分离得沉淀,用无水乙醇洗涤沉淀2次再用去离子水洗涤2次,并转入干燥箱中,在90℃下干燥至恒重,得改性柚子皮纤维吸油材料。
实例2
将柚子皮剥除外表皮后收集白色絮状物,用去离子水洗涤2次后自然风干,并装入粉碎机中粉碎,过40目筛,得预处理柚子皮,取400g预处理柚子皮装入蒸汽爆破罐中,并向蒸汽爆破罐中通入2.0MPa温度为230℃水蒸汽,保持3min后瞬间打开蒸汽爆破罐阀门,泄压至常压后取出,再浸泡在2L温度为82℃去离子水中45min,取出自然风干,得蒸汽爆破处理柚子皮,取110g蒸汽爆破处理柚子皮,加入2.2kg质量分数为5%亚氯酸钠溶液中,在72℃下以350r/min搅拌反应40min,并用冰醋酸调节pH至4.2,过滤得滤饼,将滤饼加入2.2kg质量分数为5%氢氧化钠溶液中,在85℃下继续搅拌反应35min,再用冰醋酸调节pH至中性,过滤得滤渣,用去离子水洗涤滤渣2次后置于烘箱中,在85℃下干燥至恒重,得柚子皮纤维,将柚子皮纤维置于低温等离子体处理箱中反应室的下电极,控制功率为45W,压强为28Pa,进行辉光放电190s,取出,得预处理柚子皮纤维,取55g预处理柚子皮纤维,加入55gN,N-二甲基甲酰胺中,以350r/min搅拌25min,再加入11g乙酸乙烯酯,85g碳酸钾,加热至70℃保温反应5h,冷却至室温后离心分离得沉淀,用无水乙醇洗涤沉淀2次再用去离子水洗涤2次,并转入干燥箱中,在95℃下干燥至恒重,得改性柚子皮纤维吸油材料。
实例3
将柚子皮剥除外表皮后收集白色絮状物,用去离子水洗涤3次后自然风干,并装入粉碎机中粉碎,过40目筛,得预处理柚子皮,取500g预处理柚子皮装入蒸汽爆破罐中,并向蒸汽爆破罐中通入2.5MPa温度为250℃水蒸汽,保持4min后瞬间打开蒸汽爆破罐阀门,泄压至常压后取出,再浸泡在3L温度为85℃去离子水中50min,取出自然风干,得蒸汽爆破处理柚子皮,取120g蒸汽爆破处理柚子皮,加入2.4kg质量分数为5%亚氯酸钠溶液中,在75℃下以400r/min搅拌反应50min,并用冰醋酸调节pH至4.5,过滤得滤饼,将滤饼加入2.4kg质量分数为5%氢氧化钠溶液中,在90℃下继续搅拌反应40min,再用冰醋酸调节pH至中性,过滤得滤渣,用去离子水洗涤滤渣3次后置于烘箱中,在90℃下干燥至恒重,得柚子皮纤维,将柚子皮纤维置于低温等离子体处理箱中反应室的下电极,控制功率为50W,压强为30Pa,进行辉光放电200s,取出,得预处理柚子皮纤维,取60g预处理柚子皮纤维,加入60gN,N-二甲基甲酰胺中,以400r/min搅拌30min,再加入12g乙酸乙烯酯,90g碳酸钾,加热至80℃保温反应6h,冷却至室温后离心分离得沉淀,用无水乙醇洗涤沉淀3次再用去离子水洗涤3次,并转入干燥箱中,在100℃下干燥至恒重,得改性柚子皮纤维吸油材料。
对照例:浙江某公司生产的吸油材料。
将实例及对照例的吸油材料进行检测,具体检测如下:
吸油性能的测定方法:将装有200mL风化后的油品的500mL烧杯放在20℃的恒温水浴中预热20min后,再将0.1g左右的吸油材料放到自制的铁丝网上,然后将铁丝网缓缓浸入待测油品中,分别在5s、10s、20s、30s、1min、2min、3min、5min、10min、15min时,称重(扣除丝网及丝网上粘附油品的质量),计算吸油材料的吸附量,以吸油倍率(g/g)表示。
保油性测试:称取吸油材料W1放于油品中,待其吸附15min后,移出至不锈钢网上,静置5min,称重,记为W2,分别在5min、10min、20min、40min、60min、90min和120min沥干后,取出材料称重,记为W3。
回用性测试:将吸附饱和后的吸油材料放在不锈钢网上沥干,至不再滴油为止,称取吸油材料吸油后的质量,并记下来。然后将材料放入离心机进行油和材料的分离,分离5min后进行称重,再次进行吸附及称重,然后不断重复上述过程。
具体检测结果如表1。
表1
检测项目 | 实例1 | 实例2 | 实例3 | 对照例 |
吸油倍率(g/g) | 68.26 | 62.57 | 52.3 | 43.57 |
持有率(%) | 90 | 89 | 91 | 75 |
回用率(%) | 92.57 | 91.32 | 88.68 | 75.93 |
由表1可知,本发明制备的吸油材料具有较高的吸油倍数高,保油性能好,成本低并且能够多次重复循环利用。
Claims (6)
1.一种改性柚子皮纤维吸油材料的制备方法,其特征在于具体制备步骤为:
(1)将柚子皮剥除外表皮后收集白色絮状物,水洗风干后粉碎,过40目筛,得预处理柚子皮;
(2)将预处理柚子皮装入蒸汽爆破罐中蒸汽爆破,用热水浸泡清洗后风干,得蒸汽爆破处理柚子皮;
(3)将蒸汽爆破处理柚子皮加入亚氯酸钠溶液中搅拌反应30~50min,用冰醋酸调节pH至4.0~4.5后过滤得滤饼,将滤饼加入氢氧化钠溶液中反应30~40min,再用冰醋酸调节pH至中性,过滤水洗后干燥,得柚子皮纤维;
(4)将柚子皮纤维置于低温等离子体处理箱中反应室的下电极进行辉光放电,得预处理柚子皮纤维;
(5)将预处理柚子皮纤维分散在N,N-二甲基甲酰胺中,再加入乙酸乙烯酯、碳酸钾,加热至60~80℃保温反应4~6h,冷却至室温后离心分离得沉淀,沉淀醇洗水洗后干燥,得改性柚子皮纤维吸油材料。
2.如权利要求1所述的一种改性柚子皮纤维吸油材料的制备方法,其特征在于,步骤(2)所述蒸汽爆破过程为向蒸汽爆破罐中通入1.5~2.5MPa温度为220~250℃水蒸汽,保持3~4min后瞬间打开蒸汽爆破罐阀门,泄压至常压后取出。
3.如权利要求1所述的一种改性柚子皮纤维吸油材料的制备方法,其特征在于,步骤(3)所述亚氯酸钠溶液的质量分数为5%,用量为蒸汽爆破处理柚子皮质量的16~24倍,所述氢氧化钠溶液的质量分数为5%,用量为蒸汽爆破处理柚子皮质量的16~24倍。
4.如权利要求1所述的一种改性柚子皮纤维吸油材料的制备方法,其特征在于,步骤(3)所述搅拌反应温度为70~75℃,所述反应温度为80~90℃。
5.如权利要求1所述的一种改性柚子皮纤维吸油材料的制备方法,其特征在于,步骤(4)所述辉光放电过程是控制功率为40~50W,压强为25~30Pa,进行辉光放电180~200s。
6.如权利要求1所述的一种改性柚子皮纤维吸油材料的制备方法,其特征在于,步骤(5)所述预处理柚子皮纤维、N,N-二甲基甲酰胺、乙酸乙烯酯、碳酸钾的重量份为50~60份预处理柚子皮纤维,50~60份N,N-二甲基甲酰胺,10~12份乙酸乙烯酯,75~90份碳酸钾。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201711161857.1A CN107899549A (zh) | 2017-11-21 | 2017-11-21 | 一种改性柚子皮纤维吸油材料的制备方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201711161857.1A CN107899549A (zh) | 2017-11-21 | 2017-11-21 | 一种改性柚子皮纤维吸油材料的制备方法 |
Publications (1)
Publication Number | Publication Date |
---|---|
CN107899549A true CN107899549A (zh) | 2018-04-13 |
Family
ID=61846717
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201711161857.1A Pending CN107899549A (zh) | 2017-11-21 | 2017-11-21 | 一种改性柚子皮纤维吸油材料的制备方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN107899549A (zh) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108636435A (zh) * | 2018-04-24 | 2018-10-12 | 周荣 | 一种光催化降解甲醛功能泡沫炭的制备方法 |
CN108993424A (zh) * | 2018-07-18 | 2018-12-14 | 天津科技大学 | 一种多孔木质素吸附剂的制备及再生方法 |
CN111661978A (zh) * | 2020-05-28 | 2020-09-15 | 浙江美福石油化工有限责任公司 | 一种环保型低成本高含油废水处理工艺 |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103143326A (zh) * | 2013-01-08 | 2013-06-12 | 天津大学 | 以纤维素为基体的吸油材料及其制备方法 |
CN106117463A (zh) * | 2016-06-26 | 2016-11-16 | 吴迪 | 一种可生物降解吸油树脂制备方法 |
CN106146757A (zh) * | 2016-06-30 | 2016-11-23 | 宁波江东波莫纳电子科技有限公司 | 一种改性玉米秸秆纤维吸油材料的制备方法 |
-
2017
- 2017-11-21 CN CN201711161857.1A patent/CN107899549A/zh active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103143326A (zh) * | 2013-01-08 | 2013-06-12 | 天津大学 | 以纤维素为基体的吸油材料及其制备方法 |
CN106117463A (zh) * | 2016-06-26 | 2016-11-16 | 吴迪 | 一种可生物降解吸油树脂制备方法 |
CN106146757A (zh) * | 2016-06-30 | 2016-11-23 | 宁波江东波莫纳电子科技有限公司 | 一种改性玉米秸秆纤维吸油材料的制备方法 |
Non-Patent Citations (1)
Title |
---|
李敬芬: "《药物合成反应》", 21 August 2010, 浙江大学出版社 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108636435A (zh) * | 2018-04-24 | 2018-10-12 | 周荣 | 一种光催化降解甲醛功能泡沫炭的制备方法 |
CN108993424A (zh) * | 2018-07-18 | 2018-12-14 | 天津科技大学 | 一种多孔木质素吸附剂的制备及再生方法 |
CN108993424B (zh) * | 2018-07-18 | 2021-02-05 | 天津科技大学 | 一种多孔木质素吸附剂的制备及再生方法 |
CN111661978A (zh) * | 2020-05-28 | 2020-09-15 | 浙江美福石油化工有限责任公司 | 一种环保型低成本高含油废水处理工艺 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Mashkoor et al. | Preparation, characterization and adsorption studies of the chemically modified Luffa aegyptica peel as a potential adsorbent for the removal of malachite green from aqueous solution | |
Gupta et al. | Column operation studies for the removal of dyes and phenols using a low cost adsorbent | |
Ahmad et al. | Adsorption of direct dye on palm ash: Kinetic and equilibrium modeling | |
Sathishkumar et al. | Utilization of agro-industrial waste Jatropha curcas pods as an activated carbon for the adsorption of reactive dye Remazol Brilliant Blue R (RBBR) | |
Ahmad et al. | Reduction of COD and color of dyeing effluent from a cotton textile mill by adsorption onto bamboo-based activated carbon | |
CN107899549A (zh) | 一种改性柚子皮纤维吸油材料的制备方法 | |
Jing et al. | Flexible, versatility and superhydrophobic biomass carbon aerogels derived from corn bracts for efficient oil/water separation | |
Hameed | Grass waste: A novel sorbent for the removal of basic dye from aqueous solution | |
Chen et al. | Effective removal of methyl orange and rhodamine B from aqueous solution using furfural industrial processing waste: Furfural residue as an eco-friendly biosorbent | |
Sidiras et al. | Simulation of autohydrolysis effect on adsorptivity of wheat straw in the case of oil spill cleaning | |
Li et al. | Oil removal from water with yellow horn shell residues treated by ionic liquid | |
CN107337764B (zh) | 玉米秸穰半纤维素基疏水温敏凝胶的制备方法及应用 | |
Daud et al. | Feasibility of banana (Musa sapientum) trunk biofibres for treating kitchen wastewater | |
Narayanan et al. | Theoretical and experimental investigation on the removal of oil spill by selective sorbents | |
Zhang et al. | A new type of calcium-rich biochars derived from spent mushroom substrates and their efficient adsorption properties for cationic dyes | |
Radouane et al. | Removal of the cationic textile dye by Recycled newspaper pulp and its cellulose microfibers extracted: Characterization, release, and adsorption studies | |
Nguyen et al. | Highlights of oil treatment technologies and rise of oil-absorbing materials in ocean cleaning strategy | |
Chakraborty et al. | Adsorption of crystal violet from aqueous solution onto sugarcane bagasse: central composite design for optimization of process variables | |
Liu et al. | Crude oil removal from aqueous solution using raw and carbonized Xanthoceras sorbifolia shells | |
CN108993429A (zh) | 一种染料及印染废水处理用吸附剂及其制备方法 | |
CN103331149A (zh) | 一种海绵状高分子吸附材料 | |
CN103360571A (zh) | 一种基于废植物纤维的高吸油材料的制备方法 | |
Cardoso et al. | Kinetic and equilibrium study of petroleum adsorption using pre-treated coconut fibers Estudo cinético e de equilíbrio de adsorção de petróleo utilizando fibras de coco pré-tratadas Estudio cinético y de equilibrio de la adsorción de petroleo con fibras de coco pretratadas | |
Rodríguez-Ramírez et al. | Hemicelluloses hydrogel: Synthesis, characterization, and application in dye removal | |
Vo et al. | Removal of pararosaniline hydrochloride (basic red 9) from aqueous system with lignocellulose fraction of sugarcane bagasse as adsorbent |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
TA01 | Transfer of patent application right | ||
TA01 | Transfer of patent application right |
Effective date of registration: 20180412 Address after: 213000 Room 302, unit 5, Cui Yuan Apartment, Tianning District, Changzhou, Jiangsu Applicant after: Wu Gang Address before: 213164 B 2519, Beijing University of Chemical Technology Research Institute, Changzhou science and Education City, 801 Wujin Road, Wujin, Changzhou. Applicant before: TRUSYN CHEM-TECH CO., LTD. |
|
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
WD01 | Invention patent application deemed withdrawn after publication | ||
WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180413 |