CN102921383A - Absorbent for cationic dyes in waste water and preparation method of absorbent - Google Patents
Absorbent for cationic dyes in waste water and preparation method of absorbent Download PDFInfo
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- CN102921383A CN102921383A CN2012104824726A CN201210482472A CN102921383A CN 102921383 A CN102921383 A CN 102921383A CN 2012104824726 A CN2012104824726 A CN 2012104824726A CN 201210482472 A CN201210482472 A CN 201210482472A CN 102921383 A CN102921383 A CN 102921383A
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Abstract
The invention relates to an absorbent for cationic dyes in waste water and preparation method of the absorbent and belongs to the technical field of environmental engineering. The preparation method of the absorbent for the cationic dyes comprises the steps as follows: modifying nano clay with an aminosilane coupling agent to prepare amino nano clay; stirring the amino nano clay and 0.1-6 percent by mass of dialdehyde polysaccharide solution at 30-60 DEG C for reaction for 1-4 h; and performing filtering, full washing with deionized water, vacuum drying, grinding and screening to prepare the absorbent for the cationic dyes. The absorbent for the cationic dyes is low in cost and easy to degrade, cannot cause secondary pollution, has high-activity surface groups and achieves high adsorption removal ratio for the cationic dyes; the preparation process is simple and controllable, and the absorbent is easy for large-scale industrial production; and the absorbent is suitable for daily sewage treatment, resource recovery is realized after adsorption, and cycle use is achieved.
Description
Technical field
The invention belongs to field of environment engineering technology, dye of positive ion adsorbent and preparation method thereof in a kind of waste water.
Background technology
750 tons of the about waste discharges of 1 ton of dyestuff of the every production of China, and in dyeing process, the loss amount of dyestuff is about 20%, wherein has approximately half to flow in the environment.Wherein the dye of positive ion (such as methylene blue, dimethyl diaminophenazine chloride and crystal violet) is the important chemical dyestuff of a class.Owing to the cation group of dyestuff can be in fabric the acidic-group of the 3rd monomer be combined and make stock-dye, be considered to the dedicated dye of acrylic fiber dyeing.When these dyestuffs be discharged enter water body after, tend to hinder the water body light transmission, slow down photosynthesis and the growth of water plant, reduce the dissolving of gas in the water, destroy aquatic ecosystem.In addition, dye colour is bright-coloured, dissolves in the water, in soil, atmosphere or the living environment, causes pollution on the sense organ to the people.And many dyestuffs or its catabolite have bio-toxicity; can be carcinogenic, teratogenesis even modificator gene sudden change; therefore these noxious materials will directly damage human body through the food chain transmission, remove that dye molecule is of great significance the protection of the environment tool in the water.
Many methods are arranged at present for the processing of waste water from dyestuff, such as microbial degradation, chemical oxidation, cohesion, film separation, absorption method etc.Absorption method has the advantages such as simple to operate, with low cost aspect the difficult degradation pollutant in removing water, be considered to a kind of method of effective removal organic dyestuff in wastewater, is subject to people's extensive use.Nanoclay is generally porous type chain stratiform and contains Shuifu County's zeopan class clay mineral, is interconnected by shared summit by silicon-oxy tetrahedron and magnalium octahedron to form, and zeolite cavity and hole run through total, are the porous mineral matter.Because its crystal structure inside has a large amount of zeolite cavities, and pore size is consistent, makes its effect with molecular sieve, can be used for the absorption of various industrial wastewaters.But because nanoclay only has the physical absorption ability, the material in the waste water is not had identification and a large amount of adsorption capacity, therefore need to be to its surface modification to improve its absorption property.
What the application of nanoclay surface modifying method was more is organically-modified, as adopt cationic surfactant modification (CN1793242A) or adopt chain alkyl guanidine modification (CN101538047A), although through traditional organically-modified after, absorption property with stronger organic pollution, but only limit to the absorption of hydrophobic organic pollutant such as polycyclic aromatic hydrocarbon etc., its organic matter to ionic does not have adsorption effect substantially.In addition, method of modifying commonly used uses amino graft modification in addition, such as amino coupling agent modification (CN101658782A), chitosan graft modification (CN102114412A) or ethylene polyamine or alkamine modified (CN102247807A), because its active group is mainly amino and can well combination occurs with anionic dye, but relatively poor to dye of positive ion absorption property.
The present invention adopts dialdehyde polysaccharide and amino nanoclay to carry out compound, it has nontoxic, biodegradable, the reproducible advantage of raw material, and contain a large amount of active groups such as hydroxyl, carboxyl etc. in the molecular structure, high with dye of positive ion reactivity, and have good physical and chemical stability after compound.Up to the present, not yet there are pertinent literature or invention that report was carried out in this research.
Summary of the invention
Simple nanoclay only has the physical absorption ability, material in the waste water do not had identification and a large amount of adsorption capacity, traditional organically-modifiedly do not have adsorption effect substantially to ionic organic compound, nanoclay after amino modified only has good adsorption capacity to anionic dye, the invention provides dye of positive ion adsorbent and preparation method thereof in a kind of waste water for this reason.
The present invention is achieved through the following technical solutions, and except specifying, related umber is parts by weight, and percentage is percetage by weight.
The invention provides dye of positive ion adsorbent and preparation method thereof in a kind of waste water, it is characterized in that the preparation method is as follows:
(1) nanoclay is dispersed in the toluene according to solid-liquid mass ratio 1:5-1:50, ultrasonic dispersion 30-60 minute, drip behind the amino silicane coupling agent ultrasonic 30-60 minute again, afterwards in 25-90 ℃ of reaction 10-72 hour, filtration washing after reaction finishes, vacuum drying, grinding is sieved, and namely gets amino nanoclay;
(2) be (0.1-6) % dialdehyde polysaccharide solution with above-mentioned amino nanoclay and mass fraction in temperature 30-60 ℃ stirring reaction 1-4 hour, filter afterwards and fully wash with deionized water, vacuum drying, grinding is sieved, and namely gets dye of positive ion adsorbent.
In above-mentioned technology case, described nanoclay is the layer silicate mineral with nanostructured.
In above-mentioned technology case, described dialdehyde polysaccharide makes 2 of polysaccharide for using periodic acid or periodate as oxidant, and the 3-o-dihydroxy is oxidized to dialdehyde, and aldehyde group content is the dialdehyde polysaccharide of (10-80) %.
In above-mentioned technology case, described dialdehyde polysaccharide is any one or a few mixture in dialdehyde starch, dialdehyde cellulose, dialdehyde carboxymethyl cellulose, dialdehyde sodium alginate, dialdehyde xanthans, dialdehyde Weilan gum, dialdehyde astragalus polyose, the dialdehyde SKGM.
In above-mentioned technology case, described nanoclay and amino silicane coupling agent reaction temperature are optimized for 30-70 ℃, and the reaction time is optimized for 10-40 hour.
Compared with the prior art the present invention has many-sided good effect and advantage, but concrete inductive generalization is as follows:
(1) the present invention is that natural macromolecular material and natural nano clay are compound, with low cost, and easily degraded, has good environmental-protecting performance, can not cause secondary environmental pollution;
(2) the dialdehyde polysaccharide that uses among the present invention because it has a large amount of high reaction activity groups, has good absorption property to the dye of positive ion.And it is that 5-7 all shows good adsorption effect at room temperature, pH, is fit to daily sewage disposal condition;
(3) preparation condition of modified Nano clay absorbent of the present invention is gentle, and raw material is easy to get, and is simple to operate, is easy to large-scale industrial production;
(4) modified Nano clay absorbent of the present invention can separate with water body by filter membrane, is easy to collect purifying, can repeat preparation and be used for absorption after processing through regeneration, can realize the recycling of resource.
The specific embodiment
The below provides three embodiment of the present invention, by embodiment the present invention is specifically described.Be necessary to be pointed out that at this; embodiment only is used for the present invention is further detailed; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of the invention described above.
In following examples, except specifying, related umber is parts by weight, and percentage is percetage by weight.
Embodiment 1
Take sodium carboxymethylcellulose as raw material, sodium metaperiodate is oxidant, and both ratios are 1:1, and reaction is about 4 hours under 35 ℃, pH value 3.0 conditions, is 73.85% dialdehyde carboxymethyl cellulose through making aldehyde group content after alcohol precipitation, washing, drying and the pulverizing.
Take by weighing in the toluene that 10 parts of imvites are dispersed in 100 parts, ultrasonic dispersion 30 minutes drips after 10 parts of amino coupling agent (APTES) ultrasonic 40 minutes again, in 30 ℃ of reactions 30 hours.After reaction finishes, filtration washing, vacuum drying, grinding is sieved, and namely gets amino nanoclay.Take by weighing simultaneously in the water that 10 parts of dialdehyde carboxymethyl celluloses add 990 parts to, continuous stir about 8 hours about 25 ℃ obtains mass fraction and is about 1% dialdehyde polysaccharide solution.The amino nanoclay dry product that takes by weighing 10 parts adds in the 1% dialdehyde polysaccharide solution, and, filter and fully wash with deionized water after 1 hour in 30 ℃ of stirring reactions of temperature, vacuum drying, grinding is sieved, and can make dye of positive ion adsorbent.
Embodiment 2
Take by weighing in the toluene that 30 parts of lithium algae soil are dispersed in 200 parts, ultrasonic dispersion 40 minutes drips after 45 parts of amino coupling agent (APTES) ultrasonic 30 minutes again, in 80 ℃ of reactions 20 hours.After reaction finishes, filtration washing, vacuum drying, grinding is sieved, and namely gets amino nanoclay.Take by weighing simultaneously in the water that 30 parts of dialdehyde starch add 970 parts to, continuous stir about 8 hours about 25 ℃ obtains mass fraction and is about 3% dialdehyde polysaccharide solution.The amino nanoclay dry product that takes by weighing 30 parts adds in the 3% dialdehyde polysaccharide solution, and, filter and fully wash with deionized water after 4 hours in 40 ℃ of stirring reactions of temperature, vacuum drying, grinding is sieved, and can make dye of positive ion adsorbent.
Embodiment 3
Take by weighing in the toluene that 20 parts of attapulgites are dispersed in 300 parts, ultrasonic dispersion 60 minutes drips after 40 parts of amino coupling agent (APTES) ultrasonic 40 minutes again, in 50 ℃ of reactions 40 hours.After reaction finishes, filtration washing, vacuum drying, grinding is sieved, and namely gets amino nanoclay.Take by weighing simultaneously in the water that 4 parts of dialdehyde xanthans add 996 parts to, continuous stir about 8 hours about 25 ℃ obtains mass fraction and is about 0.4% dialdehyde polysaccharide solution.The amino nanoclay dry product that takes by weighing 20 parts adds in the 0.4% dialdehyde polysaccharide solution, and, filter and fully wash with deionized water after 2 hours in the temperature 60 C stirring reaction, vacuum drying, grinding is sieved, and can make dye of positive ion adsorbent.
Embodiment 4
Take by weighing 10 parts of Dispersion of Kaolins in 400 parts toluene, ultrasonic dispersion 50 minutes drips after 30 parts of amino coupling agent (APTES) ultrasonic 50 minutes again, in 70 ℃ of reactions 50 hours.After reaction finishes, filtration washing, vacuum drying, grinding is sieved, and namely gets amino nanoclay.Take by weighing simultaneously in the water that 6 parts of dialdehyde Weilan gums add 994 parts to, continuous stir about 8 hours about 25 ℃ obtains mass fraction and is about 0.6% dialdehyde polysaccharide solution.The amino nanoclay dry product that takes by weighing 10 parts adds in the 0.6% dialdehyde polysaccharide solution, and, filter and fully wash with deionized water after 4 hours in the temperature 60 C stirring reaction, vacuum drying, grinding is sieved, and can make dye of positive ion adsorbent.
Claims (5)
1. dye of positive ion adsorbent in the waste water is characterized in that the preparation method is as follows:
(1) nanoclay is dispersed in the toluene according to solid-liquid mass ratio 1:5-1:50, ultrasonic dispersion 30-60 minute, drip behind the amino silicane coupling agent ultrasonic 30-60 minute again, afterwards in 25-90 ℃ of reaction 10-72 hour, filtration washing after reaction finishes, vacuum drying, grinding is sieved, and namely gets amino nanoclay;
(2) be (0.1-6) % dialdehyde polysaccharide solution with above-mentioned amino nanoclay and mass fraction in temperature 30-60 ℃ stirring reaction 1-4 hour, filter afterwards and fully wash with deionized water, vacuum drying, grinding is sieved, and namely gets dye of positive ion adsorbent.
2. dye of positive ion adsorbent in the waste water according to claim 1 is characterized in that described nanoclay is the layer silicate mineral with nanostructured.
3. dye of positive ion adsorbent in the waste water according to claim 1, it is characterized in that described dialdehyde polysaccharide is for using periodic acid or periodate as oxidant, make 2 of polysaccharide, the 3-o-dihydroxy is oxidized to dialdehyde, and aldehyde group content is the dialdehyde polysaccharide of (10-80) %.
4. dye of positive ion adsorbent in the waste water according to claim 1 is characterized in that described dialdehyde polysaccharide is any one or a few mixture in dialdehyde starch, dialdehyde cellulose, dialdehyde carboxymethyl cellulose, dialdehyde sodium alginate, dialdehyde xanthans, dialdehyde Weilan gum, dialdehyde astragalus polyose, the dialdehyde SKGM.
5. dye of positive ion adsorbent in the waste water according to claim 1 is characterized in that described nanoclay and amino silicane coupling agent reaction temperature are optimized for 30-70 ℃, and the reaction time is optimized for 10-40 hour.
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Cited By (9)
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|---|---|---|---|---|
| CN104861662A (en) * | 2015-06-08 | 2015-08-26 | 四川大学 | Nano composite soy protein plastic and preparation method thereof |
| CN107140711A (en) * | 2017-06-16 | 2017-09-08 | 扬州大学 | A kind of method for removing the dye of positive ion |
| CN108299564A (en) * | 2018-01-04 | 2018-07-20 | 嵊州盛泰色织科技有限公司 | A kind of preparation method of hydrophobicity cellulose base flocculation material for the coagulating treatment fabric dyeing waste water of multicomponent containing silk |
| CN108325504A (en) * | 2018-02-28 | 2018-07-27 | 武汉大学 | A kind of method of natural layered silicate nanoparticle and the charcoal secondary absorption removal dye of positive ion |
| CN108423859A (en) * | 2018-03-29 | 2018-08-21 | 浙江映山红纺织科技有限公司 | A kind for the treatment of method of printing and dying wastewater for the dye of positive ion |
| CN109181760A (en) * | 2018-10-30 | 2019-01-11 | 安徽海德化工科技有限公司 | A kind of production method of aromatic naphtha |
| CN109174023A (en) * | 2018-09-05 | 2019-01-11 | 河南科技大学 | A kind of nano-cellulose cross-linked graphene/chitosan aeroge and preparation method thereof, application |
| CN113083241A (en) * | 2021-03-26 | 2021-07-09 | 西南石油大学 | Preparation of sulfonylhydrazone modified natural polymer for efficiently treating oil field wastewater and dye wastewater |
| CN115595810A (en) * | 2022-11-10 | 2023-01-13 | 东莞市伊时针织印花有限公司（Cn） | Cationic dye for artificial fiber and preparation method thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104861662A (en) * | 2015-06-08 | 2015-08-26 | 四川大学 | Nano composite soy protein plastic and preparation method thereof |
| CN107140711A (en) * | 2017-06-16 | 2017-09-08 | 扬州大学 | A kind of method for removing the dye of positive ion |
| CN108299564A (en) * | 2018-01-04 | 2018-07-20 | 嵊州盛泰色织科技有限公司 | A kind of preparation method of hydrophobicity cellulose base flocculation material for the coagulating treatment fabric dyeing waste water of multicomponent containing silk |
| CN108325504A (en) * | 2018-02-28 | 2018-07-27 | 武汉大学 | A kind of method of natural layered silicate nanoparticle and the charcoal secondary absorption removal dye of positive ion |
| CN108325504B (en) * | 2018-02-28 | 2019-10-11 | 武汉大学 | A kind of method of natural layered silicate nanoparticle and the charcoal secondary absorption removal dye of positive ion |
| CN108423859A (en) * | 2018-03-29 | 2018-08-21 | 浙江映山红纺织科技有限公司 | A kind for the treatment of method of printing and dying wastewater for the dye of positive ion |
| CN108423859B (en) * | 2018-03-29 | 2020-05-05 | 浙江映山红纺织科技有限公司 | Printing and dyeing wastewater treatment method for cationic dye |
| CN109174023A (en) * | 2018-09-05 | 2019-01-11 | 河南科技大学 | A kind of nano-cellulose cross-linked graphene/chitosan aeroge and preparation method thereof, application |
| CN109181760A (en) * | 2018-10-30 | 2019-01-11 | 安徽海德化工科技有限公司 | A kind of production method of aromatic naphtha |
| CN113083241A (en) * | 2021-03-26 | 2021-07-09 | 西南石油大学 | Preparation of sulfonylhydrazone modified natural polymer for efficiently treating oil field wastewater and dye wastewater |
| CN115595810A (en) * | 2022-11-10 | 2023-01-13 | 东莞市伊时针织印花有限公司（Cn） | Cationic dye for artificial fiber and preparation method thereof |
| CN115595810B (en) * | 2022-11-10 | 2024-01-02 | 东莞市伊时针织印花有限公司 | Cationic dye for artificial fiber and preparation method thereof |
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