CN110280215A - 一种纳米银-笋壳生物炭复合材料的制备方法及应用 - Google Patents
一种纳米银-笋壳生物炭复合材料的制备方法及应用 Download PDFInfo
- Publication number
- CN110280215A CN110280215A CN201910735896.0A CN201910735896A CN110280215A CN 110280215 A CN110280215 A CN 110280215A CN 201910735896 A CN201910735896 A CN 201910735896A CN 110280215 A CN110280215 A CN 110280215A
- Authority
- CN
- China
- Prior art keywords
- bamboo shoot
- shoot shell
- nano silver
- carbon composite
- biology carbon
- 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.)
- Granted
Links
- 239000011425 bamboo Substances 0.000 title claims abstract description 78
- 239000002131 composite material Substances 0.000 title claims abstract description 37
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims abstract description 40
- 235000017491 Bambusa tulda Nutrition 0.000 claims abstract description 40
- 241001330002 Bambuseae Species 0.000 claims abstract description 40
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims abstract description 40
- 239000003610 charcoal Substances 0.000 claims abstract description 30
- 238000001035 drying Methods 0.000 claims abstract description 22
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 14
- UZVQOEUTOCRSJN-UHFFFAOYSA-N silver 2-hydroxypropane-1,2,3-tricarboxylic acid nitrate Chemical compound [N+](=O)([O-])[O-].[Ag+].C(CC(O)(C(=O)O)CC(=O)O)(=O)O UZVQOEUTOCRSJN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 8
- 229910052709 silver Inorganic materials 0.000 claims abstract description 8
- 239000004332 silver Substances 0.000 claims abstract description 8
- 238000003723 Smelting Methods 0.000 claims abstract description 6
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 6
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000007873 sieving Methods 0.000 claims abstract description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 30
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 21
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 10
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 230000004913 activation Effects 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000001569 carbon dioxide Substances 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000003763 carbonization Methods 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- XEFGHVQACKIFMS-UHFFFAOYSA-N 2-hydroxypropane-1,2,3-tricarboxylic acid;nitric acid Chemical compound O[N+]([O-])=O.OC(=O)CC(O)(C(O)=O)CC(O)=O XEFGHVQACKIFMS-UHFFFAOYSA-N 0.000 claims description 2
- 239000010420 shell particle Substances 0.000 claims 2
- 230000003213 activating effect Effects 0.000 claims 1
- 238000005469 granulation Methods 0.000 claims 1
- 230000003179 granulation Effects 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 12
- 239000002699 waste material Substances 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000002156 mixing Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000010815 organic waste Substances 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract 2
- 239000000243 solution Substances 0.000 description 22
- 229910052702 rhenium Inorganic materials 0.000 description 19
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 description 19
- 238000002474 experimental method Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 241001417490 Sillaginidae Species 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000002211 L-ascorbic acid Substances 0.000 description 2
- 235000000069 L-ascorbic acid Nutrition 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000009388 chemical precipitation Methods 0.000 description 2
- 150000001455 metallic ions Chemical class 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- GDSOZVZXVXTJMI-SNAWJCMRSA-N (e)-1-methylbut-1-ene-1,2,4-tricarboxylic acid Chemical compound OC(=O)C(/C)=C(C(O)=O)\CCC(O)=O GDSOZVZXVXTJMI-SNAWJCMRSA-N 0.000 description 1
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- USWJSZNKYVUTIE-UHFFFAOYSA-N bis(sulfanylidene)rhenium Chemical compound S=[Re]=S USWJSZNKYVUTIE-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 150000005837 radical ions Chemical class 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- USBWXQYIYZPMMN-UHFFFAOYSA-N rhenium;heptasulfide Chemical compound [S-2].[S-2].[S-2].[S-2].[S-2].[S-2].[S-2].[Re].[Re] USBWXQYIYZPMMN-UHFFFAOYSA-N 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
-
- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
-
- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28061—Surface area, e.g. B.E.T specific surface area being in the range 100-500 m2/g
-
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
-
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
-
- 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
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4881—Residues from shells, e.g. eggshells, mollusk shells
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Carbon And Carbon Compounds (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
本发明公开了一种纳米银‑笋壳生物炭复合材料的制备方法及应用。制备方法包括以下步骤:1)制粒:将洗净、干燥的竹笋壳粉碎,过筛;2)炭化:在惰性气氛中以一定温度炭化笋壳并冷却至室温,取出,用去离子水洗涤至中性,烘干,制得笋壳生物炭;3)载银:取笋壳生物炭和硝酸银‑柠檬酸溶液混合,向其中滴加抗坏血酸溶液,置于水浴中搅拌,浸渍,过滤,洗涤,烘干;4)活化:取适量步骤3)所得的产物,在惰性气氛中活化一定时间后冷却至室温,洗涤至中性,烘干,制得纳米银‑笋壳生物炭复合材料。本发明利用农林废弃物竹笋壳为原料制备纳米银‑笋壳生物炭复合材料,原料丰富、制备简单并对冶炼废酸溶液中高铼酸根的吸附效果显著。
Description
技术领域
本发明属于复合材料技术领域,具体涉及一种纳米银-笋壳生物炭复合材料的制备方法及应用。
背景技术
铼是一种稀散元素,银白色金属,具有高强度、高熔点、优异的延展性、机械稳定性和可塑性,是重要的金属材料。铼及其合金被广泛引用在石油化工、国防、航空航天、冶金等行业。
铼在地壳中丰度低,无可供直接开采的矿物,通常以二硫化铼或七硫化二铼形式伴生于辉钼矿和斑岩铜矿中。在冶炼过程中,铼主要以高铼酸根离子形式进入冶炼酸性废液,该冶炼酸性废液具有铼含量低、酸性强和共存金属离子浓度高且复杂等特点。
从冶炼酸性废液中提铼的方法常见的有,化学沉淀法,离子交换法和溶剂萃取法。化学沉淀法提铼常需添加共沉淀剂,易形成沉淀夹带,后续处理以及进一步从沉淀中分离纯化铼困难;离子交换法分离铼,收率高,选择性好,但离子交换剂价格昂贵,易中毒,再生频繁,失活离子交换树脂难以处理;溶剂萃取法操作简便、选择性好、分离效率高,但是萃取剂价格昂贵,多为易燃、易挥发和有毒物质,生产管理要求严格,易形成环境污染。且上述三种方法均难以适用于低浓度含铼原料液,使用前均需对低浓度含铼原料液进行提浓富集预处理。
生物炭是生物质在绝氧和相对低温(小于700℃)条件下裂解炭化而形成的一种炭材料,具有较高的比表面积、丰富的含氧官能团等特征,可以用于溶液中金属离子的分离,尤其适用于高效吸附分离溶液中低浓度金属离子。
农林废弃物,例如竹笋加工业大宗副产物笋壳难以利用,一般焚烧或填埋处理,易造成环境污染,但其可作为制备生物炭的低廉、绿色环保、可持续的制备原料,但所得原状生物炭用于吸附分离溶液中低浓度铼存在吸附量小、选择性差的缺点需对其改性以提高其性能。
发明内容
本发明的目的在于提供一种纳米银-笋壳生物炭复合材料的制备方法及应用。本发明纳米银-笋壳生物炭复合材料的制备方法工艺简单、操作便捷。并将纳米银-笋壳生物炭复合材料应用于高效吸附分离冶炼废酸溶液中的高铼酸根。
本发明采用如下技术方案:
一种纳米银-笋壳生物炭复合材料的制备方法,包括以下步骤:
1)制粒:将笋壳洗净,干燥,粉碎,过筛。
2)炭化:将步骤1)制粒所得的笋壳在惰性气氛中以一定的温度炭化笋壳并冷却至室温,洗涤至中性,烘干,制得笋壳生物炭。
3)载银:将步骤2)制得的笋壳生物炭与硝酸银-柠檬酸溶液混合,向其中滴加抗坏血酸溶液,并置于水浴中搅拌,浸渍,过滤,洗涤,烘干。
4)活化:将步骤3)制得的产物,在惰性气氛中一定温度下活化后,冷却至室温,去离子水洗涤至中性,烘干,得纳米银-笋壳生物炭复合材料。
上述所诉步骤1)中干燥温度为60-100℃,笋壳粉碎后过20-100目筛。
上述步骤2)中,惰性气氛为氮气、氩气、二氧化碳中的一种,其流速为50-150 mL/min,炭化温度为200-600℃,炭化时间为2-6 h。
上述步骤3)中,硝酸银-柠檬酸溶液中硝酸银与柠檬酸摩尔比为1:1,硝酸银浓度为1 mmol/L,柠檬酸浓度为1 mmol/L;抗坏血酸溶液浓度为10-20 mmol/L;硝酸银-柠檬酸溶液与抗坏血酸溶液体积比为2~3:1;笋壳生物炭与硝酸银-柠檬酸溶液固液比1g:20-50mL,浸渍时间为6-20 h,烘干温度为40-100 ℃。
上述步骤4)中,惰性气体为氮气、氩气、二氧化碳中的一种,流速为50-100 mL/min,活化温度为250-550 ℃,活化时间为1-6 h。
上述步骤4)中,所得纳米银-笋壳生物炭复合材料中纳米银粒径为20-60 nm。
一种上述制备方法制得的纳米银-笋壳生物炭复合材料。
一种上述制备方法制得的纳米银-笋壳生物炭复合材料应用于高效吸附分离冶炼废酸溶液中高铼酸根。
本发明的优势及其有效益效果:
1.本发明将农林废弃物笋壳制成复合材料载体,成本低廉,既能减轻环境污染又能达到“以废治废”的效果。
2.本发明制得的纳米银-笋壳生物炭吸附分离冶炼废酸溶液中的高铼酸根离子,纳米银为高铼酸根离子的有效吸附位点,并与之形成外层络合,最大吸附量为200 mg/g。
3.纳米银-笋壳生物炭复合材料比表面积最大为300 m2/g,比原状笋壳生物炭比表面积7.69 m2/g大40多倍,提供更多的有效吸附位点,利用吸附分离冶炼废酸溶液中的高铼酸根离子。
附图说明
图1为笋壳生物炭SEM图。
图2 为本发明所制备的一种纳米银-笋壳生物炭SEM图。
图3为本发明所制备的一种纳米银-笋壳生物炭及笋壳生物炭XRD图。
具体实施方式
实施例1
一种纳米银-笋壳生物炭复合材料的制备方法,包括以下步骤:
(1) 制粒:将笋壳洗净、60℃干燥后粉碎,过60目筛;
(2) 炭化:取适量过筛的笋壳,置于管式炉中,通入N2流速为100 mL/min,500℃下炭化4 h,冷却至室温后取出,洗涤至中性,烘干,制得笋壳生物炭;
(3) 载银:取1g笋壳生物炭与25 mL硝酸银-柠檬酸溶液(硝酸银与柠檬酸摩尔比为1:1,硝酸银浓度为1 mmol/L,柠檬酸浓度为1 mmol/L)混合,向其中滴加9mL10 mmol/L抗坏血酸溶液,置于25 ℃水浴中,搅拌,浸渍6 h,过滤,洗涤至中性,70℃烘干;
(4) 活化:取适量步骤(3)中制得的产物,置于程序控温管式炉中,通入N2流速为100mL/min,500 ℃下活化1 h,冷却至室温后取出,洗涤至中性,烘干,得到纳米银-笋壳生物炭复合材料,纳米银粒径为20 nm,比表面积为216 m2/g。
实施例2
一种纳米银-笋壳生物炭复合材料的制备方法及其应用,包括以下步骤:
(1) 制粒:将笋壳洗净、100℃干燥后粉碎,过20目筛;
(2) 炭化:取适量过筛的笋壳,置于管式炉中,通入CO2流速为100 mL/min,200℃下炭化6 h,冷却至室温后取出,洗涤至中性,烘干,制得笋壳生物炭;
(3) 载银:取1g笋壳生物炭与30mL 硝酸银-柠檬酸溶液(硝酸银与柠檬酸摩尔比为1:1,硝酸银浓度为1 mmol/L,柠檬酸浓度为1 mmol/L)混合,随后向混合溶液中滴加12 mL15mmol/L抗坏血酸溶液,置于25 ℃水浴中,搅拌,浸渍12 h,过滤,洗涤至中性,40℃烘干;
(4) 活化:取适量步骤(3)中制得的产物,置于程序控温管式炉中,通入CO2流速为50mL/min,250 ℃下活化6 h,冷却至室温后取出,洗涤至中性,烘干,得到纳米银-笋壳生物炭复合材料,纳米银粒径为37nm,比表面积为205 m2/g。
实施例3
一种纳米银-笋壳生物炭复合材料的制备方法及其应用,包括以下步骤:
(1) 制粒:将笋壳洗净、80℃干燥后粉碎,得到笋壳碎末过100目筛;
(2) 炭化:取适量过筛的笋壳,置于管式炉中,通入Ar流速为100 mL/min,600℃下炭化2 h,冷却至室温后取出,洗涤至中性,烘干,制得笋壳生物炭;
(3) 载银:取1g笋壳生物炭与35 mL 硝酸银-柠檬酸溶液(硝酸银与柠檬酸摩尔比为1:1,硝酸银浓度为1 mmol/L,柠檬酸浓度为1 mmol/L)混合,随后向混合溶液中滴加15mL 20mmol/L抗坏血酸溶液,置于25 ℃水浴中,搅拌,浸渍20 h,过滤,洗涤至中性,100℃烘干;
(4) 活化:取适量步骤(3)中制得的产物,置于程序控温管式炉中,通入N2流速为80mL/min,550 ℃下活化3h,冷却至室温后取出,洗涤至中性,烘干,得到纳米银-笋壳生物炭复合材料,纳米银粒径为60 nm,比表面积为222 m2/g。
应用实施例1
取0.01g笋壳生物炭加入到100 mL铼浓度为20 mg/L溶液中进行吸附实验,吸附平衡后的吸附量为14 mg/g;取0.01g实施例1制备的纳米银-笋壳生物炭复合材料加入到100 mL铼浓度为20 mg/L溶液中进行吸附实验,吸附平衡后的吸附量为185 mg/g。取0.01g笋壳生物炭加入到200 mL铼浓度为10 mg/L溶液中进行吸附实验,吸附平衡后的吸附量为6 mg/g;取0.01g实施例1制备的纳米银-笋壳生物炭复合材料加入到200mL铼浓度为10mg/L溶液中进行吸附实验,吸附平衡后的吸附量为115 mg/g。
应用实施例2
取0.01g实施例1制备的纳米银-笋壳生物炭复合材料加入到100 mL含有Cl-、NO2 -、NO3 -、SO4 2-、ReO4 -五元离子共存的溶液中且摩尔比Cl-:NO2 -:NO3 -:SO4 2-:ReO4 -为300:800:310:0.0350:1,纳米银-笋壳生物炭复合材料选择性吸附溶液Re(VII),吸附效率为70 %。
以上所述仅为本发明的较佳实施列,凡依本发明申请专利范围所做的均等变化与修饰,皆应属于本发明的涵盖范围。
Claims (8)
1.一种纳米银-笋壳生物炭复合材料的制备方法,其特征在于,包括以下步骤:
1)制粒:将洗净、干燥的笋壳粉碎,过筛,制得笋壳颗粒,备用;
2)炭化:将步骤1)制粒所得的笋壳颗粒在惰性气氛中炭化,冷却至室温,洗涤至中性,烘干,制得笋壳生物炭;
3)载银:将步骤2)制得的笋壳生物炭与硝酸银-柠檬酸溶液混合,向其中滴加抗坏血酸溶液,并置于水浴中搅拌,浸渍,过滤,洗涤,烘干;
4)活化:取适量步骤3)制得的产物,在惰性气氛中活化后冷却至室温,洗涤至中性,烘干,得到纳米银-笋壳生物炭复合材料。
2.根据权利要求1所述的一种纳米银-笋壳生物炭复合材料的制备方法,其特征在于:所述步骤1)中干燥温度为60-100 ℃,笋壳粉碎后过20-100目筛。
3.根据权利要求1所述的一种纳米银-笋壳生物炭复合材料的制备方法,其特征在于:所述步骤2)中,惰性气体为氮气、氩气、二氧化碳中的一种,流速为50-150 mL/min,炭化温度为200-600 ℃,炭化时间为1-5 h。
4.根据权利要求1所述的一种纳米银-笋壳生物炭复合材料的制备方法,其特征在于:所述步骤3) 硝酸银-柠檬酸溶液中硝酸银与柠檬酸摩尔比为1:1,硝酸银浓度为1mmol/L,柠檬酸浓度1 mmol/L,抗坏血酸溶液浓度为10-20 mmol/L;硝酸银-柠檬酸溶液与抗坏血酸溶液体积比为2~3:1;笋壳生物炭与硝酸银-柠檬酸溶液固液比1g:20-50mL,浸渍时间为1-20 h,烘干温度为40-100℃。
5.根据权利要求1所诉的一种纳米银-笋壳生物炭复合材料的制备方法,其特征在于:所述步骤4)中,惰性气体为氮气、氩气、二氧化碳中的一种,流速为50-100 mL/min,活化温度为250 ℃-550 ℃,活化时间为1-6 h。
6.根据权利要求1所述的一种纳米银-笋壳生物炭复合材料的制备方法,其特征在于:所述步骤4)中,所得纳米银-笋壳生物炭复合材料中纳米银粒径为20-60 nm。
7.如权利要求1-7任一项所述方法制备所得的纳米银-笋壳生物炭复合材料。
8.如权利要求7所述的纳米银-笋壳生物炭复合材料应用于高效吸附分离冶炼废酸溶液中高铼酸根。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910735896.0A CN110280215B (zh) | 2019-08-09 | 2019-08-09 | 一种纳米银-笋壳生物炭复合材料的制备方法及应用 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910735896.0A CN110280215B (zh) | 2019-08-09 | 2019-08-09 | 一种纳米银-笋壳生物炭复合材料的制备方法及应用 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN110280215A true CN110280215A (zh) | 2019-09-27 |
CN110280215B CN110280215B (zh) | 2020-08-11 |
Family
ID=68025036
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201910735896.0A Expired - Fee Related CN110280215B (zh) | 2019-08-09 | 2019-08-09 | 一种纳米银-笋壳生物炭复合材料的制备方法及应用 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN110280215B (zh) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113042000A (zh) * | 2021-03-23 | 2021-06-29 | 福州大学 | 一种鸡粪衍生生物炭负载纳米零价铁复合材料及其制备方法和应用 |
CN113457624A (zh) * | 2021-06-18 | 2021-10-01 | 广西大学 | 一种改性菌渣生物炭及其制备方法 |
CN113786803A (zh) * | 2021-08-24 | 2021-12-14 | 福州大学 | 一种具有炭缺陷位结构的生物炭吸附剂及其制备方法与应用 |
US20220126267A1 (en) * | 2019-11-01 | 2022-04-28 | Guangzhou University | Co-pyrolyzed sludge biochar modified by lanthanum carbonate, preparation method and use thereof |
CN115120681A (zh) * | 2022-07-19 | 2022-09-30 | 浙江长三角聚农科技开发有限公司 | 竹笋生物炭在制备治疗糖尿病及其并发症药物中的应用 |
CN116440865A (zh) * | 2023-04-25 | 2023-07-18 | 福州大学 | 一种羟基吡啶酮功能化生物炭材料及其制备方法和应用 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103232035A (zh) * | 2013-03-26 | 2013-08-07 | 赵建树 | 负载纳米银的活性炭及其制备方法 |
CN104874397A (zh) * | 2015-04-02 | 2015-09-02 | 华南理工大学 | 一种二氧化锰载银纳米粒子材料的制备方法和应用 |
CN105289490A (zh) * | 2015-11-12 | 2016-02-03 | 福州大学 | 一种用于吸附分离铼的负载型笋壳吸附剂及其制备方法 |
CN107051385A (zh) * | 2017-05-12 | 2017-08-18 | 福州大学 | 一种载铜笋壳生物炭的制备及其应用 |
-
2019
- 2019-08-09 CN CN201910735896.0A patent/CN110280215B/zh not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103232035A (zh) * | 2013-03-26 | 2013-08-07 | 赵建树 | 负载纳米银的活性炭及其制备方法 |
CN104874397A (zh) * | 2015-04-02 | 2015-09-02 | 华南理工大学 | 一种二氧化锰载银纳米粒子材料的制备方法和应用 |
CN105289490A (zh) * | 2015-11-12 | 2016-02-03 | 福州大学 | 一种用于吸附分离铼的负载型笋壳吸附剂及其制备方法 |
CN107051385A (zh) * | 2017-05-12 | 2017-08-18 | 福州大学 | 一种载铜笋壳生物炭的制备及其应用 |
Non-Patent Citations (1)
Title |
---|
HAISHENG LIN等: "Ligand-Based Modification of the Structures and Optical Properties of New Silver(I)-Rhenate(VII) Oxide/Organic Hybrid Solids", 《HAISHENG LIN等》 * |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20220126267A1 (en) * | 2019-11-01 | 2022-04-28 | Guangzhou University | Co-pyrolyzed sludge biochar modified by lanthanum carbonate, preparation method and use thereof |
CN113042000A (zh) * | 2021-03-23 | 2021-06-29 | 福州大学 | 一种鸡粪衍生生物炭负载纳米零价铁复合材料及其制备方法和应用 |
CN113457624A (zh) * | 2021-06-18 | 2021-10-01 | 广西大学 | 一种改性菌渣生物炭及其制备方法 |
CN113786803A (zh) * | 2021-08-24 | 2021-12-14 | 福州大学 | 一种具有炭缺陷位结构的生物炭吸附剂及其制备方法与应用 |
CN115120681A (zh) * | 2022-07-19 | 2022-09-30 | 浙江长三角聚农科技开发有限公司 | 竹笋生物炭在制备治疗糖尿病及其并发症药物中的应用 |
CN116440865A (zh) * | 2023-04-25 | 2023-07-18 | 福州大学 | 一种羟基吡啶酮功能化生物炭材料及其制备方法和应用 |
Also Published As
Publication number | Publication date |
---|---|
CN110280215B (zh) | 2020-08-11 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN110280215A (zh) | 一种纳米银-笋壳生物炭复合材料的制备方法及应用 | |
CN109482152B (zh) | 基于蛋壳膜模板的金属氧化物复合纳米材料、其制备方法及应用 | |
CN102872803B (zh) | 铝改性秸秆生物质炭及其制备方法和在去除水体中砷的应用 | |
WO2017111092A1 (ja) | 金属選択回収剤、金属回収方法、および、金属溶出方法 | |
CN109012565A (zh) | 一种掺氮的磁性碳材料吸附去除废水中重金属离子的方法 | |
CN105289490B (zh) | 一种用于吸附分离铼的负载型笋壳吸附剂及其制备方法 | |
CN105170108A (zh) | 一种稻壳纤维素吸附剂及其制备方法和应用 | |
CN102580743A (zh) | 一种用金矿尾矿矿渣制备氧化催化剂的方法及制备的氧化催化剂和应用 | |
CN113151667A (zh) | 一种从废led封装中回收稀贵金属元素的方法 | |
CN112371080A (zh) | 一种介孔吸附材料及其制备方法和用途 | |
CN114316993A (zh) | 一种土壤污染修复剂及其修复方法 | |
CN106076248A (zh) | 一种稀土改性粉煤灰的制备方法 | |
CN102899489A (zh) | 一种用固化柿子单宁回收电子垃圾中金的方法 | |
CN104032138A (zh) | 一种堆浸-沉淀稳定化处理含汞尾渣的方法 | |
CN113373307A (zh) | 一种利用磷酸根修饰光催化剂进行光催化溶解金属的方法 | |
CN106166473B (zh) | 一种利用废线路板中非金属分离物制备吸附剂的方法 | |
WO2023221907A1 (zh) | 一种同步脱除溶液中氟、氯、铁的方法 | |
CN110575812B (zh) | 一种陶土/软锰矿高效除磷的环保吸附材料及制备方法 | |
CN111921499A (zh) | 一种球磨改性复合生物炭及其制备方法和应用 | |
CN111455192A (zh) | 一种从低品位含钯难溶废催化剂中回收钯的方法 | |
CN110975811A (zh) | 一种利用高铝粉煤灰制备吸附剂的方法及应用 | |
CN102816921A (zh) | 一种无氯提钒工艺 | |
CN114887587A (zh) | 一种利用锂矿废渣为原料制备的废水中重金属多孔吸附剂及其制备方法 | |
CN104525104A (zh) | 一种利用微波改性硅藻土去除垃圾渗滤液中重金属的方法 | |
CN113926429A (zh) | 一种羟基修饰的二氧化钛复合材料及其制备方法和在回收锗中的应用 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20200811 |
|
CF01 | Termination of patent right due to non-payment of annual fee |