CN103212378B - Preparation method and application of citric acid modified palm tree bark adsorbing agent - Google Patents
Preparation method and application of citric acid modified palm tree bark adsorbing agent Download PDFInfo
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Abstract
The invention discloses a preparation method and an application technology of a citric acid modified palm tree bark adsorbing agent. The preparation method is characterized by comprising the following steps of: washing palm tree bark by water to remove mud and impurities, drying and crushing the washed palm tree bark, mixing the crushed palm tree bark with a 8%-20% citric acid solution according to the proportion of 1g: 5ml-15ml after the palm tree bark is dried by a NaOH aqueous solution, reacting the mixture for 35-60 minutes at room temperature, heating the reacted mixture to 50-60 DEG C, reacting the heated mixture for 24-36 hours, heating the reacted mixture to 120-130 DEG C, reacting the heated mixture for 1-2 hours, cooling the reacted mixture, washing the cooled mixture with distilled water until no citric acid exists in washing liquid, mixing the washing liquid with a 10%-20% magnesium chloride solution according to the proportion of 1g: 5ml-12ml, reacting the mixture at room temperature, performing suction filtration on the reacted mixture, washing the filtered mixture with a 5%-10% magnesium chloride solution, and finally, baking washing liquid to obtain the citric acid modified palm tree bark adsorbing agent. The adsorbing agent has high adsorption capacity to basic dye, good physical and chemical properties, high mechanical stability and strong regeneration capacity, and is recyclable, low in cost and environment-friendly.
Description
Technical field
The present invention relates to a kind of preparation method of biological adsorption agent and the applied technical field to Dye Adsorption in industrial wastewater, particularly a kind of citric acid modification palm bark absorbent preparation method and application technology.
Background technology
Along with industrial fast development, the consumption of dyestuff is also increasing, and synthetic dyestuffs, compared with natural dye, have the advantages such as easy to use, stable in properties, cost be low, wide in variety and are 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 the 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 I i of water body right, 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. conventionally.Wherein to have technique simple for absorption method, and adsorption rate is high, applied widely, and the features such as stable in properties are used widely in sewage disposal.
Since the 20 actual nineties, people utilize natural fiber cheap and easy to get in the processing of waste water from dyestuff, to obtain more research as adsorbent.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); Gong Xinhuai etc., have studied citric acid-modified bamboo bits absorption methylene blue, and it to the maximum adsorption capacity of methyl blue is: 125mg/g, (Gong Xinhuai etc., dynamics and the thermodynamic analysis of citric acid-modified bamboo bits absorption methylene blue, Yichun College's journal, 2012,34(8), 47 ~ 49); Poplar is superfine, and peanut hull meal is removed the research of azo dyes in the aqueous solution, biology magazine, 2005,22(2 as biological adsorption agent) 45 ~ 48; Li Ronghua etc., study the absorption of citric acid-modified orange skin to methyl blue in water, it to the maximum adsorption capacity of methyl blue is: 189.92mg/g, (Li Ronghua etc., the absorption of citric acid-modified orange skin to methyl blue in water, Journal of Northwest Sci Tech University of Agriculture and Forestry (natural science edition), 2009,37(10), 173 ~ 179); 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 red absorption property of bagasse centering, water science and engineering technology, 2012(5), 24 ~ 28); Chinese Patent Application No. is: in 201110208310.9 patent, disclose a kind of preparation method and application of citric acid modified rape straw adsorbent, it is characterized in that, wash clean dry rape straw soak 24h with 20% isopropyl alcohol, separate the soaking with sodium hydroxide of using again 0.1mol/L after being dried, stirring reaction 1 h, be washed to pH=7, dry, react 30min with the citric acid stirring at room temperature of 0.5mol/L again, be warming up to 50 DEG C of forced air drying 24 h, thermalization reaction 90min under the 120 DEG C of air blast conditions that heat up again, cooling washing; These agriculture and forestry are discarded to be utilized and to have the advantages such as renewable, degradable, environmental protection close friend, cheapness as the adsorbent of water treatment, important living resources, but part also comes with some shortcomings, as their bad mechanical strength, easily corrosion in water, the reusable number of times of adsorbent is very low, and adsorption capacity is limited.
Palm is perennial aiphyllium plant, 7 meters of Gao Keda; Dry upright, not branch, the palm-bark rain cape forming by leaf sheath is wrapped; Therefore the fiber of palm bark is very long, intensity is large, is typically used as making mattress, is one of most valuable ecological resources, is a kind of renewable resource.Palm is extensively planted area on the south the Changjiang river at present, is very precious long fibered raw material.This natural macromolecular material application is made absorption and is had the features such as natural, green, biodegradable, mechanical strength is large, resistance to corrosion is strong, palm bark is reused repeatedly as adsorbent is renewable, and dyestuff is had to larger adsorption capacity, palm bark chemical modification and absorption property are had no to report abroad.
Summary of the invention
One of object of the present invention is to provide a kind of citric acid modification palm bark absorbent preparation method, mainly makes the citric acid modification palm bark adsorbent that obtains larger as the adsorption capacity of the adsorbent of dyestuff in aqueous systems.
Object of the present invention is achieved through the following technical solutions.
A kind of citric acid modification palm bark absorbent preparation method, is characterised in that the method has following processing step:
(1) palm bark pretreatment: palm bark is washed with water and removes earth and impurity, putting into container is soaked in water 7 ~ 10 days, to remove non-fibrous material, by palm bark be cut into small pieces clear water clean, after vacuum drying, pulverize, by 20 ~ 40 object sieve, obtain pretreatment palm bark;
(2) palm bark basification: the NaOH aqueous solution soaking 10 ~ 20h that is 4 ~ 10% by mass percentage concentration by pretreatment palm bark, boil 10 ~ 30nim, cooling rear extremely neutral with deionized water washing, 100 ~ 120 DEG C of oven dry after suction filtration, palm bark must alkalize;
(3) citric acid palm leather is standby: in reactor, after the palm bark that alkalizes is mixed with the ratio of 1g:5 ~ 15mL with the citric acid solution of quality percentage 8 ~ 20%, room temperature reaction 35 ~ 60nim, heat up 50 ~ 60 DEG C, reaction 24 ~ 36 h, are being warming up to 120 ~ 130 DEG C, reaction 1 ~ 2 h, after cooling, wash in washing lotion and exist without citric acid with distilled water, obtain citric acid palm bark;
(4) palm bark absorbent preparation is modified in lemon acid: after citric acid palm bark is mixed with the ratio of 1g:5 ~ 12mL with the magnesium chloride solution of quality percentage 10 ~ 20%, room temperature reaction 1 ~ 6 h, suction filtration, with 5 ~ 10% magnesium chloride solution washing, 100 ~ 120 DEG C of oven dry, obtain lemon acid and modify palm bark adsorbent.
Another object of the present invention be to provide the acid of a kind of lemon modify palm bark adsorbent in aqueous systems to the application in basic-dyeable fibre absorption, feature is: the lemon acid preparing is modified to palm bark adsorbent deionized water and soak 1 ~ 2 h, adsorb by static method.
The lemon acid preparing can also be modified to palm bark adsorbent deionized water and soak 1 ~ 2 h, adsorb by dynamic method.
Advantage of the present invention and effect are:
(1) the lemon acid that the present invention obtains is modified palm bark adsorbent and is had good physical and chemical stability and excellent mechanical strength, the adsorption capacity that compares dyestuff with citric acid-modified tangerine peel, citric acid-modified bamboo bits, citric acid modification broomcorn straw is large, Reusability number of times improves greatly, can improve 50%;
(2) palm bark adsorbent is modified in the lemon acid that the present invention obtains can reach respectively 367.8mg/g, 447.7mg/g, 378.5mg/g to the adsorption capacity of methylene blue, crystal violet, basic fuchsin, and the clearance of dyestuff in sewage is reached as high as to 99.2%; The directly absorption to various basic-dyeable fibres in water body and wash-out, adsorption efficiency is high, and the speed of absorption is fast, and desorption performance is good, can within the scope of wider soda acid, use;
(3) technique of the present invention is simple, and condition is easy to control, and production cost is low, is easy to suitability for industrialized production;
(4) advantages such as the palmitic acid bark that the present invention uses is that natural regeneration macromolecular material is made adsorbent, by citric acid modification, uses this adsorbent environmentally safe, and production cost is low, and discarded object is biodegradable.
Detailed description of the invention
Embodiment 1
(1) palm bark pretreatment: palm bark is washed with water and removes earth and impurity, put into container and be soaked in water 7 days, to remove non-fibrous material, by palm bark be cut into small pieces clear water clean, after vacuum drying, pulverize, by 40 object sieve, obtain pretreatment palm bark;
(2) palm bark basification: the NaOH aqueous solution soaking 20h that is 4% by mass percentage concentration by pretreatment palm bark, boil 30nim, cooling rear extremely neutral with deionized water washing, 110 DEG C of oven dry after suction filtration, palm bark must alkalize;
(3) citric acid palm leather is standby: in reactor, after alkalization palm bark is mixed with the ratio of 1g:10mL with the citric acid solution of quality percentage 10%, room temperature reaction 60nim, heat up 50 DEG C, reaction 30 h, are being warming up to 125 DEG C, react 1 h, after cooling, wash in washing lotion and exist without citric acid with distilled water, obtain citric acid palm bark;
(4) palm bark absorbent preparation is modified in lemon acid: after citric acid palm bark is mixed with the ratio of 1g:5mL with the magnesium chloride solution of quality percentage 15%, room temperature reaction 6 h, suction filtration, with 5% magnesium chloride solution washing, 110 DEG C of oven dry, obtain lemon acid and modify palm bark adsorbent.
Embodiment 2
(1) palm bark pretreatment: palm bark is washed with water and removes earth and impurity, put into container and be soaked in water 10 days, to remove non-fibrous material, by palm bark be cut into small pieces clear water clean, after vacuum drying, pulverize, by 40 object sieve, obtain pretreatment palm bark;
(2) palm bark basification: the NaOH aqueous solution soaking 15h that is 6% by mass percentage concentration by pretreatment palm bark, boil 20nim, cooling rear extremely neutral with deionized water washing, 100 DEG C of oven dry after suction filtration, palm bark must alkalize;
(3) citric acid palm leather is standby: in reactor, after alkalization palm bark is mixed with the ratio of 1g:8mL with the citric acid solution of quality percentage 15%, room temperature reaction 40nim, heat up 50 DEG C, reaction 24 h, are being warming up to 120 DEG C, react 1.5 h, after cooling, wash in washing lotion and exist without citric acid with distilled water, obtain citric acid palm bark;
(4) palm bark absorbent preparation is modified in lemon acid: after citric acid palm bark is mixed with the ratio of 1g:6mL with the magnesium chloride solution of quality percentage 20%, room temperature reaction 2 h, suction filtration, with 5% magnesium chloride solution washing, 100 DEG C of oven dry, obtain lemon acid and modify palm bark adsorbent.
Embodiment 3
(1) palm bark pretreatment: palm bark is washed with water and removes earth and impurity, put into container and be soaked in water 7 days, to remove non-fibrous material, by palm bark be cut into small pieces clear water clean, after vacuum drying, pulverize, by 20 object sieve, obtain pretreatment palm bark;
(2) palm bark basification: the NaOH aqueous solution soaking 12h that is 8% by mass percentage concentration by pretreatment palm bark, boil 15nim, cooling rear extremely neutral with deionized water washing, 120 DEG C of oven dry after suction filtration, palm bark must alkalize;
(3) citric acid palm leather is standby: in reactor, after alkalization palm bark is mixed with the ratio of 1g:15mL with the citric acid solution of quality percentage 8%, room temperature reaction 60nim, heat up 60 DEG C, reaction 36 h, are being warming up to 125 DEG C, react 1.5 h, after cooling, wash in washing lotion and exist without citric acid with distilled water, obtain citric acid palm bark;
(4) palm bark absorbent preparation is modified in lemon acid: after citric acid palm bark is mixed with the ratio of 1g:10mL with the magnesium chloride solution of quality percentage 10%, room temperature reaction 4 h, suction filtration, with 8% magnesium chloride solution washing, 110 DEG C of oven dry, obtain lemon acid and modify palm bark adsorbent.
Embodiment 4
(1) palm bark pretreatment: palm bark is washed with water and removes earth and impurity, put into container and be soaked in water 10 days, to remove non-fibrous material, by palm bark be cut into small pieces clear water clean, after vacuum drying, pulverize, by 20 object sieve, obtain pretreatment palm bark;
(2) palm bark basification: the NaOH aqueous solution soaking 10h that is 10% by mass percentage concentration by pretreatment palm bark, boil 10nim, cooling rear extremely neutral with deionized water washing, 100 DEG C of oven dry after suction filtration, palm bark must alkalize;
(3) citric acid palm leather is standby: in reactor, after alkalization palm bark is mixed with the ratio of 1g:10mL with the citric acid solution of quality percentage 12%, room temperature reaction 50nim, heat up 55 DEG C, reaction 30 h, are being warming up to 130 DEG C, react 1 h, after cooling, wash in washing lotion and exist without citric acid with distilled water, obtain citric acid palm bark;
(4) palm bark absorbent preparation is modified in lemon acid: after citric acid palm bark is mixed with the ratio of 1g:8mL with the magnesium chloride solution of quality percentage 18%, room temperature reaction 5 h, suction filtration, with 8% magnesium chloride solution washing, 110 DEG C of oven dry, obtain lemon acid and modify palm bark adsorbent.
Embodiment 5
(1) palm bark pretreatment: palm bark is washed with water and removes earth and impurity, put into container and be soaked in water 7 days, to remove non-fibrous material, by palm bark be cut into small pieces clear water clean, after vacuum drying, pulverize, by 40 object sieve, obtain pretreatment palm bark;
(2) palm bark basification: the NaOH aqueous solution soaking 18h that is 5% by mass percentage concentration by pretreatment palm bark, boil 25nim, cooling rear extremely neutral with deionized water washing, 120 DEG C of oven dry after suction filtration, palm bark must alkalize;
(3) citric acid palm leather is standby: in reactor, after alkalization palm bark is mixed with the ratio of 1g:5mL with the citric acid solution of quality percentage 20%, room temperature reaction 60nim, heat up 55 DEG C, reaction 32 h, are being warming up to 125 DEG C, react 1 h, after cooling, wash in washing lotion and exist without citric acid with distilled water, obtain citric acid palm bark;
(4) palm bark absorbent preparation is modified in lemon acid: after citric acid palm bark is mixed with the ratio of 1g:5mL with the magnesium chloride solution of quality percentage 20%, room temperature reaction 6 h, suction filtration, with 10% magnesium chloride solution washing, 120 DEG C of oven dry, obtain lemon acid and modify palm bark adsorbent.
Embodiment 6
Take 0.10g lemon acid modification palm bark adsorbent and be placed in 250mL tool plug conical flask, adding 100mL concentration is in 550mg/L dye solution, taking the pH value of acid or alkali regulation system in 4.5 ~ 9.0 scopes, at room temperature concussion absorption 1 ~ 6 h, get supernatant, by the concentration of spectrophotometric determination dyestuff, according to the concentration difference of dyestuff in water before and after absorption, calculate the adsorption capacity that palm bark adsorbent is modified in lemon acid, the prepared lemon acid of embodiment 1 ~ 5 is modified palm bark adsorbent the adsorption capacity result of dyestuff is listed in to table 1.
The adsorption capacity measurement result of palm bark adsorbent to dyestuff modified in the acid of table 1 lemon
| Adsorbent title | pH | Adsorption time (h) | Methylene blue (mg/g) | Crystal violet (mg/g) | Basic fuchsin (mg/g) |
| Embodiment 1 | 5.5 | 2 | 365.6 | 446.5 | 375.2 |
| Embodiment 1 | 7.0 | 3 | 366.9 | 445.3 | 376.9 |
| Embodiment 2 | 6.0 | 4 | 367.8 | 447.2 | 377.2 |
| Embodiment 2 | 8.5 | 5 | 367.5 | 447.7 | 378.5 |
| Embodiment 3 | 5.0 | 6 | 366.2 | 446.9 | 378.4 |
| Embodiment 3 | 8.2 | 3.5 | 365.8 | 445.6 | 376.8 |
| Embodiment 4 | 4.5 | 2.5 | 364.8 | 444.2 | 375.1 |
| Embodiment 4 | 7.5 | 4.5 | 365.9 | 445.6 | 376.2 |
| Embodiment 5 | 7.2 | 5.5 | 367.2 | 447.5 | 377.9 |
| Embodiment 5 | 8.8 | 1 | 364.2 | 443.2 | 376.1 |
PH value adsorbent in 4.5 ~ 9.0 scopes does not affect the absorption of dyestuff as seen from Table 1, more than at room temperature concussion absorption 1 h, dyestuff adsorbs completely substantially, and the adsorption capacity of methylene blue, crystal violet, basic fuchsin can reach respectively 367.8 mg/g, 447.7 mg/g, 378.5 mg/g.
Embodiment 7
Take 1.0g lemon acid modification palm bark adsorbent and be placed in 250mL tool plug conical flask, adding 100mL concentration is in 200mg/L dye solution, taking the pH value of acid or alkali regulation system in 6.5 scopes, at room temperature concussion absorption 2 h, get supernatant, by the concentration of spectrophotometric determination dyestuff, according to the concentration difference of dyestuff in water before and after absorption, calculate lemon acid and modify the clearance of palm bark adsorbent to dyestuff, the prepared lemon acid of embodiment 1 ~ 5 is modified palm bark adsorbent the clearance result of dyestuff is listed in to this adsorbent pair of table 2., methylene blue, crystal violet, three kinds of dyestuffs of basic fuchsin going in water processed all more than 95%, reach as high as 99.2%.
The clearance of palm bark adsorbent to dyestuff modified in the acid of table 2 lemon
| Adsorbent title | Methylene blue (%) | Crystal violet (%) | Basic fuchsin (%) |
| Embodiment 1 | 96.6 | 98.2 | 97.6 |
| Embodiment 2 | 97.9 | 97.8 | 95.6 |
| Embodiment 3 | 99.2 | 96.9 | 99.2 |
| Embodiment 4 | 99 | 99.1 | 96.7 |
| Embodiment 5 | 98.5 | 98.2 | 97.6 |
Claims (3)
1. a preparation method for citric acid modification palm bark adsorbent, is characterized in that, the method has following processing step:
(1) palm bark pretreatment: palm bark is washed with water and removes earth and impurity, putting into container is soaked in water 7～10 days, to remove non-fibrous material, palm bark is cut into small pieces, and also clear water is clean, after vacuum drying, pulverize, by 20～40 object sieve, obtain pretreatment palm bark;
(2) palm bark basification: the NaOH aqueous solution soaking 10～20h that is 4～10% by mass percentage concentration by pretreatment palm bark, boil 10～30min, cooling rear extremely neutral with deionized water washing, after suction filtration, in 100～120 DEG C of oven dry, palm bark must alkalize;
(3) citric acid palm leather is standby: in reactor, after the citric acid solution that is 8～20% with mass percentage concentration by alkalization palm bark mixes with the ratio of 1g:5～15mL, room temperature reaction 35～60min, heat up 50～60 DEG C, reaction 24～36h, then be warming up to 120～130 DEG C, reaction 1～2h, after cooling, wash in washing lotion and exist without citric acid with distilled water, obtain citric acid palm bark;
(4) twist lemon acid and modify palm bark absorbent preparation: after the magnesium chloride solution that is 10～20% with mass percentage concentration by citric acid palm bark mixes with the ratio of 1g:5～12mL, room temperature reaction 1～6h, suction filtration, with 5～10% magnesium chloride solution washing, 100～120 DEG C of oven dry, obtain citric acid modification palm bark adsorbent.
2. the preparation method of a kind of citric acid modification palm bark adsorbent according to claim 1, is characterized in that, described magnesium chloride is pure for analyzing.
3. the preparation method of a kind of citric acid modification palm bark adsorbent according to claim 1, is characterized in that, citric acid modification palm bark adsorbent is for the absorption of the basic-dyeable fibre of industrial wastewater.
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| CN103464118B (en) * | 2013-09-26 | 2015-10-21 | 济南大学 | A kind of preparations and applicatio of epoxychloropropane palm fibre modification palmitic acid bark adsorbent |
| CN103464119B (en) * | 2013-09-28 | 2015-07-08 | 济南大学 | Preparation method and application of modified cysteine palm bark adsorbent |
| CN103566905B (en) * | 2013-10-29 | 2015-08-12 | 湖南大学 | Modified wood chips adsorbent, preparation method and in process containing the application in basic-dyeable fibre waste water |
| CN103566909B (en) * | 2013-11-13 | 2015-08-19 | 济南大学 | A kind of preparation method of citric acid cotton stalk skin and application |
| CN103920469B (en) * | 2014-05-06 | 2016-04-20 | 济南大学 | A kind of preparation method of citric acid silk adsorbent |
| CN105664869B (en) * | 2016-02-17 | 2017-10-27 | 济南大学 | A kind of lauroylamidopropyl betaine is modified the preparation of palm bark adsorbent |
| CN105668666A (en) * | 2016-04-19 | 2016-06-15 | 魏倩 | Sewage treating agent and preparation method and application thereof |
| CN107486169B (en) * | 2017-09-11 | 2019-03-15 | 济南大学 | A kind of preparation method of mercapto-propionyl-glycin modified magnetic complex microsphere |
| CN109289791A (en) * | 2018-11-29 | 2019-02-01 | 运城学院 | A method of dephosphorization adsorbent is prepared using citric acid-modified |
| CN109482156A (en) * | 2018-12-13 | 2019-03-19 | 重庆工商大学 | Preparation method of modified corn core biological adsorption agent and products thereof and application |
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| CN102266756A (en) * | 2011-07-25 | 2011-12-07 | 武汉工程大学 | Preparation method of citric acid modified rape straw adsorbent and application thereof |
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| CN102266756A (en) * | 2011-07-25 | 2011-12-07 | 武汉工程大学 | Preparation method of citric acid modified rape straw adsorbent and application thereof |
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