CN115403101A - Dyeing and printing industrial sewage treatment agent and preparation method thereof - Google Patents
Dyeing and printing industrial sewage treatment agent and preparation method thereof Download PDFInfo
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- CN115403101A CN115403101A CN202211352595.8A CN202211352595A CN115403101A CN 115403101 A CN115403101 A CN 115403101A CN 202211352595 A CN202211352595 A CN 202211352595A CN 115403101 A CN115403101 A CN 115403101A
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- Prior art keywords
- deionized water
- industrial sewage
- loofah sponge
- printing
- dyeing
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- 239000010865 sewage Substances 0.000 title claims abstract description 46
- 238000004043 dyeing Methods 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 244000280244 Luffa acutangula Species 0.000 claims abstract description 54
- 235000009814 Luffa aegyptiaca Nutrition 0.000 claims abstract description 54
- 239000000835 fiber Substances 0.000 claims abstract description 53
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 33
- 239000003463 adsorbent Substances 0.000 claims abstract description 30
- 239000002131 composite material Substances 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 239000004113 Sepiolite Substances 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 18
- 235000019355 sepiolite Nutrition 0.000 claims abstract description 18
- 229910052624 sepiolite Inorganic materials 0.000 claims abstract description 18
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 14
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims abstract description 14
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 8
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 52
- 239000008367 deionised water Substances 0.000 claims description 51
- 229910021641 deionized water Inorganic materials 0.000 claims description 51
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 45
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 42
- 238000003756 stirring Methods 0.000 claims description 40
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 229920001661 Chitosan Polymers 0.000 claims description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000007864 aqueous solution Substances 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 20
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 14
- 235000006408 oxalic acid Nutrition 0.000 claims description 14
- LTVDFSLWFKLJDQ-UHFFFAOYSA-N α-tocopherolquinone Chemical compound CC(C)CCCC(C)CCCC(C)CCCC(C)(O)CCC1=C(C)C(=O)C(C)=C(C)C1=O LTVDFSLWFKLJDQ-UHFFFAOYSA-N 0.000 claims description 14
- 239000002612 dispersion medium Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- 239000004202 carbamide Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 10
- 239000012065 filter cake Substances 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- NDEMNVPZDAFUKN-UHFFFAOYSA-N guanidine;nitric acid Chemical compound NC(N)=N.O[N+]([O-])=O.O[N+]([O-])=O NDEMNVPZDAFUKN-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 10
- 229920002401 polyacrylamide Polymers 0.000 claims description 10
- 239000001509 sodium citrate Substances 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 10
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 10
- 229940038773 trisodium citrate Drugs 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 10
- 229940045136 urea Drugs 0.000 claims description 6
- 239000011246 composite particle Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 4
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 4
- 239000002609 medium Substances 0.000 claims 1
- 238000004321 preservation Methods 0.000 claims 1
- 229920002521 macromolecule Polymers 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 description 11
- 238000000576 coating method Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 239000000975 dye Substances 0.000 description 8
- 238000005530 etching Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 239000004005 microsphere Substances 0.000 description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 3
- 239000010842 industrial wastewater Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000002262 Schiff base Substances 0.000 description 2
- 150000004753 Schiff bases Chemical class 0.000 description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
- 230000005591 charge neutralization Effects 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- OUUQCZGPVNCOIJ-UHFFFAOYSA-N hydroperoxyl Chemical group O[O] OUUQCZGPVNCOIJ-UHFFFAOYSA-N 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 238000010534 nucleophilic substitution reaction Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- SJEYSFABYSGQBG-UHFFFAOYSA-M Patent blue Chemical compound [Na+].C1=CC(N(CC)CC)=CC=C1C(C=1C(=CC(=CC=1)S([O-])(=O)=O)S([O-])(=O)=O)=C1C=CC(=[N+](CC)CC)C=C1 SJEYSFABYSGQBG-UHFFFAOYSA-M 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000000980 acid dye Substances 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 238000003321 atomic absorption spectrophotometry Methods 0.000 description 1
- 239000000981 basic dye Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000000982 direct dye Substances 0.000 description 1
- 239000000986 disperse dye Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- 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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- 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
- 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
- B01J20/28002—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 physical properties
- B01J20/28009—Magnetic properties
-
- 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
-
- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
-
- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
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)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a printing and dyeing industrial sewage treating agent and a preparation method thereof, belonging to the technical field of sewage treatment and comprising the following raw materials in parts by weight: 30-45 parts of composite adsorbent, 10-15 parts of modified loofah sponge fiber, 20-25 parts of sepiolite powder and 10-20 parts of polysilicate aluminum ferric sulfate; the dyeing and printing industrial sewage treating agent is prepared by the following steps: grinding and crushing the modified loofah sponge fiber, adding the composite adsorbent, sepiolite powder and poly-silicate aluminum ferric sulfate, and uniformly mixing to obtain the printing and dyeing industrial sewage treatment agent; the modified loofah sponge flocculant is prepared by mixing raw materials such as a composite adsorbent and modified loofah sponge fibers, the polysilicate aluminum ferric sulfate can be used as an inorganic flocculant, macromolecules can be rapidly settled when the flocculant is used, flocs are large, and the like.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to a printing and dyeing industrial sewage treatment agent and a preparation method thereof.
Background
At present, commercial dyes are numerous and mainly divided into three main classes: cationic dye: namely a basic dye; anionic dyes: including acid dyes, direct dyes, and the like; nonionic dyes: i.e. disperse dyes. In recent years, researchers at home and abroad often treat dye sewage by adopting methods such as an adsorption method, a flocculation method, a chemical method, an oxidation method, an electrolysis method and the like according to different properties of dyes.
The printing and dyeing industry sewage refers to industrial wastewater generated in the printing and dyeing industry, and is one of industrial wastewater which is difficult to treat because the wastewater has complex components and good chemical stability and is difficult to degrade in life. At present, a plurality of products are used for treating and purifying sewage in the printing and dyeing industry at home, but the currently adopted sewage treating agent cannot be repeatedly used for many times, so that the sewage treating cost is higher, and secondary pollution is easily caused to destroy the environment.
Disclosure of Invention
In order to solve the technical problems mentioned in the background technology, the invention aims to provide a printing and dyeing industrial sewage treatment agent and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
the dyeing and printing industrial sewage treatment agent comprises the following raw materials in parts by weight: 30-45 parts of composite adsorbent, 10-15 parts of modified loofah sponge fiber, 20-25 parts of sepiolite powder and 10-20 parts of polysilicate aluminum ferric sulfate;
the preparation method of the composite adsorbent comprises the following steps:
step S1, adding trisodium citrate, ferric chloride hexahydrate and urea into deionized water, stirring at a constant speed for 30min, adding polyacrylamide, stirring at a constant speed for 10min, transferring into a reaction kettle, reacting at 200 ℃ for 12h, cooling to room temperature after the reaction is finished, removing a supernatant, performing centrifugal separation, performing centrifugal washing for 2 times with deionized water and absolute ethyl alcohol, performing vacuum drying to obtain hollow ferroferric oxide, dispersing the prepared hollow ferroferric oxide into the deionized water, performing ultrasonic dispersion for 30min, adding oxalic acid, stirring at a constant speed at room temperature, reacting for 90min, separating after the reaction is finished, washing for five times with the deionized water, performing vacuum drying to obtain porous ferroferric oxide, and controlling the dosage ratio of the trisodium citrate, the ferric chloride hexahydrate, the urea, the polyacrylamide and the deionized water to be 5-8 mmol: 3-5 mmol: 12 mmol: 0.3-0.5 g: 100mL, and the dosage ratio of the hollow ferroferric oxide, the oxalic acid and the deionized water to be 50 mg: 150 mg: 100mL;
step S1, firstly preparing hollow ferroferric oxide by a hydrothermal method, then performing acid etching by oxalic acid, etching a porous structure on the prepared hollow ferroferric oxide substrate, increasing the specific surface area, and forming a microsphere structure with a hollow interior and a porous spherical surface.
And S2, adding chitosan and the prepared porous ferroferric oxide into a hydrochloric acid aqueous solution with the mass fraction of 0.5%, stirring while adding to prepare a suspension, then adding the suspension into a dispersion medium, slowly dropwise adding a glutaraldehyde aqueous solution with the mass fraction of 50% after uniformly mixing, heating to 50 ℃ after dropwise adding, continuously stirring for 1h, filtering, washing a filter cake with absolute ethyl alcohol and deionized water for three times respectively, drying at 65 ℃ to prepare composite particles, and controlling the dosage ratio of the chitosan, the porous ferroferric oxide, the hydrochloric acid aqueous solution, the dispersion medium and the glutaraldehyde aqueous solution to be 1-1.2 g: 1.5-2.0 g: 50 mL: 150 mL: 0.5mL.
In the step S2, span 80 is used as a surfactant, cyclohexane is used as a solvent, glutaraldehyde is used as a cross-linking agent, after blending, amino on chitosan reacts with carbonyl on glutaraldehyde to generate Schiff base, the chitosan is cross-linked to form a grid structure, part of the rest amino and hydroxyl are carried on the cross-linked chitosan, a 3d empty orbit of an iron atom and an arc on a nitrogen atom act on electrons or hydroxyl oxygen atoms to form a coordinate bond, and then the ferroferric oxide is coated, and the contact area and the contact site with the chitosan can be increased by preparing a porous and hollow structure from the ferroferric oxide, so that the coating stability is improved, on the other hand, the special porous and hollow structure can improve the coating efficiency and promote coating, the self weight of the hollow structure can be reduced, the coating effect is prevented from being influenced under the influence of self gravity, and the coating body is promoted to be more regular and uniform.
Further, the dispersion medium in the step S2 is formed by mixing cyclohexane and span 80 according to the volume ratio of 150mL to 1 mL.
Further, the preparation method of the modified loofah sponge fiber comprises the following steps:
dispersing loofah sponge fiber in deionized water, stirring at a constant speed for 10min to prepare slurry, adding sodium hydroxide, continuously stirring for 30min, adding 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, uniformly mixing, sequentially adding hydroxylamine hydrochloride and guanidine nitrate, heating to 50-55 ℃ while stirring, preserving heat for reaction for 3h, filtering after the reaction is finished, washing a filter cake with deionized water, drying at 65 ℃ for 20-24h to prepare modified loofah sponge fiber, and controlling the weight ratio of the loofah sponge fiber, the deionized water, the sodium hydroxide, the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, the hydroxylamine hydrochloride and the guanidine nitrate to be 8-10: 100: 0.6-0.7: 1.5-1.8: 0.035-0.045: 0.024-0.032.
In the preparation process, hydroxylamine hydrochloride and guanidine nitrate are added, so that the viscosity of an alkaline system can be reduced, the internal tissue of the loofah sponge fiber under the alkaline system is loose, the contact area of a modifier 3-chloro-2-hydroxypropyl trimethyl ammonium chloride and the loofah sponge fiber can be increased, nucleophilic substitution is carried out on the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride and the loofah sponge fiber, the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride is grafted on the surface and the internal tissue of the loofah sponge fiber, the loofah sponge fiber is cationized, charge neutralization reaction can be carried out on the loofah sponge fiber and printing and dyeing sewage, the adsorption effect of the loofah sponge fiber on dye and metal ions is improved, and in addition, the loofah sponge fiber can be degraded, is environment-friendly and cannot cause secondary pollution.
Further, the particle size of the sepiolite powder is 100-300 meshes.
A preparation method of a dyeing industrial sewage treatment agent comprises the following steps: and grinding and crushing the modified loofah sponge fiber, adding the composite adsorbent, sepiolite powder and poly-silicate aluminum ferric sulfate, and uniformly mixing to obtain the printing and dyeing industrial sewage treatment agent.
The invention has the beneficial effects that:
the invention relates to a dyeing and printing industrial sewage treatment agent, which is formed by mixing a composite adsorbent, modified loofah sponge fibers and other raw materials, wherein polysilicate aluminum ferric sulfate can be used as an inorganic flocculant, macromolecules can be rapidly settled when in use, flocs are large and the like, the composite adsorbent and sepiolite powder have good adsorption performance, span 80 is used as a surfactant in the preparation process of the composite adsorbent, cyclohexane is used as a solvent, glutaraldehyde is used as a cross-linking agent, after blending, amino on chitosan reacts with carbonyl on glutaraldehyde to generate Schiff base, the chitosan is cross-linked into a grid structure, part of residual amino and hydroxyl are carried on the cross-linked chitosan, a 3d empty orbit of an iron atom and an arc on a nitrogen atom act on electrons or hydroxyl oxygen atoms to form a coordinate bond, so that ferroferric oxide is coated, a porous and hollow structure is prepared by virtue of the ferroferric oxide, the contact area and contact sites with the chitosan can be increased, the coating stability is improved, on the other hand, the special porous and hollow structure can improve the coating efficiency, promote the coating of the coating structure to reduce the weight, prevent the influence of the ferroferric oxide coating under the self-coated ferroferric oxide coating, and can be used for maintaining the sewage treatment effect of the composite adsorbent and can be more excellent for the sewage treatment by virtue of the composite adsorbent, and the composite adsorbent when the sewage treatment agent is used for multiple times, the sewage treatment;
the modified loofah sponge fiber is prepared, hydroxylamine hydrochloride and guanidine nitrate are added in the preparation process, the viscosity of an alkaline system can be reduced, the internal tissue of the loofah sponge fiber under the alkaline system is loose, the contact area of a modifier 3-chloro-2-hydroxypropyl trimethyl ammonium chloride and the loofah sponge fiber can be increased, nucleophilic substitution is carried out on the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride and the loofah sponge fiber, the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride is grafted on the surface and the internal tissue of the loofah sponge fiber, the loofah sponge fiber is cationized, charge neutralization reaction can be carried out on the loofah sponge fiber and printing and dyeing sewage, the adsorption effect of the loofah sponge fiber on dyes and metal ions is improved, and in addition, the loofah sponge fiber can be degraded, is environment-friendly and cannot cause secondary pollution.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The preparation method of the modified loofah sponge fiber comprises the following steps:
dispersing loofah sponge fiber in deionized water, stirring at a constant speed for 10min to prepare slurry, adding sodium hydroxide, continuously stirring for 30min, adding 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, uniformly mixing, sequentially adding hydroxylamine hydrochloride and guanidine nitrate, heating to 50 ℃ while stirring, preserving heat, reacting for 3h, filtering after the reaction is finished, washing a filter cake with the deionized water, drying for 20h at 65 ℃ to prepare modified loofah sponge fiber, and controlling the weight ratio of the loofah sponge fiber to the deionized water to 0.6: 1.5: 0.035: 0.024.
Example 2
The preparation method of the modified loofah sponge fiber comprises the following steps:
dispersing loofah sponge fiber in deionized water, stirring at a constant speed for 10min to prepare slurry, adding sodium hydroxide, continuously stirring for 30min, adding 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, uniformly mixing, sequentially adding hydroxylamine hydrochloride and guanidine nitrate, heating to 52 ℃ while stirring, preserving heat, reacting for 3h, filtering after the reaction is finished, washing a filter cake with the deionized water, drying for 22h at 65 ℃ to prepare modified loofah sponge fiber, and controlling the weight ratio of the loofah sponge fiber to the deionized water to 0.7: 1.6: 0.040: 0.028.
Example 3
The preparation method of the modified loofah sponge fiber comprises the following steps:
dispersing loofah sponge fiber in deionized water, stirring at a constant speed for 10min to prepare slurry, adding sodium hydroxide, continuously stirring for 30min, adding 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, uniformly mixing, sequentially adding hydroxylamine hydrochloride and guanidine nitrate, heating to 55 ℃ while stirring, preserving heat, reacting for 3h, filtering after the reaction is finished, washing a filter cake with the deionized water, and drying for 24h at 65 ℃ to prepare modified loofah sponge fiber, wherein the weight ratio of the loofah sponge fiber to the deionized water to the sodium hydroxide to the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride to the hydroxylamine hydrochloride to the guanidine nitrate is controlled to be 10: 100: 0.7: 1.8: 0.045: 0.032.
Example 4
The preparation method of the composite adsorbent comprises the following steps:
step S1, adding trisodium citrate, ferric chloride hexahydrate and urea into deionized water, stirring at a constant speed for 30min, adding polyacrylamide, stirring at a constant speed for 10min, transferring into a reaction kettle, reacting at 200 ℃ for 12h, cooling to room temperature after the reaction is finished, removing a supernatant, performing centrifugal separation, performing centrifugal washing for 2 times with deionized water and absolute ethyl alcohol, performing vacuum drying to obtain hollow ferroferric oxide, dispersing the prepared hollow ferroferric oxide into the deionized water, performing ultrasonic dispersion for 30min, adding oxalic acid, stirring at a constant speed at room temperature, reacting for 90min, separating after the reaction is finished, washing for five times with the deionized water, performing vacuum drying to obtain porous ferroferric oxide, and controlling the dosage ratio of the trisodium citrate, the ferric chloride hexahydrate, the urea, the polyacrylamide and the deionized water to be 5 mmol: 3 mmol: 12 mmol: 0.3 g: 100mL, wherein the dosage ratio of the hollow ferroferric oxide, the oxalic acid and the deionized water to be 50 mg: 150 mg: 100mL;
step S1, firstly preparing hollow ferroferric oxide by a hydrothermal method, then performing acid etching by oxalic acid, etching a porous structure on the prepared hollow ferroferric oxide substrate, increasing the specific surface area, and forming a microsphere structure with a hollow interior and a porous spherical surface.
And S2, adding chitosan and the prepared porous ferroferric oxide into a hydrochloric acid aqueous solution with the mass fraction of 0.5%, stirring while adding to prepare a suspension, then adding the suspension into a dispersion medium, slowly dropwise adding a glutaraldehyde aqueous solution with the mass fraction of 50% after uniformly mixing, heating to 50 ℃ after dropwise adding, continuously stirring for 1h, filtering, washing a filter cake with absolute ethyl alcohol and deionized water for three times respectively, drying at 65 ℃ to prepare composite particles, and controlling the dosage ratio of the chitosan, the porous ferroferric oxide, the hydrochloric acid aqueous solution, the dispersion medium and the glutaraldehyde aqueous solution to be 1 g: 1.5 g: 50 mL: 150 mL: 0.5mL.
Example 5
The preparation method of the composite adsorbent comprises the following steps:
step S1, adding trisodium citrate, ferric chloride hexahydrate and urea into deionized water, stirring at a constant speed for 30min, adding polyacrylamide, stirring at a constant speed for 10min, transferring into a reaction kettle, reacting at 200 ℃ for 12h, cooling to room temperature after the reaction is finished, removing supernatant, performing centrifugal separation, performing centrifugal washing for 2 times by deionized water and absolute ethyl alcohol, performing vacuum drying to obtain hollow ferroferric oxide, dispersing the prepared hollow ferroferric oxide into deionized water, performing ultrasonic dispersion for 30min, adding oxalic acid, stirring at a constant speed at room temperature, reacting for 90min, separating after the reaction is finished, washing for five times by the deionized water, and performing vacuum drying to obtain porous ferroferric oxide, wherein the dosage ratio of the trisodium citrate, the ferric chloride hexahydrate, the urea, the polyacrylamide and the deionized water is controlled to be 5-8 mmol: 4 mmol: 12 mmol: 0.4 g: 100mL, and the dosage ratio of the hollow ferroferric oxide, the oxalic acid and the deionized water is controlled to be 50 mg: 150 mg: 100mL;
step S1, firstly preparing hollow ferroferric oxide by a hydrothermal method, then performing acid etching by oxalic acid, etching a porous structure on the prepared hollow ferroferric oxide substrate, increasing the specific surface area, and forming a microsphere structure with a hollow interior and a porous spherical surface.
And S2, adding chitosan and the prepared porous ferroferric oxide into a hydrochloric acid aqueous solution with the mass fraction of 0.5%, stirring while adding to prepare a suspension, then adding the suspension into a dispersion medium, slowly dropwise adding a glutaraldehyde aqueous solution with the mass fraction of 50%, heating to 50 ℃ after dropwise adding is finished, continuously stirring for 1h, filtering, washing a filter cake with absolute ethyl alcohol and deionized water for three times respectively, and drying at 65 ℃ to prepare composite particles, wherein the dosage ratio of the chitosan, the porous ferroferric oxide, the hydrochloric acid aqueous solution, the dispersion medium and the glutaraldehyde aqueous solution is controlled to be 1.1 g: 1.8 g: 50 mL: 150 mL: 0.5mL.
Example 6
The preparation method of the composite adsorbent comprises the following steps:
step S1, adding trisodium citrate, ferric chloride hexahydrate and urea into deionized water, stirring at a constant speed for 30min, adding polyacrylamide, stirring at a constant speed for 10min, transferring into a reaction kettle, reacting at 200 ℃ for 12h, cooling to room temperature after the reaction is finished, removing a supernatant, performing centrifugal separation, performing centrifugal washing for 2 times with deionized water and absolute ethyl alcohol, performing vacuum drying to obtain hollow ferroferric oxide, dispersing the prepared hollow ferroferric oxide into the deionized water, performing ultrasonic dispersion for 30min, adding oxalic acid, stirring at a constant speed at room temperature, reacting for 90min, separating after the reaction is finished, washing for five times with the deionized water, performing vacuum drying to obtain porous ferroferric oxide, and controlling the dosage ratio of the trisodium citrate, the ferric chloride hexahydrate, the urea, the polyacrylamide and the deionized water to be 8 mmol: 5 mmol: 12 mmol: 0.5 g: 100mL, wherein the dosage ratio of the hollow ferroferric oxide, the oxalic acid and the deionized water to be 50 mg: 150 mg: 100mL;
step S1, firstly preparing hollow ferroferric oxide by a hydrothermal method, then carrying out acid etching by oxalic acid, etching a porous structure on the prepared hollow ferroferric oxide substrate, increasing the specific surface area, and forming a microsphere structure with hollow inside and spherical porous surface.
And S2, adding chitosan and the prepared porous ferroferric oxide into a hydrochloric acid aqueous solution with the mass fraction of 0.5%, stirring while adding to prepare a suspension, then adding the suspension into a dispersion medium, slowly dropwise adding a glutaraldehyde aqueous solution with the mass fraction of 50% after uniformly mixing, heating to 50 ℃ after dropwise adding, continuously stirring for 1h, filtering, washing a filter cake with absolute ethyl alcohol and deionized water for three times respectively, drying at 65 ℃ to prepare composite particles, and controlling the dosage ratio of the chitosan, the porous ferroferric oxide, the hydrochloric acid aqueous solution, the dispersion medium and the glutaraldehyde aqueous solution to be 1.2 g: 2.0 g: 50 mL: 150 mL: 0.5mL.
Control group: the chitosan coated ferroferric oxide magnetic adsorbent is sold in the market.
The magnetic adsorbents of examples 4 to 6 and the control were examined for their adsorption and reuse properties, and the results are shown in the following table 1:
50mL of water source (Cr0.045-0.056 mg/L) is taken to be put into a 250mL triangular flask, 3g of the magnetic adsorbents in the examples 4-6 and the control group are respectively added into the triangular flask, the triangular flask is shaken in a constant temperature shaking box for 90min and then is kept stand and filtered, volatile phenol in the filtrate is measured by gas chromatography, cr (VI) in the filtrate is measured by atomic absorption spectrophotometry, the removal rate of the Cr (VI) is calculated, then the magnetic adsorbent is separated, and the experiment is repeated for 10 times after the filtrate is washed by deionized water, so that the removal rate of the Cr (VI) is calculated.
TABLE 1
| Example 4 | Example 5 | Example 6 | Control group | |
| 1 time removal rate% | 93.15 | 93.18 | 93.20 | 93.26 |
| Removal rate after 10 times% | 75.68 | 95.66 | 96.02 | 47.6 |
It can be seen from table 1 above that the adsorbents prepared in examples 4 to 6 of the present invention have excellent reuse properties.
Example 7
The dyeing and printing industrial sewage treatment agent comprises the following raw materials in parts by weight: 30 parts of the composite adsorbent prepared in example 4, 10 parts of the modified loofah sponge fiber prepared in example 1, 20 parts of sepiolite powder and 10 parts of polysilicate aluminum ferric sulfate;
the dyeing and printing industrial sewage treating agent is prepared by the following steps: and grinding and crushing the modified loofah sponge fiber, adding the composite adsorbent, sepiolite powder and poly-silicate aluminum ferric sulfate, and uniformly mixing to obtain the printing and dyeing industrial sewage treatment agent.
The particle size of the sepiolite powder is 100 meshes.
Example 8
The dyeing and printing industrial sewage treatment agent comprises the following raw materials in parts by weight: 40 parts of the composite adsorbent prepared in example 5, 12 parts of the modified loofah sponge fiber prepared in example 2, 22 parts of sepiolite powder and 15 parts of polysilicate aluminum ferric sulfate;
the dyeing and printing industrial sewage treating agent is prepared by the following steps: and grinding and crushing the modified loofah sponge fiber, adding the composite adsorbent, sepiolite powder and poly-silicate aluminum ferric sulfate, and uniformly mixing to obtain the printing and dyeing industrial sewage treatment agent.
The particle size of the sepiolite powder is 200 meshes.
Example 9
The dyeing and printing industrial sewage treatment agent comprises the following raw materials in parts by weight: 45 parts of the composite adsorbent prepared in example 6, 15 parts of the modified loofah sponge fiber prepared in example 3, 25 parts of sepiolite powder and 20 parts of polysilicate aluminum ferric sulfate;
the dyeing and printing industrial sewage treatment agent is prepared by the following steps: and grinding and crushing the modified loofah sponge fiber, adding the composite adsorbent, sepiolite powder and poly-silicate aluminum ferric sulfate, and uniformly mixing to obtain the printing and dyeing industrial sewage treatment agent.
The particle size of the sepiolite powder is 300 meshes.
Comparative example 1
This comparative example compares to example 7, replacing the composite adsorbent with chitosan.
Comparative example 2
Compared with example 7, the comparative example uses loofah sponge fiber to replace modified loofah sponge fiber.
Comparative example 3
The comparative example is a commercial industrial wastewater treatment agent.
In a sewage treatment plant of a certain printing and dyeing mill, the treating agents prepared in examples 7-9 and comparative examples 1-3 are put into sewage with the same dosage, stirred for 20min and kept stand for 30min, and the treated sewage is taken for detection, wherein each detection index is shown in table 2, and the unit of the substance content is mg/L;
TABLE 2
| Input amount | CODCr | BOD5 | SS | NH 3 -N | Color intensity | Transmittance of light | |
| Waste water | 315 | 58 | 180 | 140 | 180 | 20% | |
| Emission standard | 100 | 25 | 70 | 15 | 40 | 90 | |
| Example 7 | 100 | 24 | 9 | 4 | 11 | 8 | 98 |
| Example 8 | 100 | 25 | 10 | 5 | 11 | 6 | 98 |
| Example 9 | 100 | 23 | 9 | 5 | 10 | 7 | 98 |
| Comparative example 1 | 100 | 28 | 11 | 8 | 11 | 10 | 98 |
| Comparative example 2 | 100 | 56 | 16 | 12 | 13 | 12 | 95 |
| Comparative example 3 | 100 | 68 | 18 | 14 | 14 | 15 | 93 |
It can be seen from table 2 above that the treating agent prepared in the examples of the present invention has excellent sewage treatment effect.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (8)
1. The treating agent for the printing and dyeing industrial sewage is characterized by comprising the following raw materials in parts by weight: 30-45 parts of composite adsorbent, 10-15 parts of modified loofah sponge fiber, 20-25 parts of sepiolite powder and 10-20 parts of polysilicate aluminum ferric sulfate;
the preparation method of the composite adsorbent comprises the following steps:
step S1, adding trisodium citrate, ferric chloride hexahydrate and urea into deionized water, stirring at a constant speed for 30min, adding polyacrylamide, stirring at a constant speed for 10min, transferring into a reaction kettle, reacting at 200 ℃ for 12h, cooling to room temperature after the reaction is finished, removing supernate, performing centrifugal separation, performing centrifugal washing for 2 times by using deionized water and absolute ethyl alcohol, performing vacuum drying to prepare hollow ferroferric oxide, dispersing the prepared hollow ferroferric oxide into deionized water, performing ultrasonic dispersion for 30min, adding oxalic acid, stirring at a constant speed at room temperature, reacting for 90min, separating after the reaction is finished, washing for five times by using the deionized water, and performing vacuum drying to prepare porous ferroferric oxide;
and S2, adding chitosan and the prepared porous ferroferric oxide into a hydrochloric acid aqueous solution with the mass fraction of 0.5%, stirring while adding to prepare a suspension, then adding the suspension into a dispersion medium, uniformly mixing, slowly dropwise adding a glutaraldehyde aqueous solution with the mass fraction of 50%, heating to 50 ℃ after dropwise adding, continuously stirring for 1h, filtering, washing a filter cake with absolute ethyl alcohol and deionized water for three times respectively, and drying at 65 ℃ to prepare the composite particles.
2. The treatment agent for printing and dyeing industrial sewage according to claim 1, characterized in that in step S1, the dosage ratio of trisodium citrate, ferric chloride hexahydrate, urea, polyacrylamide and deionized water is controlled to be 5-8 mmol: 3-5 mmol: 12 mmol: 0.3-0.5 g: 100mL, and the dosage ratio of hollow ferroferric oxide, oxalic acid and deionized water is 50 mg: 150 mg: 100mL.
3. The treating agent for the printing and dyeing industrial sewage according to claim 1, wherein in the step S2, the dosage ratio of the chitosan, the porous ferroferric oxide, the aqueous solution of hydrochloric acid, the dispersion medium and the aqueous solution of glutaraldehyde is controlled to be 1-1.2 g: 1.5-2.0 g: 50 mL: 150 mL: 0.5mL.
4. The treating agent for the dyeing industrial sewage according to claim 3, wherein the dispersing medium in the step S2 is formed by mixing cyclohexane and span 80 according to a volume ratio of 150mL to 1 mL.
5. The treatment agent for the printing and dyeing industrial sewage according to claim 1, wherein the preparation method of the modified loofah sponge fiber comprises the following steps:
dispersing loofah sponge fiber in deionized water, stirring at a constant speed for 10min to prepare slurry, adding sodium hydroxide, continuously stirring for 30min, adding 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, uniformly mixing, sequentially adding hydroxylamine hydrochloride and guanidine nitrate, heating to 50-55 ℃ while stirring, carrying out heat preservation reaction for 3h, filtering after the reaction is finished, washing a filter cake with deionized water, and drying at 65 ℃ for 20-24h to prepare the modified loofah sponge fiber.
6. The treating agent for dyeing industrial sewage according to claim 5, wherein the weight ratio of loofah sponge fiber, deionized water, sodium hydroxide, 3-chloro-2-hydroxypropyltrimethylammonium chloride, hydroxylamine hydrochloride and guanidine nitrate is controlled to be 8-10: 100: 0.6-0.7: 1.5-1.8: 0.035-0.045: 0.024-0.032.
7. The treating agent for the industrial sewage generated by dyeing and printing as claimed in claim 1, wherein the particle size of the sepiolite powder is 100-300 meshes.
8. The preparation method of the dyeing industrial sewage treatment agent according to claim 1, characterized by comprising the following steps: and grinding and crushing the modified loofah sponge fiber, adding the composite adsorbent, sepiolite powder and poly-silicate aluminum ferric sulfate, and uniformly mixing to obtain the printing and dyeing industrial sewage treatment agent.
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