CN103464115A - Preparation and application of flax adsorbent - Google Patents
Preparation and application of flax adsorbent Download PDFInfo
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- CN103464115A CN103464115A CN2013104434772A CN201310443477A CN103464115A CN 103464115 A CN103464115 A CN 103464115A CN 2013104434772 A CN2013104434772 A CN 2013104434772A CN 201310443477 A CN201310443477 A CN 201310443477A CN 103464115 A CN103464115 A CN 103464115A
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Abstract
The invention discloses a preparation method and application technology of an epoxy chloropropane modified flax adsorbent. The preparation method is characterized by washing waste short fiber flax of a flax textile factory by using water, drying and crushing; processing by using NaOH and OP water solution and drying to obtain degummed flax; adding the following components in percentage by mass in a reactor: 22-40% of epoxy chloropropane, 12-25% of degummed flax, 4-8% of NaOH, 5-10% of isopropyl alcohol and 32-55% of water, wherein the sum of all the components is 100%; stirring at the constant temperature of 55-65 DEG C, carrying out backflow reaction for 1.0-4h, cooling, washing by using de-ionized water, carrying out suction extracting and filtering until the filtrate is neutral, washing by using a small amount of ethanol, drying in a 50-55 DEG C vacuum drying box, so as to obtain the epoxy chloropropane modified flax. The adsorbent has very high adsorbing capacity to basic dye, has high regeneration property, can be used repeatedly for several times, and is low in cost and environment-friendly.
Description
Technical field
The preparation method who the present invention relates to a kind of biological adsorption agent reaches the applied technical field to Dye Adsorption in industrial wastewater, the application technology that particularly a kind of epoxychloropropane is modified flax absorbent preparation method and sewage neutral and alkali Dye Adsorption is separated.
Background technology
Shortage of resources and environmental pollution have become two large subject matters of the world today, therefore, utilize natural reproducible resource, and the friendly type product of development environment and technology will become the inexorable trend of sustainable development.Flax is annual herbaceous plant, is one of the most valuable ecological resources, is a kind of renewable resource.The cultivated area of current national flax reaches more than 300 ten thousand mu, long stapled output is generally in 60kg/ mu left and right, flax has a series of premium properties as textile fabric, the characteristics such as good as softness, good luster, well-pressed, nice and cool, moisture pick-up properties and permeability are very precious textile fiber materials.But the short fiber that 2% left and right is arranged in fabrication processes is discarded object, it is the serious waste of flax resource that these discarded objects can not utilize fully, also makes the on-site environment of enterprise be polluted.Taken full advantage of these short fibers and both can also can create considerable economic benefit by environmental contamination reduction, utilized the absorption of these short fiber synthesizing new adsorbents for dyes, made this adsorbent there are natural, green, biodegradable characteristics.
Along with industrial fast development, the consumption of dyestuff is also increasing, and synthetic dyestuffs are compared with natural dye, has the advantages such as easy to use, stable in properties, cost be low, wide in variety and is widely used in weaving, papermaking, pharmacy and food industry.Waste water from dyestuff has become one of at present main pollutant effluents of China, and solving problem of environmental pollution is very urgent problem.The structure of most synthetic dyestuffs has complicated aromatic ring structure, and character is very stable, is difficult to biodegradation.These dyestuffs can threaten to the mankind's health, enter food chain, may cause people's allergy, the various injuries such as sudden change of cancer and gene.Being widely used of dyestuff causes being discharged in a large number in natural water of dye wastewater, cause water pollution, even if a small amount of waste water from dyestuff discharge also can cause water body painted, heavy damage the natural, ecological chain of water body, also greatly reduce the economic worth of water body simultaneously.Therefore, the dyestuff of how removing in industrial wastewater is the focus of domestic and international experts and scholars' research.In industrial production, waste water from dyestuff adopts flocculence, oxidizing process, biological treatment, membrane filter method, absorption method etc. usually.Wherein to have technique simple for absorption method, and adsorption rate is high, applied widely, and the characteristics such as stable in properties are used widely in sewage disposal.
Since the nineties in 20th century, people utilize natural fiber cheap and easy to get to obtain more research as adsorbent in the processing of waste water from dyestuff.Neha Gupta etc. has studied methylene blue and the malachite green in potato stalk adsorbed water, its maximum adsorption capacity is: 52.6mg/g, (Neha Gupta, Application of potato (Solanum tuberosum) plant wastes for the removal of methylene blue and malachite green dye from aqueous solution. Arabian Journal of Chemistry, (2011)); Runping Han etc. has studied the fallen leaves of Chinese parasol tree tree to the methylene blue adsorption number in water, its maximum adsorption capacity is: 89.7mg/g, (Runping Han, Biosorption of methylene blue from aqueous solution by fallen phoenix tree ' s leaves. Journal of Hazardous Materials, 141 (2007) 156 – 162); Li Shan etc., studied methylene blue in epoxychloropropane modified peanut shell adsorbed water, and its maximum adsorption capacity to methyl blue is: 25mg/g, (Li Shan etc., the research of methylene blue in epoxychloropropane modified peanut shell adsorbed water, dyestuff and dyeing, 2008,45(2): 49 ~ 51); Deng Jun is strong etc., has studied the red absorption property of bagasse centering, and the red maximum adsorption capacity of its centering is: 27.10mg/g, (Deng Junqiang etc., the research of the experiment of the absorption property that the bagasse centering is red, water science and engineering technology, 2012(5), 24 ~ 28).Natural macromolecular material is utilized as adsorbent has the advantages such as renewable, degradable, environmental protection be friendly, cheap, is important living resources.
Flax chemical modification and absorption property are also had to research abroad, M. Cox etc. has studied and has prepared active carbon with flax modification noble metal is adsorbed, its adsorption capacity is 1.708 mg/g(M. Cox, Sorption of precious metals onto chemically prepared carbon from flax shive. Hydrometallurgy, 78 (2005), 137-144).Li Xiaomin, HNO
3the research of flax waste material adsorbent of modifying to the zinc ion adsorptivity.Yili Teacher College's journal (natural science edition), 2011(1), its adsorption capacity of 45-48. is 0.324mmol/g.In the aqueous systems that the modification of employing flax chemical is obtained, the adsorbance of the adsorbent of metal ion is less, and the pH that is subject to absorption system affects larger, application number is: disclose preparation method and the application of a kind of sulfydryl flax in 201110276212.9 patent, sulfydryl flax is to Cd
2+adsorption capacity can be up to 282mg/g, high adsorption rate can reach 99.6%, to Pb
2+maximal absorptive capacity be 519mg/g, to Cu
2+maximal absorptive capacity be 160mg/g, the absorption that adopts flax to prepare is to the Dye Adsorption report seldom.
Summary of the invention
One of purpose of the present invention is to provide a kind of epoxychloropropane and modifies flax absorbent preparation method, and it is larger as the adsorbance of the adsorbent of dyestuff in aqueous systems that the epoxychloropropane that mainly makes to obtain is modified flax.
Purpose of the present invention is achieved through the following technical solutions.
A kind of epoxychloropropane is modified flax absorbent preparation method, is characterised in that the method has following processing step:
(1) flax pretreatment: short fiber flax that Flax Textile Enterprises is discarded washes, and after drying, is pulverized, and by 10 purpose sieve, obtains pretreatment flax;
(2) flax of coming unstuck: by pretreatment flax by 200 ~ 300g/L solid-to-liquid ratio, with being 1.5 ~ 4% and containing the emulsifier op-10 mass percentage concentration solution that is 0.5 ~ 1.5% containing the NaOH mass percentage concentration, soaking at room temperature 6 ~ 12 h, boil again 10 ~ 20min, constantly add water during azeotropic, to keep liquor capacity constant, cooling rear extremely neutral with the deionized water washing, dry under 75 ℃ after suction filtration, obtain the flax of coming unstuck;
(3) epoxychloropropane is modified flax preparation: in reactor, add epoxychloropropane by following composition mass percent: 22 ~ 40%, and the flax of coming unstuck: 12 ~ 25%, NaOH:4 ~ 8%; Isopropyl alcohol: 5 ~ 10%; Water: 32 ~ 55%, each component sum is absolutely, in 55 ~ 65 ℃ of constant temperature, stirring, back flow reaction 1.0 ~ 4 h, after cooling, with deionized water washing, suction filtration, till being neutrality to filtrate, with after a small amount of ethanol washing, be placed on drying in 50 ~ 55 ℃ of vacuum drying chambers, obtain epoxychloropropane and modify flax.
Another object of the present invention is to provide a kind of epoxychloropropane modification flax adsorbent adsorbs basic-dyeable fibre in aqueous systems, and characteristics are: the epoxychloropropane prepared is modified to deionized water immersion 1 ~ 2h for flax adsorbent, adsorb by static method.
The epoxychloropropane prepared is modified to flax adsorbent and by deionized water, soak 1 ~ 2h, by dynamic method absorption.
Advantage of the present invention and effect are:
(1) epoxychloropropane that the present invention obtains is modified flax adsorbent and is had good physical and chemical stability and excellent mechanical strength, and the adsorption capacity that compares dyestuff with modification tangerine peel, modified bamboo bits, broomcorn straw is large, and the Reusability number of times can reach more than 7 times;
(2) epoxychloropropane that the present invention obtains is modified absorption and the wash-out of flax adsorbent to various basic-dyeable fibres in water body, and adsorption efficiency is high, and the speed of absorption is fast, and desorption performance is good, can in wider soda acid scope, use;
(3) good stability, be the natural green product, biodegradable, the more important thing is the waste utilization of linen textile, so not only saved raw-material cost but also realized twice laid;
(4) the synthetic condition of crossing range request is easily controlled, and energy consumption is low, simple to operate, in whole production process, without " three wastes " discharge, belongs to process for cleanly preparing, is easy to suitability for industrialized production.
The specific embodiment
Embodiment 1
(1) flax pretreatment: short fiber flax that Flax Textile Enterprises is discarded washes, and after drying, is pulverized, and by 10 purpose sieve, obtains pretreatment flax;
(2) flax of coming unstuck: by pretreatment flax 20g, with 100mL, containing the NaOH mass percentage concentration, be 1.5% and containing the emulsifier op-10 mass percentage concentration solution that is 1.0%, soaking at room temperature 10h, boil again 15min, constantly add water during azeotropic, to keep liquor capacity constant, cooling rear extremely neutral with the deionized water washing, dry under 75 ℃ after suction filtration, obtain the flax of coming unstuck;
(3) epoxychloropropane is modified flax preparation: in reactor, add respectively epoxychloropropane: 20mL, the flax of coming unstuck: 10g, NaOH:2g; Isopropyl alcohol: 5mL; Water: 33mL, in 50 ℃ of constant temperature, stirring, back flow reaction 2 h, cooling after, with deionized water washing, suction filtration, till being neutrality to filtrate, with after a small amount of ethanol washing, be placed in 55 ℃ of vacuum drying chambers dryly, obtain epoxychloropropane modification flax.
Embodiment 2
(1) flax pretreatment: short fiber flax that Flax Textile Enterprises is discarded washes, and after drying, is pulverized, and by 10 purpose sieve, obtains pretreatment flax;
(2) flax of coming unstuck: by pretreatment flax 25g, with 100mL, containing the NaOH mass percentage concentration, be 2% and containing the emulsifier op-10 mass percentage concentration solution that is 0.5%, soaking at room temperature 6h, boil again 20min, constantly add water during azeotropic, to keep liquor capacity constant, cooling rear extremely neutral with the deionized water washing, dry under 75 ℃ after suction filtration, obtain the flax of coming unstuck;
(3) epoxychloropropane is modified flax preparation: in reactor, add respectively epoxychloropropane: 22mL, the flax of coming unstuck: 25g, NaOH:4; Isopropyl alcohol: 5mL; Water: 44mL, in 55 ℃ of constant temperature, stirring, back flow reaction 4h, cooling after, with deionized water washing, suction filtration, till being neutrality to filtrate, with after a small amount of ethanol washing, be placed in 55 ℃ of vacuum drying chambers dryly, obtain epoxychloropropane modification flax.
Embodiment 3
(1) flax pretreatment: short fiber flax that Flax Textile Enterprises is discarded washes, and after drying, is pulverized, and by 10 purpose sieve, obtains pretreatment flax;
(2) flax of coming unstuck: by pretreatment flax 30g, with 100mL, containing the NaOH mass percentage concentration, be 4% and containing the emulsifier op-10 mass percentage concentration solution that is 1.5%, soaking at room temperature 12h, boil again 10min, constantly add water during azeotropic, to keep liquor capacity constant, cooling rear extremely neutral with the deionized water washing, dry under 75 ℃ after suction filtration, obtain the flax of coming unstuck;
(3) epoxychloropropane is modified flax preparation: in reactor, add respectively epoxychloropropane: 40mL, the flax of coming unstuck: 15g, NaOH:4g; Isopropyl alcohol: 5mL; Water: 36mL, in 50 ℃ of constant temperature, stirring, back flow reaction 3 h, cooling after, with deionized water washing, suction filtration, till being neutrality to filtrate, with after a small amount of ethanol washing, be placed in 50 ℃ of vacuum drying chambers dryly, obtain epoxychloropropane modification flax.
Embodiment 4
(1) flax pretreatment: short fiber flax that Flax Textile Enterprises is discarded washes, and after drying, is pulverized, and by 10 purpose sieve, obtains pretreatment flax;
(2) flax of coming unstuck: by pretreatment flax 40g, with 200mL, containing the NaOH mass percentage concentration, be 4% and containing the emulsifier op-10 mass percentage concentration solution that is 0.5%, soaking at room temperature 8h, boil again 10min, constantly add water during azeotropic, to keep liquor capacity constant, cooling rear extremely neutral with the deionized water washing, dry under 75 ℃ after suction filtration, obtain the flax of coming unstuck;
(3) epoxychloropropane is modified flax preparation: in reactor, add respectively epoxychloropropane: 30mL, the flax of coming unstuck: 20g, NaOH:8g; Isopropyl alcohol: 10mL; Water: 32mL, in 55 ℃ of constant temperature, stirring, back flow reaction 2 h, cooling after, with deionized water washing, suction filtration, till being neutrality to filtrate, with after a small amount of ethanol washing, be placed in 55 ℃ of vacuum drying chambers dryly, obtain epoxychloropropane modification flax.
Embodiment 5
(1) flax pretreatment: short fiber flax that Flax Textile Enterprises is discarded washes, and after drying, is pulverized, and by 10 purpose sieve, obtains pretreatment flax;
(2) flax of coming unstuck: by pretreatment flax 50g, with 200mL, containing the NaOH mass percentage concentration, be 3% and containing the emulsifier op-10 mass percentage concentration solution that is 1.0%, soaking at room temperature 8h, boil again 10min, constantly add water during azeotropic, to keep liquor capacity constant, cooling rear extremely neutral with the deionized water washing, dry under 75 ℃ after suction filtration, obtain the flax of coming unstuck;
(3) epoxychloropropane is modified flax preparation: in reactor, add respectively epoxychloropropane: 22mL, the flax of coming unstuck: 12g, NaOH:5g; Isopropyl alcohol: 6mL; Water: 55mL, in 50 ℃ of constant temperature, stirring, back flow reaction 3 h, cooling after, with deionized water washing, suction filtration, till being neutrality to filtrate, with after a small amount of ethanol washing, be placed in 55 ℃ of vacuum drying chambers dryly, obtain epoxychloropropane modification flax.
Embodiment 6
(1) flax pretreatment: short fiber flax that Flax Textile Enterprises is discarded washes, and after drying, is pulverized, and by 10 purpose sieve, obtains pretreatment flax;
(2) flax of coming unstuck: by pretreatment flax 20g, with 100mL, containing the NaOH mass percentage concentration, be 2% and containing the emulsifier op-10 mass percentage concentration solution that is 1.5%, soaking at room temperature 12h, boil again 15min, constantly add water during azeotropic, to keep liquor capacity constant, cooling rear extremely neutral with the deionized water washing, dry under 75 ℃ after suction filtration, obtain the flax of coming unstuck;
(3) epoxychloropropane is modified flax preparation: in reactor, add respectively epoxychloropropane: 30mL, the flax of coming unstuck: 15g, NaOH:5g; Isopropyl alcohol: 10mL; Water: 40mL, in 55 ℃ of constant temperature, stirring, back flow reaction 2 h, cooling after, with deionized water washing, suction filtration, till being neutrality to filtrate, with after a small amount of ethanol washing, be placed in 55 ℃ of vacuum drying chambers dryly, obtain epoxychloropropane modification flax.
Embodiment 6
Take 1.0g epoxychloropropane modification flax adsorbent and be placed in 250mL tool plug conical flask, adding 100mL concentration is in the 500mg/L dye solution, take the pH value of acid or alkali regulation system in 4.0 ~ 9.0 scopes, at room temperature concussion absorption 0.5 ~ 1.5 h, get supernatant, by the concentration of spectrophotometric determination dyestuff, according to the concentration difference of dyestuff in water before and after absorption, calculate epoxychloropropane and modify the adsorption capacity of flax adsorbent
Result shows the adsorbent not impact of absorption on dyestuff in 4.5 ~ 8.5 scopes of pH value, more than at room temperature concussion absorption 0.5h, dyestuff adsorbs fully substantially, and the adsorption capacity of methylene blue, crystal violet, basic fuchsin and malachite green can reach 139.2mg/g, 175.5mg/g, 137.1mg/g, 156.2mg/g respectively.
Embodiment 7
Take 2.0g epoxychloropropane modification flax adsorbent and be placed in 250mL tool plug conical flask, adding 100mL concentration is in the 100mg/L dye solution, take the pH value of acid or alkali regulation system in 5.5 scopes, at room temperature concussion absorption 0.5h, get supernatant, concentration with the spectrophotometric determination dyestuff, concentration difference according to dyestuff in water before and after absorption, calculate epoxychloropropane and modify the clearance of flax adsorbent to dyestuff, result shows, this adsorbent is to methylene blue, crystal violet, four kinds of dyestuffs of basic fuchsin and malachite green going in water processed all more than 95%, reach as high as 98.2%%.
Embodiment 8
Epoxychloropropane is modified flax adsorbent Dynamic Adsorption application process: adopt spectrophotometry after separating, the step of its concrete grammar is as follows:
(1) preparation of extraction column: the epoxychloropropane prepared is modified to flax adsorbent, take water as homogenate, carry out wet method dress post, this post washes with water repeatedly standby successively;
(2) getting 100mL concentration is 50mg/L waste water from dyestuff solution, regulating the pH value is 5.5 left and right, pass through respectively solid-phase extraction column with 0.25mL/ min, with deionized water drip washing solid-phase extraction column, by the 15mL volume fraction, be 15% ethanol solution hydrochloride wash-out again, flow velocity is 0.25mL/ min, collects eluent;
(3) content of spectrophotometry dyestuff for eluent.
Claims (4)
1. an epoxychloropropane is modified flax absorbent preparation method, is characterised in that the method has following processing step:
(1) flax pretreatment: short fiber flax that Flax Textile Enterprises is discarded washes, and after drying, is pulverized, and by 10 purpose sieve, obtains pretreatment flax;
(2) flax of coming unstuck: by pretreatment flax by 200 ~ 300g/L solid-to-liquid ratio, with being 1.5 ~ 4% and containing the emulsifier op-10 mass percentage concentration solution that is 0.5 ~ 1.5% containing the NaOH mass percentage concentration, soaking at room temperature 6 ~ 12 h, boil again 10 ~ 20min, cooling rear extremely neutral with the deionized water washing, dry under 75 ℃ after suction filtration, obtain the flax of coming unstuck;
(3) epoxychloropropane is modified flax preparation: in reactor, add epoxychloropropane by following composition mass percent: 22 ~ 40%, and the flax of coming unstuck: 12 ~ 25%, NaOH:4 ~ 8%; Isopropyl alcohol: 5 ~ 10%; Water: 32 ~ 55%, each component sum is absolutely, in 55 ~ 65 ℃ of constant temperature, stirring, back flow reaction 1.0 ~ 4 h, after cooling, with deionized water washing, suction filtration, till being neutrality to filtrate, with after a small amount of ethanol washing, be placed on drying in 50 ~ 55 ℃ of vacuum drying chambers, obtain epoxychloropropane and modify flax.
2. modify flax absorbent preparation according to the epoxychloropropane described in claim 1, it is characterized in that: flax is the discarded short fiber flax waste material of Flax Textile Enterprises.
3. modify flax absorbent preparation according to the epoxychloropropane described in claim 1, it is characterized in that: in step (2), emulsifier op-10 is the condensation product of alkyl phenol and oxirane, belongs to nonionic surface active agent.
4. modify flax absorbent preparation according to the epoxychloropropane described in claim 1, it is characterized in that the application to water neutral and alkali Dye Adsorption.
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Cited By (10)
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| CN103933942A (en) * | 2014-03-13 | 2014-07-23 | 济南大学 | Preparation and application of (mercaptopropyl)trimethoxy silane modified flax adsorbent |
| CN104289190A (en) * | 2014-09-10 | 2015-01-21 | 济南大学 | Preparation of dimethyl diallyl ammonium chloride modified flax adsorbent |
| CN104772125A (en) * | 2015-03-23 | 2015-07-15 | 济南大学 | Epoxy resin modified sand absorption material and preparation method thereof |
| CN105440475A (en) * | 2015-10-30 | 2016-03-30 | 嘉善贝马五金配件有限公司 | Lignocellulose-toughened polyvinyl chloride automobile internal decorating material and preparation method therefor |
| CN105728058A (en) * | 2016-02-17 | 2016-07-06 | 济南大学 | Preparation method for hemp-supported nanometer titanium dioxide photocatalyst |
| CN106186368A (en) * | 2016-10-11 | 2016-12-07 | 福建省农业科学院农业工程技术研究所 | A kind of preparation method of saprobia fermentation process agent |
| CN106348360A (en) * | 2016-10-26 | 2017-01-25 | 商丘师范学院 | Wastewater cleaning agent based on photocatalysis |
| CN106560238A (en) * | 2016-10-11 | 2017-04-12 | 伊犁师范学院 | Preparation method and applications of tartaric acid modified flax |
| CN106560237A (en) * | 2016-10-11 | 2017-04-12 | 伊犁师范学院 | Preparation method and application of DL-malic acid modified flax adsorbent |
| CN109289823A (en) * | 2018-11-06 | 2019-02-01 | 湖南鸿捷新材料有限公司 | A kind of regeneration method of the waste active carbon of hydrometallurgy extraction process |
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Cited By (10)
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|---|---|---|---|---|
| CN103933942A (en) * | 2014-03-13 | 2014-07-23 | 济南大学 | Preparation and application of (mercaptopropyl)trimethoxy silane modified flax adsorbent |
| CN104289190A (en) * | 2014-09-10 | 2015-01-21 | 济南大学 | Preparation of dimethyl diallyl ammonium chloride modified flax adsorbent |
| CN104772125A (en) * | 2015-03-23 | 2015-07-15 | 济南大学 | Epoxy resin modified sand absorption material and preparation method thereof |
| CN105440475A (en) * | 2015-10-30 | 2016-03-30 | 嘉善贝马五金配件有限公司 | Lignocellulose-toughened polyvinyl chloride automobile internal decorating material and preparation method therefor |
| CN105728058A (en) * | 2016-02-17 | 2016-07-06 | 济南大学 | Preparation method for hemp-supported nanometer titanium dioxide photocatalyst |
| CN106186368A (en) * | 2016-10-11 | 2016-12-07 | 福建省农业科学院农业工程技术研究所 | A kind of preparation method of saprobia fermentation process agent |
| CN106560238A (en) * | 2016-10-11 | 2017-04-12 | 伊犁师范学院 | Preparation method and applications of tartaric acid modified flax |
| CN106560237A (en) * | 2016-10-11 | 2017-04-12 | 伊犁师范学院 | Preparation method and application of DL-malic acid modified flax adsorbent |
| CN106348360A (en) * | 2016-10-26 | 2017-01-25 | 商丘师范学院 | Wastewater cleaning agent based on photocatalysis |
| CN109289823A (en) * | 2018-11-06 | 2019-02-01 | 湖南鸿捷新材料有限公司 | A kind of regeneration method of the waste active carbon of hydrometallurgy extraction process |
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