CN110665467A - Preparation method of straw-based adsorbent for adsorbing anions/cations - Google Patents
Preparation method of straw-based adsorbent for adsorbing anions/cations Download PDFInfo
- Publication number
- CN110665467A CN110665467A CN201810714626.7A CN201810714626A CN110665467A CN 110665467 A CN110665467 A CN 110665467A CN 201810714626 A CN201810714626 A CN 201810714626A CN 110665467 A CN110665467 A CN 110665467A
- Authority
- CN
- China
- Prior art keywords
- straw
- powder material
- solution
- based powder
- washed
- 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
- 239000010902 straw Substances 0.000 title claims abstract description 177
- 239000003463 adsorbent Substances 0.000 title claims abstract description 63
- 150000001450 anions Chemical class 0.000 title claims abstract description 28
- 150000001768 cations Chemical class 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 48
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000000843 powder Substances 0.000 claims abstract description 43
- 238000000746 purification Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 44
- 238000003756 stirring Methods 0.000 claims description 28
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims description 15
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 14
- 239000000839 emulsion Substances 0.000 claims description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 10
- 229960000583 acetic acid Drugs 0.000 claims description 10
- 230000007935 neutral effect Effects 0.000 claims description 10
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 10
- PUVAFTRIIUSGLK-UHFFFAOYSA-M trimethyl(oxiran-2-ylmethyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC1CO1 PUVAFTRIIUSGLK-UHFFFAOYSA-M 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 235000021355 Stearic acid Nutrition 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000012362 glacial acetic acid Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 claims description 5
- 239000011654 magnesium acetate Substances 0.000 claims description 5
- 229940069446 magnesium acetate Drugs 0.000 claims description 5
- 235000011285 magnesium acetate Nutrition 0.000 claims description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 5
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 5
- 239000003208 petroleum Substances 0.000 claims description 5
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 5
- 229920006395 saturated elastomer Polymers 0.000 claims description 5
- 238000007711 solidification Methods 0.000 claims description 5
- 230000008023 solidification Effects 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 239000008117 stearic acid Substances 0.000 claims description 5
- 239000008399 tap water Substances 0.000 claims description 5
- 235000020679 tap water Nutrition 0.000 claims description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 51
- 230000000694 effects Effects 0.000 abstract description 5
- 125000000129 anionic group Chemical group 0.000 abstract description 4
- 125000002091 cationic group Chemical group 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000010865 sewage Substances 0.000 abstract description 2
- RQEHWMDDNSYALA-UHFFFAOYSA-N 2-[(oxiran-2-ylmethyltrisulfanyl)methyl]oxirane Chemical compound C1OC1CSSSCC1CO1 RQEHWMDDNSYALA-UHFFFAOYSA-N 0.000 abstract 1
- 238000006640 acetylation reaction Methods 0.000 abstract 1
- NQMRYBIKMRVZLB-UHFFFAOYSA-N methylamine hydrochloride Chemical compound [Cl-].[NH3+]C NQMRYBIKMRVZLB-UHFFFAOYSA-N 0.000 abstract 1
- 241000209094 Oryza Species 0.000 description 18
- 235000007164 Oryza sativa Nutrition 0.000 description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 18
- 235000009566 rice Nutrition 0.000 description 18
- 239000000975 dye Substances 0.000 description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- GCFAQSYBSUQUPL-UHFFFAOYSA-I pentasodium 5-[[4-chloro-6-[3-(2-sulfonatooxyethylsulfonyl)anilino]-1,3,5-triazin-2-yl]amino]-3-[(1,5-disulfonatonaphthalen-2-yl)diazenyl]-4-hydroxynaphthalene-2,7-disulfonate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].Oc1c(N=Nc2ccc3c(cccc3c2S([O-])(=O)=O)S([O-])(=O)=O)c(cc2cc(cc(Nc3nc(Cl)nc(Nc4cccc(c4)S(=O)(=O)CCOS([O-])(=O)=O)n3)c12)S([O-])(=O)=O)S([O-])(=O)=O GCFAQSYBSUQUPL-UHFFFAOYSA-I 0.000 description 9
- 239000004408 titanium dioxide Substances 0.000 description 9
- 230000008859 change Effects 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 239000000706 filtrate Substances 0.000 description 6
- 238000003911 water pollution Methods 0.000 description 5
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 239000002028 Biomass Substances 0.000 description 3
- 238000007385 chemical modification Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 229920005610 lignin Polymers 0.000 description 3
- 239000000985 reactive dye Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229920002488 Hemicellulose Polymers 0.000 description 2
- 239000000980 acid dye Substances 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000000982 direct dye Substances 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- -1 Ca 2+ Chemical class 0.000 description 1
- 235000019750 Crude protein Nutrition 0.000 description 1
- 238000005576 amination reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 239000007764 o/w emulsion Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- 239000002699 waste material Substances 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
-
- 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
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
本发明涉及一种吸附阴/阳离子稻草秸秆基吸附剂的制备方法,属于污水净化处理领域。本发明以稻草秸秆为原料,将稻草秸秆进行提纯,进行乙酰化反应,再制备为稻草秸秆基粉体材料,分别对稻草秸秆基粉体材料接枝二硫化碳和2,3‑环氧丙基三甲基氯化铵,得到含阴/阳离子稻草秸秆基吸附剂。本发明的稻草秸秆基吸附剂可以同时吸附阴/阳离子,并且吸附效果明显,20min可达到吸附平衡,对阳离子镉离子和阴离子酸性染料红1的吸附量分别为79.9mg/g和93.4mg/g。本发明中吸附阴/阳离子的稻草秸秆基吸附剂制备工艺简单,吸附效果明显,成本低廉,具有广泛的应用前景。The invention relates to a preparation method for adsorbing anionic/cationic straw-based adsorbents, belonging to the field of sewage purification treatment. In the invention, the straw is used as the raw material, and the straw is purified, subjected to an acetylation reaction, and then prepared into a straw-based powder material, and carbon disulfide and 2,3-epoxypropyl trisulfide are respectively grafted to the straw-based powder material. Methylammonium chloride to obtain anionic/cationic straw-based adsorbents. The straw-based adsorbent of the present invention can adsorb anions and cations simultaneously, and the adsorption effect is obvious. The adsorption equilibrium can be reached in 20 minutes. . The preparation process of the straw-based adsorbent for adsorbing anions/cations in the present invention is simple, the adsorption effect is obvious, the cost is low, and the adsorbent has wide application prospects.
Description
技术领域technical field
本发明涉及一种吸附阴/阳离子稻草秸秆基吸附剂的制备方法,属于污水净化处理领域。The invention relates to a preparation method for adsorbing anionic/cationic straw-based adsorbents, belonging to the field of sewage purification treatment.
背景技术Background technique
目前,水污染的治理是我们当前面临的一个主要难题。水污染的治理方法很多,吸附剂吸附的方法是其中一种重要方法。受污染的水体中含有很多各种离子,其中,阴离子和阳离子占主要部分。在目前的很多吸附剂中,它们主要针对单一离子的吸附,如单一阴离子,或单一阳离子等。如果能将阴离子和阳离子同时吸附去除,则意义重大,本发明基于此目的,制备了一种吸附阴/阳离子稻草秸秆基吸附剂,此吸附剂可同时吸附水体中的阴离子和阳离子。At present, the treatment of water pollution is a major problem we are currently facing. There are many treatment methods for water pollution, and the method of adsorbent adsorption is one of the important methods. Polluted water contains many kinds of ions, of which anions and cations are the main part. In many current adsorbents, they are mainly aimed at the adsorption of a single ion, such as a single anion, or a single cation. It is of great significance if anions and cations can be adsorbed and removed at the same time. Based on this purpose, the present invention prepares an anion/cationic straw-based adsorbent, which can adsorb anions and cations in water at the same time.
稻草秸秆由于木质素含量低、营养价值低和热值低等原因不适于主要的再利用途径,被大量焚烧或者丢弃,不仅浪费大量生物质能源,也污染了环境。水污染已经严重影响到人类的健康,治理水污染已成为人们亟待解决的问题。如果稻草秸秆能高效应用于水污染的治理,此研究将是有意义的;实际上,生物质资源的高效利用已成为当今科学界的研究热点。稻草秸秆含有大量的纤维素、半纤维素、木质素和少量的粗蛋白、无机盐等,其中,纤维素、半纤维素和木质素含有大量的活性羟基,为其进行化学改性提供了很好的条件,此外,活性羟基也是良好的吸附基团。申请号201110247024.3报道了二氧化硫稻草秸秆吸附剂的制备和使用方法,此发明通过对稻草秸秆溶胀、氧化和胺化改性制备得到,此方法制备的稻草秸秆吸附剂主要用于二氧化硫气体的吸附,对水体中的有害离子尚不能去除。稻草秸秆由于结构的独特性以及资源的普遍性,其作为吸附剂应用于吸附各种水体离子得到广大研究者的兴趣。然而,稻草秸秆基吸附剂由于自身的结构特点,其密度小,在水中不易下沉,经过简单的化学改性后,仍然难改变其在水体上浮的特点;另外,其比表面积小,吸附位点少,吸附量也有待进一步提高,简单的化学改性也难以改变这一现状。针对这些不利因素,本发明拟将稻草秸秆制备为粉体材料的吸附剂,其可以同时吸附水体中的阴/阳离子。Due to the low lignin content, low nutritional value and low calorific value, straw straw is not suitable for the main reuse method, and is incinerated or discarded in large quantities, which not only wastes a large amount of biomass energy, but also pollutes the environment. Water pollution has seriously affected human health, and water pollution control has become an urgent problem to be solved. This research will be meaningful if rice straw can be efficiently applied to the control of water pollution; in fact, the efficient utilization of biomass resources has become a research hotspot in today's scientific community. Rice straw contains a large amount of cellulose, hemicellulose, lignin and a small amount of crude protein, inorganic salts, etc. Among them, cellulose, hemicellulose and lignin contain a large amount of active hydroxyl groups, which provide a good opportunity for their chemical modification. In addition, the active hydroxyl group is also a good adsorption group. Application No. 201110247024.3 reports the preparation and use method of sulfur dioxide straw adsorbent. This invention is prepared by swelling, oxidation and amination modification of straw straw. The straw adsorbent prepared by this method is mainly used for the adsorption of sulfur dioxide gas. Harmful ions in water cannot be removed yet. Due to the unique structure and the universality of resources, straw straw has been widely used as an adsorbent to adsorb various water ions. However, due to its own structural characteristics, straw-based adsorbents have low density and are not easy to sink in water. After simple chemical modification, it is still difficult to change their floating characteristics in water; The adsorption capacity also needs to be further improved, and simple chemical modification is difficult to change this situation. In view of these unfavorable factors, the present invention intends to prepare rice straw as an adsorbent for powder materials, which can simultaneously adsorb anions/cations in a water body.
发明内容SUMMARY OF THE INVENTION
水体中的重金属阳离子和有机染料阴离子对环境的污染日益加剧,为了解决水体的重金属阳离子和有机染料阴离子污染的问题,本发明的目的在于提供一种用于吸附阴/阳离子的稻草秸秆基吸附剂制备方法,所述方法包括如下步骤:The pollution of heavy metal cations and organic dye anions in the water body is increasing day by day. In order to solve the problem of heavy metal cations and organic dye anions pollution in water bodies, the purpose of the present invention is to provide a straw-based adsorbent for adsorbing anions/cations. Preparation method, described method comprises the steps:
(1)稻草秸秆的提纯:将稻草秸秆用自来水多次清洗,将清洗后的稻草秸秆用粉碎机打碎至50-100目数;用0.1mol/L的盐酸溶液和0.5mol/L氢氧化钠溶液先后浸泡1h,用清水清洗至中性;将清洗后的稻草秸秆烘干、备用。(1) Purification of straw straws: Wash straw straws with tap water for several times, crush the washed straw straws to 50-100 mesh with a pulverizer; use 0.1mol/L hydrochloric acid solution and 0.5mol/L hydrogen peroxide The sodium solution was soaked for 1 h successively, and washed with water until neutral; the washed straws were dried and used for later use.
(2)乙酰化稻草秸秆的制备:取5-10g步骤(1)提纯的稻草秸秆在50mL冰醋酸中溶胀2h,然后将其溶于50-100mL乙酸酐和50-100mL乙酸的混合溶液中,向体系中滴加 2-5mL5%的稀硫酸,在50-70℃下反应2h,反应结束后,用1-3g无水醋酸镁中和,然后将上述反应物倒入800-1000mL的蒸馏水中析出乙酰化稻草秸秆,最后将所得乙酰化稻草秸秆离心冲洗至中性,再真空干燥。(2) Preparation of acetylated rice straw: 5-10 g of the purified rice straw in step (1) was swollen in 50 mL of glacial acetic acid for 2 h, and then dissolved in a mixed solution of 50-100 mL of acetic anhydride and 50-100 mL of acetic acid, Add 2-5mL of 5% dilute sulfuric acid dropwise to the system, react at 50-70℃ for 2h, after the reaction, neutralize with 1-3g of anhydrous magnesium acetate, and then pour the above reactant into 800-1000mL of distilled water The acetylated straw straws are separated out, and finally the obtained acetylated straw straws are centrifuged and washed until neutral, and then vacuum dried.
(3)乳液的制备:取步骤(2)制备的3-5g的乙酰化稻草秸秆材料至圆底烧瓶,加入20-40mL石油醚,使其在恒温电磁搅拌器上于38-43℃下持续搅拌并完全溶解。当乙酰化稻草秸秆完全溶解后,将混合溶液加入至盛有2-5mL宁乳32的圆底烧瓶中,搅拌使其混合均匀。将以上混合液缓慢加入50-100mL饱和硬脂酸水溶液中,用磁力转子均匀搅拌,得到水包油(O/W)型乳液。(3) Preparation of emulsion: take 3-5 g of the acetylated straw straw material prepared in step (2) into a round-bottomed flask, add 20-40 mL of petroleum ether, and keep it on a constant temperature electromagnetic stirrer at 38-43° C. Stir and dissolve completely. When the acetylated straw is completely dissolved, add the mixed solution to a round-bottomed flask containing 2-5 mL of Ningru 32, and stir to mix evenly. The above mixed solution is slowly added to 50-100 mL of saturated aqueous stearic acid solution, and uniformly stirred with a magnetic rotor to obtain an oil-in-water (O/W) emulsion.
(4)稻草秸秆基粉体材料的固化:在不断搅拌条件下,将步骤(3)制备的乳液加入到 300-1000mL的乙酸乙酯溶剂中,不断搅拌得到沉淀液。将沉淀液进行离心分离、多次洗涤和低温真空干燥得到稻草秸秆基粉体材料。(4) Solidification of the straw-based powder material: under the condition of constant stirring, the emulsion prepared in step (3) is added to 300-1000 mL of ethyl acetate solvent, and the precipitate is obtained by constant stirring. The precipitation liquid is centrifuged, washed for many times and vacuum-dried at low temperature to obtain a straw-based powder material.
(5)稻草秸秆基粉体材料接枝二硫化碳:在45-60℃中,取步骤(4)制备的3-5g稻草秸秆基粉体材料置于三口烧瓶中,将5-10mLCS2和1-2g碳酸钾溶解在50-100mL四氢呋喃溶液中,将此溶液在1-2h内滴加到装有稻草秸秆基粉体材料的三口烧瓶,滴加完毕后继续搅拌反应2-3h,然后过滤、洗涤和干燥,得到二硫化碳接枝稻草秸秆基粉体材料。(5) Grafting carbon disulfide to the straw-based powder material: at 45-60 °C, take 3-5 g of the straw-based powder material prepared in step (4) into a three-necked flask, and mix 5-10 mL of CS 2 and 1- 2g potassium carbonate was dissolved in 50-100mL tetrahydrofuran solution, and the solution was added dropwise to the three-necked flask containing the straw-based powder material within 1-2h. After the dropwise addition, the stirring reaction was continued for 2-3h, and then filtered and washed. and drying to obtain carbon disulfide grafted straw-based powder material.
(6)稻草秸秆基吸附剂的制备:在55-65℃温度下,取步骤(5)制备的1-2g二硫化碳接枝稻草秸秆基粉体材料置于三口烧瓶中,调控三口烧瓶中水溶液pH值至8-10, 20mL10-15%2,3-环氧丙基三甲基氯化铵(EPC)水溶液在0.5-1h内滴加入装有二硫化碳接枝稻草秸秆基粉体材料三口烧瓶,滴加完毕后继续搅拌反应2-3h,然后过滤、洗涤和干燥,得到用于吸附阴/阳离子的稻草秸秆基吸附剂。(6) Preparation of straw-based adsorbent: at a temperature of 55-65 °C, take 1-2 g of the carbon disulfide-grafted straw-based powder material prepared in step (5) into a three-necked flask, and adjust the pH of the aqueous solution in the three-necked flask. value to 8-10, 20mL of 10-15% 2,3-epoxypropyltrimethylammonium chloride (EPC) aqueous solution was added dropwise to a three-necked flask containing carbon disulfide grafted straw-based powder material within 0.5-1h, dripping After the addition is completed, the stirring reaction is continued for 2-3 hours, followed by filtration, washing and drying to obtain a straw-based adsorbent for adsorbing anions/cations.
本发明上述的用于吸附阴/阳离子的稻草秸秆基吸附剂制备方法涉及的化学反应如下:The chemical reactions involved in the above-mentioned preparation method of the straw-based adsorbent for absorbing anions/cations of the present invention are as follows:
步骤(5)涉及的化学反应:The chemical reaction involved in step (5):
步骤(6)涉及的化学反应:The chemical reaction involved in step (6):
与现有技术相比,本发明具有如下的有益效果:Compared with the prior art, the present invention has the following beneficial effects:
(1)本发明制备的吸附剂是以稻草为主要原料,稻草是一种可再生的生物质资源,价格低廉,对其进行高效利用可以大幅提高其经济价值。(1) The adsorbent prepared by the present invention uses straw as the main raw material, which is a renewable biomass resource with low price, and its economic value can be greatly improved by using it efficiently.
(2)本发明制备的吸附剂可以同时吸附阴/阳离子,并且吸附效果明显,20min可达到吸附平衡,对阳离子镉离子和阴离子酸性染料红1的吸附量分别为79.9mg/g和 93.4mg/g。(2) The adsorbent prepared by the present invention can simultaneously adsorb anions/cations, and the adsorption effect is obvious, and the adsorption equilibrium can be reached in 20 minutes. g.
(3)本发明中吸附阴/阳离子的稻草秸秆基吸附剂的制备工艺简单,吸附效果明显,成本低廉,具有广泛的应用前景。(3) The preparation process of the straw-based adsorbent for adsorbing anions/cations in the present invention is simple, the adsorption effect is obvious, the cost is low, and it has a wide application prospect.
具体实施方式Detailed ways
实施例1:Embodiment 1:
(1)稻草秸秆的提纯:将稻草秸秆用自来水多次清洗,将清洗后的稻草秸秆用粉碎机打碎至50目数;用0.1mol/L的盐酸溶液和0.5mol/L氢氧化钠溶液先后浸泡1h,用清水清洗至中性;将清洗后的稻草秸秆烘干、备用。(1) Purification of rice straw: Wash the rice straw with tap water for many times, and crush the washed rice straw to 50 mesh with a pulverizer; use 0.1 mol/L hydrochloric acid solution and 0.5 mol/L sodium hydroxide solution Soak for 1 hour successively, wash with clean water until neutral; dry the washed straw for later use.
(2)乙酰化稻草秸秆的制备:取5g步骤(1)提纯的稻草秸秆在50mL冰醋酸中溶胀2h,然后将其溶于50mL乙酸酐和50mL乙酸的混合溶液中,向体系中滴加2mL5%的稀硫酸,在58℃下反应2h,反应结束后,用1g无水醋酸镁中和,然后将上述反应物倒入 1000mL的蒸馏水中析出乙酰化稻草秸秆,最后将所得乙酰化稻草秸秆离心冲洗至中性,再真空干燥。(2) Preparation of acetylated rice straw: 5 g of the purified rice straw in step (1) was swollen in 50 mL of glacial acetic acid for 2 hours, then dissolved in a mixed solution of 50 mL of acetic anhydride and 50 mL of acetic acid, and 2 mL of 5 mL was added dropwise to the system. % dilute sulfuric acid was reacted at 58°C for 2 hours. After the reaction was completed, neutralize it with 1 g of anhydrous magnesium acetate, then pour the above reactant into 1000 mL of distilled water to precipitate acetylated straw straws, and finally centrifuge the obtained acetylated straw straws. Rinse until neutral and vacuum dry.
(3)乳液的制备:取步骤(2)制备的3g的乙酰化稻草秸秆材料至圆底烧瓶,加入20mL 石油醚,使其在恒温电磁搅拌器上于39℃下持续搅拌并完全溶解。当乙酰化稻草秸秆完全溶解后,将混合溶液加入至盛有2mL宁乳32的圆底烧瓶中,搅拌使其混合均匀。将以上混合液缓慢加入50mL饱和硬脂酸水溶液中,用磁力转子均匀搅拌,得到O/W型乳液。(3) Preparation of emulsion: take 3 g of acetylated straw material prepared in step (2) into a round-bottomed flask, add 20 mL of petroleum ether, and keep stirring at 39°C on a constant-temperature electromagnetic stirrer to dissolve completely. When the acetylated straw is completely dissolved, add the mixed solution to a round-bottomed flask containing 2 mL of Ningru 32, and stir to mix evenly. The above mixed solution was slowly added to 50 mL of saturated aqueous stearic acid solution, and stirred uniformly with a magnetic rotor to obtain an O/W emulsion.
(4)稻草秸秆基粉体材料的固化:在不断搅拌条件下,将步骤(3)制备的乳液加入到 800mL的乙酸乙酯溶剂中,不断搅拌得到沉淀液。将沉淀液进行离心分离、多次洗涤和低温真空干燥得到稻草秸秆基粉体材料。(4) Solidification of the straw-based powder material: under the condition of constant stirring, the emulsion prepared in step (3) was added to 800 mL of ethyl acetate solvent, and the precipitate was obtained by constant stirring. The precipitation liquid is centrifuged, washed for many times and vacuum-dried at low temperature to obtain a straw-based powder material.
(5)稻草秸秆基粉体材料接枝二硫化碳:在50℃中,取步骤(4)制备的3g稻草秸秆基粉体材料置于三口烧瓶中,将5mLCS2和1g碳酸钾溶解在100mL四氢呋喃溶液中,将此溶液在1-2h内滴加到装有稻草秸秆基粉体材料的三口烧瓶,滴加完毕后继续搅拌反应2-3h,然后过滤、洗涤和干燥得到二硫化碳接枝稻草秸秆基粉体材料。(5) Grafting carbon disulfide to the straw-based powder material: at 50°C, take 3 g of the straw-based powder material prepared in step (4) and place it in a three-necked flask, and dissolve 5 mL of CS 2 and 1 g of potassium carbonate in 100 mL of tetrahydrofuran solution , the solution was added dropwise to the three-necked flask containing the straw-based powder material within 1-2 hours, and the stirring reaction was continued for 2-3 hours after the dropwise addition, and then filtered, washed and dried to obtain carbon disulfide-grafted straw-based powder. body material.
(6)稻草秸秆基吸附剂的制备:在60℃温度下,取步骤(5)制备的2g二硫化碳接枝稻草秸秆基粉体材料置于三口烧瓶中,调控三口烧瓶中水溶液pH值至8-10,20mL10%2, 3-环氧丙基三甲基氯化铵(EPC)水溶液在0.5-1h内滴加入装有二硫化碳接枝稻草秸秆基粉体材料三口烧瓶,滴加完毕后继续搅拌反应2-3h,然后过滤、洗涤和干燥得到用于吸附阴/阳离子的稻草秸秆基吸附剂I。(6) Preparation of straw-based adsorbent: at a temperature of 60 °C, take 2 g of the carbon disulfide-grafted straw-based powder material prepared in step (5) into a three-necked flask, and adjust the pH of the aqueous solution in the three-necked flask to 8- 10,20mL of 10% 2,3-epoxypropyltrimethylammonium chloride (EPC) aqueous solution was added dropwise to a three-necked flask containing carbon disulfide grafted straw-based powder material within 0.5-1h, and the stirring reaction was continued after the dropwise addition was completed. 2-3h, then filtered, washed and dried to obtain a straw-based adsorbent I for adsorbing anions/cations.
实施例2:Embodiment 2:
(1)稻草秸秆的提纯:将稻草秸秆用自来水多次清洗,将清洗后的稻草秸秆用粉碎机打碎至50目数;用0.1mol/L的盐酸溶液和0.5mol/L氢氧化钠溶液先后浸泡1h,用清水清洗至中性;将清洗后的稻草秸秆烘干、备用。(1) Purification of rice straw: Wash the rice straw with tap water for many times, and crush the washed rice straw to 50 mesh with a pulverizer; use 0.1 mol/L hydrochloric acid solution and 0.5 mol/L sodium hydroxide solution Soak for 1 hour successively, wash with clean water until neutral; dry the washed straw for later use.
(2)乙酰化稻草秸秆的制备:取10g步骤(1)提纯的稻草秸秆在50mL冰醋酸中溶胀2h,然后将其溶于100mL乙酸酐和100mL乙酸的混合溶液中,向体系中滴加5mL5%的稀硫酸,在61℃下反应2h,反应结束后,用2g无水醋酸镁中和,然后将上述反应物倒入1000mL的蒸馏水中析出乙酰化稻草秸秆,最后将所得乙酰化稻草秸秆离心冲洗至中性,再真空干燥。(2) Preparation of acetylated rice straw: 10 g of the purified rice straw in step (1) was swollen in 50 mL of glacial acetic acid for 2 hours, then dissolved in a mixed solution of 100 mL of acetic anhydride and 100 mL of acetic acid, and 5 mL of 5 mL was added dropwise to the system. % dilute sulfuric acid was reacted at 61 °C for 2 hours. After the reaction, neutralize with 2 g of anhydrous magnesium acetate, and then pour the above reactant into 1000 mL of distilled water to precipitate acetylated straw straws. Finally, the obtained acetylated straw straws were centrifuged. Rinse until neutral and vacuum dry.
(3)乳液的制备:取步骤(2)制备的4g的乙酰化稻草秸秆材料至圆底烧瓶,加入25mL 石油醚,使其在恒温电磁搅拌器上于40℃下持续搅拌并完全溶解。当乙酰化稻草秸秆完全溶解后,将混合溶液加入至盛有2.5mL宁乳32的圆底烧瓶中,搅拌使其混合均匀。将以上混合液缓慢加入80mL饱和硬脂酸水溶液中,用磁力转子均匀搅拌,得到O/W型乳液。(3) Preparation of emulsion: Take 4 g of the acetylated straw material prepared in step (2) into a round-bottomed flask, add 25 mL of petroleum ether, keep stirring at 40°C on a constant temperature electromagnetic stirrer and dissolve completely. When the acetylated straw is completely dissolved, add the mixed solution to a round-bottomed flask containing 2.5 mL of Ningru 32, and stir to mix it evenly. The above mixed solution was slowly added to 80 mL of saturated aqueous stearic acid solution, and stirred uniformly with a magnetic rotor to obtain an O/W emulsion.
(4)稻草秸秆基粉体材料的固化:在不断搅拌条件下,将步骤(3)制备的乳液加入到 1000mL的乙酸乙酯溶剂中,不断搅拌得到沉淀液。将沉淀液进行离心分离、多次洗涤和低温真空干燥得到稻草秸秆基粉体材料。(4) Solidification of the straw-based powder material: under the condition of constant stirring, the emulsion prepared in step (3) was added to 1000 mL of ethyl acetate solvent, and the precipitate was obtained by constant stirring. The precipitation liquid is centrifuged, washed for many times and vacuum-dried at low temperature to obtain a straw-based powder material.
(5)稻草秸秆基粉体材料接枝二硫化碳:在52℃中,取步骤(4)制备的3g稻草秸秆基粉体材料置于三口烧瓶中,将5mLCS2和1.5g碳酸钾溶解在80mL四氢呋喃溶液中,将此溶液在1-2h内滴加到装有稻草秸秆基粉体材料的三口烧瓶,滴加完毕后继续搅拌反应2-3h,然后过滤、洗涤和干燥得到二硫化碳接枝稻草秸秆基粉体材料。(5) Grafting carbon disulfide to the straw-based powder material: at 52°C, take 3 g of the straw-based powder material prepared in step (4) and place it in a three-necked flask, and dissolve 5 mL of CS 2 and 1.5 g of potassium carbonate in 80 mL of tetrahydrofuran. In the solution, the solution is added dropwise to a three-necked flask containing the powder material of straw-based straw within 1-2 hours, and the stirring reaction is continued for 2-3 hours after the dropwise addition, and then filtered, washed and dried to obtain the carbon disulfide grafted straw-based straw. powder material.
(6)稻草秸秆基吸附剂的制备:在61℃温度下,取步骤(5)制备的2.5g二硫化碳接枝稻草秸秆基粉体材料置于三口烧瓶中,调控三口烧瓶中水溶液pH值至8-10, 20mL15%2,3-环氧丙基三甲基氯化铵(EPC)水溶液在0.5-1h内滴加入装有二硫化碳接枝稻草秸秆基粉体材料三口烧瓶,滴加完毕后继续搅拌反应2-3h,然后过滤、洗涤和干燥,得到用于吸附阴/阳离子的稻草秸秆基吸附剂II。(6) Preparation of straw-based adsorbent: at a temperature of 61°C, take 2.5 g of the carbon disulfide-grafted straw-based powder material prepared in step (5) into a three-necked flask, and adjust the pH value of the aqueous solution in the three-necked flask to 8 -10, 20mL of 15% 2,3-epoxypropyltrimethylammonium chloride (EPC) aqueous solution was added dropwise to a three-necked flask containing carbon disulfide grafted straw-based powder material within 0.5-1h, and continued stirring after the dropwise addition was completed The reaction was carried out for 2-3 h, followed by filtration, washing and drying to obtain a straw-straw-based adsorbent II for adsorbing anions/cations.
实施例3:Embodiment 3:
(1)稻草秸秆的提纯:将稻草秸秆用自来水多次清洗,将清洗后的稻草秸秆用粉碎机打碎至100目数;用0.1mol/L的盐酸溶液和0.5mol/L氢氧化钠溶液先后浸泡1h,用清水清洗至中性;将清洗后的稻草秸秆烘干、备用。(1) Purification of straw: Wash the straw with tap water for several times, and crush the washed straw to 100 mesh with a pulverizer; use 0.1 mol/L hydrochloric acid solution and 0.5 mol/L sodium hydroxide solution Soak for 1 hour successively, wash with clean water until neutral; dry the washed straw for later use.
(2)乙酰化稻草秸秆的制备:取8g步骤(1)提纯的稻草秸秆在50mL冰醋酸中溶胀2h,然后将其溶于80mL乙酸酐和80mL乙酸的混合溶液中,向体系中滴加4mL5%的稀硫酸,在60℃下反应2h,反应结束后,用3g无水醋酸镁中和,然后将上述反应物倒入 1000mL的蒸馏水中析出乙酰化稻草秸秆,最后将所得乙酰化稻草秸秆离心冲洗至中性,再真空干燥。(2) Preparation of acetylated rice straw: 8 g of the purified rice straw in step (1) was swollen in 50 mL of glacial acetic acid for 2 hours, then dissolved in a mixed solution of 80 mL of acetic anhydride and 80 mL of acetic acid, and 4 mL of 5 mL was added dropwise to the system. % dilute sulfuric acid was reacted at 60 °C for 2 hours. After the reaction was completed, neutralize with 3 g of anhydrous magnesium acetate, then pour the above reactant into 1000 mL of distilled water to precipitate acetylated straw straws, and finally centrifuge the obtained acetylated straw straws. Rinse until neutral and vacuum dry.
(3)乳液的制备:取步骤(2)制备的5g的乙酰化稻草秸秆材料至圆底烧瓶,加入40mL 石油醚,使其在恒温电磁搅拌器上于40℃下持续搅拌并完全溶解。当乙酰化稻草秸秆完全溶解后,将混合溶液加入至盛有5mL宁乳32的圆底烧瓶中,搅拌使其混合均匀。将以上混合液缓慢加入100mL饱和硬脂酸水溶液中,用磁力转子均匀搅拌,得到O/W型乳液。(3) Preparation of emulsion: Take 5 g of acetylated straw material prepared in step (2) into a round-bottomed flask, add 40 mL of petroleum ether, and keep stirring at 40°C on a constant-temperature electromagnetic stirrer to dissolve completely. When the acetylated straw is completely dissolved, add the mixed solution to a round-bottomed flask containing 5 mL of Ningru 32, and stir to mix evenly. The above mixed solution was slowly added to 100 mL of saturated aqueous stearic acid solution, and uniformly stirred with a magnetic rotor to obtain an O/W emulsion.
(4)稻草秸秆基粉体材料的固化:在不断搅拌条件下,将步骤(3)制备的乳液加入到 900mL的乙酸乙酯溶剂中,不断搅拌得到沉淀液。将沉淀液进行离心分离、多次洗涤和低温真空干燥得到稻草秸秆基粉体材料。(4) Solidification of the straw-based powder material: under the condition of constant stirring, the emulsion prepared in step (3) was added to 900 mL of ethyl acetate solvent, and the precipitate was obtained by constant stirring. The precipitation liquid is centrifuged, washed for many times and vacuum-dried at low temperature to obtain a straw-based powder material.
(5)稻草秸秆基粉体材料接枝二硫化碳:在52℃中,取步骤(4)制备的4.5g稻草秸秆基粉体材料置于三口烧瓶中,将10mLCS2和2g碳酸钾溶解在100mL四氢呋喃溶液中,将此溶液在1-2h内滴加到装有稻草秸秆基粉体材料的三口烧瓶,滴加完毕后继续搅拌反应2-3h,然后过滤、洗涤和干燥,得到二硫化碳接枝稻草秸秆基粉体材料。(5) Grafting carbon disulfide from the straw-based powder material: at 52° C., take 4.5 g of the straw-based powder material prepared in step (4) and place it in a three-necked flask, and dissolve 10 mL of CS 2 and 2 g of potassium carbonate in 100 mL of tetrahydrofuran. In the solution, the solution is added dropwise to the three-necked flask containing the straw-based powder material within 1-2 hours. After the dropwise addition, the stirring reaction is continued for 2-3 hours, and then filtered, washed and dried to obtain carbon disulfide grafted rice straw. base powder material.
(6)稻草秸秆基吸附剂的制备:在61℃温度下,取步骤(5)制备的2g二硫化碳接枝稻草秸秆基粉体材料置于三口烧瓶中,调控三口烧瓶中水溶液pH值至8-10,20mL10%2, 3-环氧丙基三甲基氯化铵(EPC)水溶液在0.5-1h内滴加入装有二硫化碳接枝稻草秸秆基粉体材料三口烧瓶,滴加完毕后继续搅拌反应2-3h,然后过滤、洗涤和干燥,得到用于吸附阴/阳离子的稻草秸秆基吸附剂III。(6) Preparation of straw-based adsorbent: at a temperature of 61 °C, take 2 g of the carbon disulfide-grafted straw-based powder material prepared in step (5) into a three-necked flask, and adjust the pH of the aqueous solution in the three-necked flask to 8- 10,20mL of 10% 2,3-epoxypropyltrimethylammonium chloride (EPC) aqueous solution was added dropwise to a three-necked flask containing carbon disulfide grafted straw-based powder material within 0.5-1h, and the stirring reaction was continued after the dropwise addition was completed. 2-3h, then filtered, washed and dried to obtain a straw-straw-based adsorbent III for adsorbing anions/cations.
对本发明制备的用于吸附阴/阳离子的稻草秸秆基吸附剂I,II,III进行吸附性能测试:The adsorption performance tests are carried out on the straw-based adsorbents I, II and III prepared by the present invention for adsorbing anions/cations:
a.吸附浓度对吸附性能的影响测试a. Influence test of adsorption concentration on adsorption performance
配制质量浓度分别为20、40、100、200、300、400、600mg/L的活性红195溶液,每个浓度分别称取50mL,溶液的pH标定为7,然后分别加入0.1g的稻草秸秆基吸附剂I,在20℃条件下恒温震荡2h,然后过滤,取滤液测定吸附前后溶液中活性红195浓度变化。采用相同的操作方法,将吸附剂换成稻草秸秆基吸附剂II,III,活性炭和二氧化钛,分别进行测定,得到吸附量如表1所示。Reactive red 195 solutions with mass concentrations of 20, 40, 100, 200, 300, 400, and 600 mg/L were prepared, 50 mL of each concentration was weighed, and the pH of the solution was calibrated to 7, and then 0.1 g of straw-based The adsorbent I was shaken at a constant temperature of 20°C for 2 hours, then filtered, and the filtrate was taken to measure the concentration change of reactive red 195 in the solution before and after adsorption. Using the same operation method, the adsorbents were replaced with straw-based adsorbents II, III, activated carbon and titanium dioxide, respectively, and the adsorption amounts were obtained as shown in Table 1.
表1稻草秸秆基吸附剂I,II,III在不同吸附浓度下的吸附性能Table 1 Adsorption performance of straw-based adsorbents I, II, III at different adsorption concentrations
从表1中可以看出,在相同的染料浓度下,稻草秸秆基吸附剂I,II,III对活性染料活性红195的吸附量明显高于活性炭和二氧化钛。It can be seen from Table 1 that under the same dye concentration, the adsorption capacity of the straw-based adsorbents I, II and III on the reactive dye reactive red 195 is significantly higher than that of activated carbon and titanium dioxide.
b.吸附温度对吸附性能的影响测试b. Influence test of adsorption temperature on adsorption performance
配制质量浓度为300mg/L的活性红195溶液,每个浓度分别称取50mL,溶液的pH 标定为7,然后分别加入0.1g的稻草秸秆基吸附剂I,分别在10℃、20℃、30℃、40℃、50℃条件下恒温震荡2h,然后过滤,取滤液测定吸附前后溶液中活性红195浓度变化。采用相同的操作方法,将吸附剂换成稻草秸秆基吸附剂II,III,活性炭和二氧化钛,分别进行测定,得到吸附量如表2所示。A reactive red 195 solution with a mass concentration of 300 mg/L was prepared, 50 mL of each concentration was weighed, and the pH of the solution was calibrated to 7, and then 0.1 g of straw-based adsorbent I was added, respectively, at 10 °C, 20 °C, and 30 °C. Under the conditions of ℃, 40 ℃ and 50 ℃, it was shaken at constant temperature for 2 hours, and then filtered, and the filtrate was taken to measure the concentration change of reactive red 195 in the solution before and after adsorption. Using the same operation method, the adsorbents were replaced with straw-based adsorbents II, III, activated carbon and titanium dioxide, respectively, and the adsorption amount was obtained as shown in Table 2.
表2稻草秸秆基吸附剂I,II,III在不同温度下的吸附性能Table 2 Adsorption performance of straw-based adsorbents I, II, III at different temperatures
从表2中可以看出,在相同的温度下,稻草秸秆基吸附剂I,II,III对活性染料活性红195的吸附量明显高于活性炭和二氧化钛。此外,随着温度的增加,稻草秸秆基吸附剂I,II,III的吸附量略有增加。It can be seen from Table 2 that at the same temperature, the adsorption capacity of the straw-based adsorbents I, II, and III on the reactive dye reactive red 195 is significantly higher than that of activated carbon and titanium dioxide. In addition, the adsorption capacity of the straw-based adsorbents I, II, III increased slightly with the increase of temperature.
c.吸附时间对吸附性能的影响测试c. Test of the effect of adsorption time on adsorption performance
配制质量浓度为300mg/L的活性红195溶液,每个浓度分别称取50mL,溶液的pH 标定为7,然后分别加入0.1g的稻草秸秆基吸附剂I,在20℃条件下恒温分别震荡10min、20min、30min、40min、50min,然后过滤,取滤液测定吸附前后溶液中活性红195 浓度变化。采用相同的操作方法,将吸附剂换成稻草秸秆基吸附剂II,III,活性炭和二氧化钛,分别进行测定,得到吸附量如表3所示。A reactive red 195 solution with a mass concentration of 300 mg/L was prepared, 50 mL of each concentration was weighed, and the pH of the solution was calibrated to 7, and then 0.1 g of straw-based adsorbent I was added respectively, and the constant temperature was shaken for 10 min at 20 °C. , 20min, 30min, 40min, 50min, and then filtered, and the filtrate was taken to measure the concentration change of reactive red 195 in the solution before and after adsorption. Using the same operation method, the adsorbents were replaced by straw-based adsorbents II, III, activated carbon and titanium dioxide, respectively, and the adsorption amounts were obtained as shown in Table 3.
表3稻草秸秆基吸附剂I,II,III经过不同吸附时间后的吸附性能Table 3 Adsorption properties of straw-based adsorbents I, II, III after different adsorption times
从表3中可以看出,稻草秸秆基吸附剂I,II,III的吸附时间在20min时达到平衡,而活性炭和二氧化钛的吸附平衡时间为30min,说明稻草秸秆基吸附剂I,II,III可以在较短的时间内实现染料的吸附。It can be seen from Table 3 that the adsorption time of the straw-based adsorbents I, II, and III reached equilibrium at 20 min, while the adsorption equilibrium time of activated carbon and titanium dioxide was 30 min, indicating that the straw-based adsorbents I, II, and III could The dye adsorption is achieved in a short time.
d.对不同种类含阴离子的有机染料的吸附性能测试d. Adsorption performance test for different kinds of organic dyes containing anions
配制质量浓度为300mg/L的各种不同染料溶液,每个浓度分别称取50mL,溶液的pH标定为7,然后分别加入0.1g的稻草秸秆基吸附剂I,在20℃条件下恒温震荡2h,然后过滤,取滤液测定吸附前后溶液中染料浓度变化。采用相同的操作方法,将稻草秸秆基吸附剂I换成稻草秸秆基吸附剂II,III,活性炭和二氧化钛,分别进行测定,得到吸附量如表4所示。Various dye solutions with a mass concentration of 300 mg/L were prepared, 50 mL of each concentration was weighed, and the pH of the solution was calibrated to 7. Then 0.1 g of straw-based adsorbent I was added, and the solution was shaken at a constant temperature of 20 °C for 2 hours. , and then filtered, and the filtrate was taken to measure the change of dye concentration in the solution before and after adsorption. Using the same operation method, the straw-based adsorbent I was replaced by the straw-based adsorbent II, III, activated carbon and titanium dioxide, respectively, and the adsorption capacity was obtained as shown in Table 4.
表4稻草秸秆基吸附剂I,II,III对不同种类含阴离子的有机染料的吸附性能Table 4 Adsorption properties of straw-based adsorbents I, II, III for different kinds of anion-containing organic dyes
从表4中可以看出,对于不同种类含阴离子的有机染料,如:活性染料活性红195、直接染料湖蓝71、直接染料红4BS、酸性染料蓝80、酸性染料红1,稻草秸秆基吸附剂 I,II,III均具有很强的吸附性能。As can be seen from Table 4, for different kinds of organic dyes containing anions, such as: reactive dye reactive red 195, direct dye lake blue 71, direct dye red 4BS, acid dye blue 80, acid dye red 1, straw-based adsorption Agents I, II, and III all have strong adsorption properties.
e.对不同种类金属阳离子的吸附性能测试e. Adsorption performance test for different kinds of metal cations
配制质量浓度为300mg/L的各种不同染料溶液,每个浓度分别称取50mL,溶液的pH标定为7,然后分别加入0.1g的稻草秸秆基吸附剂I,在20℃条件下恒温震荡2h,然后过滤,取滤液测定吸附前后溶液中染料浓度变化。采用相同的操作方法,将稻草秸秆基吸附剂I换成稻草秸秆基吸附剂II,III,活性炭和二氧化钛,分别进行测定,得到吸附量如表5所示。Various dye solutions with a mass concentration of 300 mg/L were prepared, 50 mL of each concentration was weighed, and the pH of the solution was calibrated to 7. Then 0.1 g of straw-based adsorbent I was added, and the solution was shaken at a constant temperature of 20 °C for 2 hours. , and then filtered, and the filtrate was taken to measure the change of dye concentration in the solution before and after adsorption. Using the same operation method, the straw-based adsorbent I was replaced by the straw-based adsorbent II, III, activated carbon and titanium dioxide, respectively, and the adsorption capacity was obtained as shown in Table 5.
表5稻草秸秆基吸附剂I,II,III对不同种类的金属阳离子的吸附性能Table 5 Adsorption properties of straw-based adsorbents I, II, III for different kinds of metal cations
从表5中可以看出,对于不同种类的金属阳离子,如:Ca2+、Zn2+、Cu2+、Cd2+、 Hg2+,稻草秸秆基吸附剂I,II,III均具有很强的吸附性能。It can be seen from Table 5 that for different kinds of metal cations, such as Ca 2+ , Zn 2+ , Cu 2+ , Cd 2+ , Hg 2+ , the straw-based adsorbents I, II, and III all have very good properties. Strong adsorption properties.
f.对同时含有金属阳离子和含阴离子有机染料水溶液的吸附性能测试f. Adsorption performance test for aqueous solution containing both metal cations and anion-containing organic dyes
配制质量浓度为300mg/L的金属阳离子和300mg/L含阴离子有机染料的混合水溶液,每个浓度分别称取50mL,溶液的pH标定为7,然后分别加入0.1g的稻草秸秆基吸附剂I,在20℃条件下恒温震荡2h,然后过滤,取滤液测定吸附前后溶液中染料浓度变化。采用相同的操作方法,将吸附剂换成稻草秸秆基吸附剂II,III,活性炭和二氧化钛,分别进行测定,得到吸附量如表6所示。Prepare a mixed aqueous solution with a mass concentration of 300 mg/L of metal cations and 300 mg/L of anionic organic dyes, weigh 50 mL of each concentration, and the pH of the solution is calibrated to 7, and then add 0.1 g of straw-based adsorbent I, respectively, Under the condition of 20 ℃, constant temperature shaking for 2h, then filtration, the filtrate was taken to measure the change of dye concentration in the solution before and after adsorption. Using the same operation method, the adsorbents were replaced with straw-based adsorbents II, III, activated carbon and titanium dioxide, respectively, and the adsorption amount was obtained as shown in Table 6.
表6稻草秸秆基吸附剂I,II,III对同时含有金属阳离子和含阴离子有机染料水溶液的吸附性能Table 6 Adsorption properties of straw-based adsorbents I, II, and III on aqueous solutions containing both metal cations and anions containing organic dyes
从表6中可以看出,对于同时含有金属阳离子和含阴离子有机染料水溶液,稻草秸秆基吸附剂I,II,III均具有很强的吸附性能。It can be seen from Table 6 that the straw-based adsorbents I, II, and III all have strong adsorption performance for aqueous solutions containing both metal cations and anion-containing organic dyes.
最后需要说明,上述描述仅为本发明的优选实施例,本领域的技术人员在本发明的启示下,在不违背本发明宗旨及权利要求的前提下,可以做出多种类似的表示,这样的变换均落入本发明的保护范围之内。Finally, it should be noted that the above description is only a preferred embodiment of the present invention. Under the inspiration of the present invention, those skilled in the art can make a variety of similar expressions under the premise of not violating the purpose and claims of the present invention. The transformations fall within the protection scope of the present invention.
Claims (1)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810714626.7A CN110665467A (en) | 2018-07-03 | 2018-07-03 | Preparation method of straw-based adsorbent for adsorbing anions/cations |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810714626.7A CN110665467A (en) | 2018-07-03 | 2018-07-03 | Preparation method of straw-based adsorbent for adsorbing anions/cations |
Publications (1)
Publication Number | Publication Date |
---|---|
CN110665467A true CN110665467A (en) | 2020-01-10 |
Family
ID=69065538
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201810714626.7A Pending CN110665467A (en) | 2018-07-03 | 2018-07-03 | Preparation method of straw-based adsorbent for adsorbing anions/cations |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN110665467A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111389378A (en) * | 2020-03-27 | 2020-07-10 | 重庆大学 | A kind of amphoteric self-floating adsorbent, preparation method and application |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102626608A (en) * | 2012-04-16 | 2012-08-08 | 南京大学 | Straw modified into amphiprotic adsorbent and preparation method thereof |
CN105776481A (en) * | 2016-03-16 | 2016-07-20 | 江阴职业技术学院 | Xanthate cation dual-modified straw fiber printing and dyeing wastewater treatment agent and preparation method thereof |
CN106824111A (en) * | 2017-02-27 | 2017-06-13 | 湖南云平环保科技有限公司 | The method that stalk prepares heavy metal chelant |
CN107213875A (en) * | 2017-06-21 | 2017-09-29 | 武汉纺织大学 | A kind of modified ramie porous microsphere sorbent of Adsorption of Heavy Metals ion and preparation method and application |
CN107552012A (en) * | 2017-10-24 | 2018-01-09 | 武汉纺织大学 | Composite nanometer particle adsorbent of adsorpting anion organic dyestuff and preparation method thereof |
CN107626284A (en) * | 2016-09-13 | 2018-01-26 | 塔里木大学 | The method that cotton stalk adsorbent is prepared using carbon disulfide modification |
-
2018
- 2018-07-03 CN CN201810714626.7A patent/CN110665467A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102626608A (en) * | 2012-04-16 | 2012-08-08 | 南京大学 | Straw modified into amphiprotic adsorbent and preparation method thereof |
CN105776481A (en) * | 2016-03-16 | 2016-07-20 | 江阴职业技术学院 | Xanthate cation dual-modified straw fiber printing and dyeing wastewater treatment agent and preparation method thereof |
CN107626284A (en) * | 2016-09-13 | 2018-01-26 | 塔里木大学 | The method that cotton stalk adsorbent is prepared using carbon disulfide modification |
CN106824111A (en) * | 2017-02-27 | 2017-06-13 | 湖南云平环保科技有限公司 | The method that stalk prepares heavy metal chelant |
CN107213875A (en) * | 2017-06-21 | 2017-09-29 | 武汉纺织大学 | A kind of modified ramie porous microsphere sorbent of Adsorption of Heavy Metals ion and preparation method and application |
CN107552012A (en) * | 2017-10-24 | 2018-01-09 | 武汉纺织大学 | Composite nanometer particle adsorbent of adsorpting anion organic dyestuff and preparation method thereof |
Non-Patent Citations (1)
Title |
---|
ERMENG LV ET AL.: "Preparation of an Efficient Oil-Spill Adsorbent Based on Wheat Straw", 《BIORESOURCES》 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111389378A (en) * | 2020-03-27 | 2020-07-10 | 重庆大学 | A kind of amphoteric self-floating adsorbent, preparation method and application |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN103127914B (en) | Magnetic chitosan microsphere treatment agent and preparation method thereof | |
CN108325506B (en) | A kind of preparation method of modified cellulose aerogel adsorbing heavy metals | |
CN104387617B (en) | A kind of preparation method of corn stalk modified cellulose gel | |
CN104475023B (en) | A kind of preparation method of modified konjac glucomannan carbosphere heavy-metal adsorption material | |
CN103464117B (en) | Preparation method of ethanediamine based porous dextrangel adsorbent | |
CN108905995A (en) | A kind of preparation method and its application method of magnetic response amination cellulose base heavy-metal adsorption material | |
CN108295820A (en) | A kind of preparation method and applications of plant fiber adsorbing material | |
CN103464119A (en) | Preparation method and application of modified cysteine palm bark adsorbent | |
CN106964321B (en) | A kind of preparation method and applications of banana fiber chitosan composite hydrogel | |
CN106390949A (en) | Preparation method of chitosan/nanometer oxycellulose/nanometer quaternary ammonium salt cellulose ether blended membrane | |
CN111229179A (en) | Lignin-based anionic dye adsorbent and preparation method and application thereof | |
CN111229167A (en) | Thiosemicarbazide modified magnetic graphene oxide adsorbent and preparation method and application thereof | |
CN106362712A (en) | Rice husk base ion-exchange adsorption material, preparation method thereof and application | |
CN110665467A (en) | Preparation method of straw-based adsorbent for adsorbing anions/cations | |
CN111167417A (en) | A kind of modified bagasse and its preparation method and application as adsorbent | |
CN110302837A (en) | A cellulose-based catalytic membrane for advanced oxidation process treatment of dye wastewater and its preparation method | |
CN110711560A (en) | Preparation method of biomass adsorbent for printing and dyeing wastewater treatment | |
CN101264436A (en) | Application of loofah as adsorbent in the adsorption of metal ions | |
CN102921359A (en) | Preparation method of biological capsule for sewage treatment | |
CN103127917B (en) | Preparation method of drinking water treatment agent | |
CN106378102A (en) | Carboxymethylated paper pulp fiber heavy-metal adsorbing material, and preparation method and application thereof | |
CN108404874A (en) | A kind of plant fiber/LDHs sorbing materials and preparation method and application | |
JP7486222B2 (en) | Method for producing Cu2O composite amidoxime group adsorbent and its application | |
CN106362705A (en) | Carboxymethyl cationic dye adsorption material prepared from paper pulp fiber, preparation method and application | |
CN117696033A (en) | Aluminum cluster/cellulose composite adsorption material for adsorbing organic pollutants in water |
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 | ||
WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20200110 |
|
WD01 | Invention patent application deemed withdrawn after publication |