CN105268418A - Preparation method of cross-linked chitosan modified shaddock peel adsorption material for removing low-concentration heavy metals in waste water - Google Patents
Preparation method of cross-linked chitosan modified shaddock peel adsorption material for removing low-concentration heavy metals in waste water Download PDFInfo
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Abstract
The invention relates to a preparation method of a cross-linked chitosan modified shaddock peel adsorption material for removing low-concentration heavy metals in waste water and belongs to the field of waste water treatment. According to the preparation method, substances, such as chitosan, methanol water and the like, are filtered after being subjected to water circumfluence; filter residues are acid-pickled, alkaline-leached, washed and dried and are mixed with acetic acid and epichlorohydrin; after a pH value is regulated, the reaction is performed; by suction filtration, washing, drying and sieving, chitosan powder is obtained; then shaddock peel is obtained, is washed and dried and is ground into particles; the particles are added into sodium hydroxide solution and absolute ethyl alcohol for soaking; after centrifugation is carried out and the pH value is regulated, the obtained product is dried and is placed into a vacuum flask; in a negative pressure state, the obtained product is added into chitosan modification liquid for soaking; processing is carried out in a plasma form; filtration is carried out to obtain filter residues; and the filter residues are washed and dried to obtain the cross-linked chitosan modified shaddock peel adsorption material. In waste water treated by the cross-linked chitosan modified shaddock peel adsorption material prepared by the preparation method, mercury content is reduced to 0.5 to 1mg/L, nickel content is reduced to 0.5 to 0.7mg/L, and copper ion content is reduced to 0.04 to 0.05mg/L; treatment efficiency is high; secondary pollution cannot be generated.
Description
Technical field
The present invention relates to the preparation method that a kind of cross-linked chitosan modification pomelo peel removes low-concentration heavy metal sorbing material in waste water, belong to field of waste water treatment.
Background technology
Heavy metal wastewater thereby mostly from enterprises such as mining, ore dressing, smelting, intermetallic composite coating, by food chain, is easily enriched in organism, and harm humans is healthy.The method of process heavy metal wastewater thereby can be summarized as chemical method, physical-chemical process, bioanalysis three class.Wherein chemical method has moderate water-cut stage, sulphide precipitation, the ferrite precipitation method, the barium salt precipitation method etc.; Physical-chemical process has ion-exchange, absorption method, solvent extraction, liquid-film method, hyperfiltration and electroosmose process; Bioanalysis is divided into biological adsorption and biogenic sediment.
Method the most frequently used is at present chemical precipitation method, can remove the metal ion in waste water fast, and technical process is simple, but the shortcoming such as it is higher to there is water outlet metal concentration, easily produces secondary pollution, and waste water calcic is high, reuse is difficult.When concentration of metal ions low to 1 ~ 10mg/L time, be difficult to reach desirable effect with chemical precipitation and solution extracting.Other method is as ion-exchange, active carbon adsorption, electrodialysis, counter-infiltration etc., although treatment effect is better, but because operating cost and the cost of raw material are relatively too high, as: traditional absorption method adopts the adsorbents such as expensive active carbon and ion exchange resin, is difficult to the needs adapting to extensive wastewater treatment.
Summary of the invention
The technical problem that the present invention mainly solves: although the metal ion in waste water can be removed fast for chemical precipitation method, but it is higher to there is water outlet metal concentration, easy generation secondary pollution, waste water calcic is high, the problems such as reuse difficulty, provide the preparation method that a kind of cross-linked chitosan modification pomelo peel removes low-concentration heavy metal sorbing material in waste water, the present invention mainly utilizes cross-linked chitosan to process low concentration heavy metal water, adsorption capacity in conjunction with pomelo peel processes, the Mercury in Wastewater content 40 ~ 45mg/L of process of the present invention is down to 0.5 ~ 1mg/L, nickel content 30 ~ 40mg/L is down to 0.5 ~ 0.7mg/L, copper ion 25 ~ 35mg/L is down to 0.04 ~ 0.05mg/L, treatment effeciency is high, secondary pollution can not be produced.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention:
(1) count by weight, choose the shitosan of 20 ~ 45 parts respectively, the mass fraction of 15 ~ 30 parts is the methanol aqueous solution of 40%, the mass fraction of 20 ~ 25 parts is the benzaldehyde solution of 10% and the acetone of 20 ~ 25 parts, under temperature is 85 ~ 90 DEG C of water bath with thermostatic control conditions, reflux 1h in there-necked flask, after backflow completes, it is filtered, collect filter residue;
(2) by the filter residue of above-mentioned collection at temperature is 25 ~ 30 DEG C, be soak 48h in the hydrochloric acid solution of 4% at mass fraction, after benzaldehyde to be removed, 3 ~ 5min is soaked again by the NaOH solution of 0.5mol/L, after pickling alkali has soaked, adopt deionized water cyclic washing to be 7.0 to pH, be placed on dry 10 ~ 12h in 55 ~ 60 DEG C of baking ovens subsequently, be prepared into modification of chitosan particle;
(3) 1:10 in mass ratio, be the aqueous acetic acid of 1% by the modification of chitosan particle of above-mentioned preparation and mass fraction, be uniformly mixed and dissolve completely to it, be prepared into chitosan gum lime set, 1:25 in mass ratio again, is added to epoxychloropropane in chitosan gel rubber, is uniformly mixed under 2600 ~ 2800r/min, and drip mass fraction be 10% sodium hydroxide solution regulate its pH to be 8.5 ~ 9.5, reaction 10 ~ 15h;
(4) after question response completes, dropping mass concentration is that the hydrochloric acid solution of 1.25mol/L regulates its pH to be 7.0, subsequently filter cake is collected to its suction filtration, by it by deionized water washing 3 ~ 5 times, and be placed in the dry 10 ~ 12h of 75 ~ 80 DEG C of baking ovens, taken out subsequently and milled and sieved, be prepared into 180 ~ 200 order Chitosan powder for subsequent use;
(5) fresh grapefruit skin is got, after respectively washing 3 ~ 5 times by running water and distilled water, constant weight is dried in 65 ~ 70 DEG C of baking ovens, subsequently it is freezingly milled and sieved, be prepared into 35 ~ 40 order pomelo peel particles, count by weight subsequently, choose the sodium hydroxide solution of the mass concentration 0.85mol/L of 30 ~ 55 parts respectively, the absolute ethyl alcohol of the pomelo peel particle of 5 ~ 10 parts and 40 ~ 60 parts, 10 ~ 12h is soaked at being placed on 20 ~ 30 DEG C, taken out subsequently and centrifugal filtration, collecting precipitation to spend deionized water to pH be after 7.0, be placed on dry 20 ~ 24h in 70 ~ 75 DEG C of baking ovens, be prepared into pretreatment pomelo peel particle,
(6) Chitosan powder prepared by step (4) and deionized water, be uniformly mixed by solid-liquid mass ratio 1:10, form chitin modified liquid, subsequently the pomelo peel particle of above-mentioned preparation is put into the Dewar bottle that volume is 1L, pass into nitrogen deaeration, after air is discharged completely, again nitrogen in bottle is detached, forming vacuum pressure is-0.05MPa, under negative pressure state, by pomelo peel particle and modified solution mass ratio 1:25, chitin modified liquid is added in Dewar bottle, ensures complete for pomelo peel particle submergence;
(7) submergence 10 ~ 15min is treated, plasma modification device rf frequency is set, open radio-frequency power supply, add the discharge power of 200 ~ 300kw between outer electrode when processing, in process bottle, nitrogen forms plasma form, after plasma treatment 30 ~ 40min, removed and filtered, collect filter residue and spend deionized water 3 ~ 5 times, and being placed in the dry 10 ~ 12h of 70 ~ 80 DEG C of baking ovens, a kind of cross-linked chitosan modification pomelo peel can be prepared into and remove low-concentration heavy metal sorbing material in waste water.
Application of the present invention: getting a kind of cross-linked chitosan modification pomelo peel that 20 ~ 40mg obtains, to remove in waste water that low-concentration heavy metal sorbing material is carried on aperture be on the screen cloth of 15 ~ 17 μm, screen cloth is holded up and is placed in low concentration heavy metal water treatment pond, one is laid every 40 ~ 50cm, process 1 ~ 3h, the Mercury in Wastewater content 40 ~ 45mg/L of process of the present invention is down to 0.5 ~ 1mg/L, nickel content 30 ~ 40mg/L is down to 0.5 ~ 0.7mg/L, copper ion 25 ~ 35mg/L is down to 0.04 ~ 0.05mg/L, treatment effeciency is high, secondary pollution can not be produced, meet state sewage emission standard, secondary pollution can not be produced.
The invention has the beneficial effects as follows:
(1) the Mercury in Wastewater content 40 ~ 45mg/L processed is down to 0.5 ~ 1mg/L, and nickel content 30 ~ 40mg/L is down to 0.5 ~ 0.7mg/L, and copper ion 25 ~ 35mg/L is down to 0.04 ~ 0.05mg/L, and treatment effeciency is high, and treatment effeciency is high;
(2) secondary pollution can not be produced;
(3) preparation process is simple, and cost is low.
Detailed description of the invention
First count by weight, choose the shitosan of 20 ~ 45 parts respectively, the mass fraction of 15 ~ 30 parts is the methanol aqueous solution of 40%, the mass fraction of 20 ~ 25 parts is the benzaldehyde solution of 10% and the acetone of 20 ~ 25 parts, under temperature is 85 ~ 90 DEG C of water bath with thermostatic control conditions, reflux 1h in there-necked flask, after backflow completes, it is filtered, collect filter residue, by the filter residue of above-mentioned collection at temperature is 25 ~ 30 DEG C, be soak 48h in the hydrochloric acid solution of 4% at mass fraction, after benzaldehyde to be removed, 3 ~ 5min is soaked again by the NaOH solution of 0.5mol/L, after pickling alkali has soaked, adopt deionized water cyclic washing to be 7.0 to pH, be placed on dry 10 ~ 12h in 55 ~ 60 DEG C of baking ovens subsequently, be prepared into modification of chitosan particle, 1:10 in mass ratio again, be the aqueous acetic acid of 1% by the modification of chitosan particle of above-mentioned preparation and mass fraction, be uniformly mixed and dissolve completely to it, be prepared into chitosan gum lime set, 1:25 in mass ratio again, is added to epoxychloropropane in chitosan gel rubber, is uniformly mixed under 2600 ~ 2800r/min, and drip mass fraction be 10% sodium hydroxide solution regulate its pH to be 8.5 ~ 9.5, reaction 10 ~ 15h, after question response completes, dropping mass concentration is that the hydrochloric acid solution of 1.25mol/L regulates its pH to be 7.0, subsequently filter cake is collected to its suction filtration, by it by deionized water washing 3 ~ 5 times, and be placed in the dry 10 ~ 12h of 75 ~ 80 DEG C of baking ovens, taken out subsequently and milled and sieved, be prepared into 180 ~ 200 order Chitosan powder for subsequent use, then fresh grapefruit skin is got, after respectively washing 3 ~ 5 times by running water and distilled water, constant weight is dried in 65 ~ 70 DEG C of baking ovens, subsequently it is freezingly milled and sieved, be prepared into 35 ~ 40 order pomelo peel particles, count by weight subsequently, choose the sodium hydroxide solution of the mass concentration 0.85mol/L of 30 ~ 55 parts respectively, the absolute ethyl alcohol of the pomelo peel particle of 5 ~ 10 parts and 40 ~ 60 parts, 10 ~ 12h is soaked at being placed on 20 ~ 30 DEG C, taken out subsequently and centrifugal filtration, collecting precipitation to spend deionized water to pH be after 7.0, be placed on dry 20 ~ 24h in 70 ~ 75 DEG C of baking ovens, be prepared into pretreatment pomelo peel particle, finally by Chitosan powder and deionized water, be uniformly mixed by solid-liquid mass ratio 1:10, form chitin modified liquid, subsequently the pomelo peel particle of above-mentioned preparation is put into the Dewar bottle that volume is 1L, pass into nitrogen deaeration, after air is discharged completely, then detached by nitrogen in bottle, forming vacuum pressure is-0.05MPa, under negative pressure state, by pomelo peel particle and modified solution mass ratio 1:25, chitin modified liquid is added in Dewar bottle, ensures complete for pomelo peel particle submergence, treat submergence 10 ~ 15min, plasma modification device rf frequency is set, open radio-frequency power supply, add the discharge power of 200 ~ 300kw between outer electrode when processing, in process bottle, nitrogen forms plasma form, after plasma treatment 30 ~ 40min, removed and filtered, collect filter residue and spend deionized water 3 ~ 5 times, and being placed in the dry 10 ~ 12h of 70 ~ 80 DEG C of baking ovens, a kind of cross-linked chitosan modification pomelo peel can be prepared into and remove low-concentration heavy metal sorbing material in waste water.
Example 1
First count by weight, choose the shitosan of 45 parts respectively, the mass fraction of 15 parts is the methanol aqueous solution of 40%, the mass fraction of 20 parts is the benzaldehyde solution of 10% and the acetone of 20 parts, under temperature is 90 DEG C of water bath with thermostatic control conditions, reflux 1h in there-necked flask, after backflow completes, it is filtered, collect filter residue, by the filter residue of above-mentioned collection at temperature is 30 DEG C, be soak 48h in the hydrochloric acid solution of 4% at mass fraction, after benzaldehyde to be removed, 5min is soaked again by the NaOH solution of 0.5mol/L, after pickling alkali has soaked, adopt deionized water cyclic washing to be 7.0 to pH, be placed on dry 12h in 60 DEG C of baking ovens subsequently, be prepared into modification of chitosan particle, 1:10 in mass ratio again, be the aqueous acetic acid of 1% by the modification of chitosan particle of above-mentioned preparation and mass fraction, be uniformly mixed and dissolve completely to it, be prepared into chitosan gum lime set, 1:25 in mass ratio again, is added to epoxychloropropane in chitosan gel rubber, is uniformly mixed under 2800r/min, and drip mass fraction be 10% sodium hydroxide solution regulate its pH to be 9.5, reaction 15h, after question response completes, dropping mass concentration is that the hydrochloric acid solution of 1.25mol/L regulates its pH to be 7.0, subsequently filter cake is collected to its suction filtration, it is washed 5 times by deionized water, and be placed in 80 DEG C of dry 12h of baking oven, taken out subsequently and milled and sieved, be prepared into 200 order Chitosan powder for subsequent use, then fresh grapefruit skin is got, after respectively washing 5 times by running water and distilled water, constant weight is dried in 70 DEG C of baking ovens, subsequently it is freezingly milled and sieved, be prepared into 40 order pomelo peel particles, count by weight subsequently, choose the sodium hydroxide solution of the mass concentration 0.85mol/L of 55 parts respectively, the absolute ethyl alcohol of the pomelo peel particle of 5 parts and 40 parts, 12h is soaked at being placed on 30 DEG C, taken out subsequently and centrifugal filtration, collecting precipitation to spend deionized water to pH be after 7.0, be placed on dry 24h in 75 DEG C of baking ovens, be prepared into pretreatment pomelo peel particle, finally by Chitosan powder and deionized water, be uniformly mixed by solid-liquid mass ratio 1:10, form chitin modified liquid, subsequently the pomelo peel particle of above-mentioned preparation is put into the Dewar bottle that volume is 1L, pass into nitrogen deaeration, after air is discharged completely, then detached by nitrogen in bottle, forming vacuum pressure is-0.05MPa, under negative pressure state, by pomelo peel particle and modified solution mass ratio 1:25, chitin modified liquid is added in Dewar bottle, ensures complete for pomelo peel particle submergence, treat submergence 15min, plasma modification device rf frequency is set, open radio-frequency power supply, add the discharge power of 300kw between outer electrode when processing, in process bottle, nitrogen forms plasma form, after plasma treatment 40min, removed and filtered, collect filter residue and spend deionized water 5 times, and being placed in 80 DEG C of dry 10h of baking oven, a kind of cross-linked chitosan modification pomelo peel can be prepared into and remove low-concentration heavy metal sorbing material in waste water.Getting a 40mg cross-linked chitosan modification pomelo peel, to remove in waste water that low-concentration heavy metal sorbing material is carried on aperture be on the screen cloth of 17 μm, screen cloth is holded up and is placed in low concentration heavy metal water treatment pond, one is laid every 50cm, process 3h, the Mercury in Wastewater content 45mg/L of process of the present invention is down to 1mg/L, nickel content 40mg/L is down to 0.5 ~ 0.7mg/L, copper ion 35mg/L is down to 0.04 ~ 0.05mg/L, treatment effeciency is high, secondary pollution can not be produced, meet state sewage emission standard, can not secondary pollution be produced.
Example 2
First count by weight, choose the shitosan of 20 parts respectively, the mass fraction of 30 parts be the methanol aqueous solution of 40%, the mass fraction of 25 parts be 10% benzaldehyde solution and, the acetone of 25 parts, under temperature is 85 DEG C of water bath with thermostatic control conditions, reflux 1h in there-necked flask, after backflow completes, it is filtered, collect filter residue, by the filter residue of above-mentioned collection at temperature is 25 DEG C, be soak 48h in the hydrochloric acid solution of 4% at mass fraction, after benzaldehyde to be removed, 3min is soaked again by the NaOH solution of 0.5mol/L, after pickling alkali has soaked, adopt deionized water cyclic washing to be 7.0 to pH, be placed on dry 10h in 55 DEG C of baking ovens subsequently, be prepared into modification of chitosan particle, 1:10 in mass ratio again, be the aqueous acetic acid of 1% by the modification of chitosan particle of above-mentioned preparation and mass fraction, be uniformly mixed and dissolve completely to it, be prepared into chitosan gum lime set, 1:25 in mass ratio again, is added to epoxychloropropane in chitosan gel rubber, is uniformly mixed under 2600r/min, and drip mass fraction be 10% sodium hydroxide solution regulate its pH to be 8.5, reaction 10h, after question response completes, dropping mass concentration is that the hydrochloric acid solution of 1.25mol/L regulates its pH to be 7.0, subsequently filter cake is collected to its suction filtration, it is washed 3 times by deionized water, and be placed in 75 DEG C of dry 10h of baking oven, taken out subsequently and milled and sieved, be prepared into 180 order Chitosan powder for subsequent use, then fresh grapefruit skin is got, after respectively washing 3 times by running water and distilled water, constant weight is dried in 65 DEG C of baking ovens, subsequently it is freezingly milled and sieved, be prepared into 35 order pomelo peel particles, count by weight subsequently, choose the sodium hydroxide solution of the mass concentration 0.85mol/L of 30 parts respectively, the absolute ethyl alcohol of the pomelo peel particle of 10 parts and 60 parts, 12h is soaked at being placed on 30 DEG C, taken out subsequently and centrifugal filtration, collecting precipitation to spend deionized water to pH be after 7.0, be placed on dry 24h in 75 DEG C of baking ovens, be prepared into pretreatment pomelo peel particle, finally by Chitosan powder and deionized water, be uniformly mixed by solid-liquid mass ratio 1:10, form chitin modified liquid, subsequently the pomelo peel particle of above-mentioned preparation is put into the Dewar bottle that volume is 1L, pass into nitrogen deaeration, after air is discharged completely, then detached by nitrogen in bottle, forming vacuum pressure is-0.05MPa, under negative pressure state, by pomelo peel particle and modified solution mass ratio 1:25, chitin modified liquid is added in Dewar bottle, ensures complete for pomelo peel particle submergence, treat submergence 15min, plasma modification device rf frequency is set, open radio-frequency power supply, add the discharge power of 200kw between outer electrode when processing, in process bottle, nitrogen forms plasma form, after plasma treatment 30min, removed and filtered, collect filter residue and spend deionized water 3 times, and being placed in 70 DEG C of dry 10h of baking oven, a kind of cross-linked chitosan modification pomelo peel can be prepared into and remove low-concentration heavy metal sorbing material in waste water.Getting a kind of cross-linked chitosan modification pomelo peel that 20mg obtains, to remove in waste water that low-concentration heavy metal sorbing material is carried on aperture be on the screen cloth of 15 μm, screen cloth is holded up and is placed in low concentration heavy metal water treatment pond, one is laid every 40cm, process 1h, the Mercury in Wastewater content 40mg/L of process of the present invention is down to 0.5 ~ 1mg/L, nickel content 30mg/L is down to 0.5 ~ 0.7mg/L, copper ion 25mg/L is down to 0.04mg/L, treatment effeciency is high, secondary pollution can not be produced, meet state sewage emission standard, can not secondary pollution be produced.
Example 3
First count by weight, choose the shitosan of 40 parts respectively, the mass fraction of 20 parts is the methanol aqueous solution of 40%, the mass fraction of 20 parts is the benzaldehyde solution of 10% and the acetone of 20 parts, under temperature is 87 DEG C of water bath with thermostatic control conditions, reflux 1h in there-necked flask, after backflow completes, it is filtered, collect filter residue, by the filter residue of above-mentioned collection at temperature is 27 DEG C, be soak 48h in the hydrochloric acid solution of 4% at mass fraction, after benzaldehyde to be removed, 4min is soaked again by the NaOH solution of 0.5mol/L, after pickling alkali has soaked, adopt deionized water cyclic washing to be 7.0 to pH, be placed on dry 11h in 57 DEG C of baking ovens subsequently, be prepared into modification of chitosan particle, 1:10 in mass ratio again, be the aqueous acetic acid of 1% by the modification of chitosan particle of above-mentioned preparation and mass fraction, be uniformly mixed and dissolve completely to it, be prepared into chitosan gum lime set, 1:25 in mass ratio again, is added to epoxychloropropane in chitosan gel rubber, is uniformly mixed under 2600 ~ 2800r/min, and drip mass fraction be 10% sodium hydroxide solution regulate its pH to be 9.0, reaction 12h, after question response completes, dropping mass concentration is that the hydrochloric acid solution of 1.25mol/L regulates its pH to be 7.0, subsequently filter cake is collected to its suction filtration, it is washed 4 times by deionized water, and be placed in 77 DEG C of dry 11h of baking oven, taken out subsequently and milled and sieved, be prepared into 190 order Chitosan powder for subsequent use, then fresh grapefruit skin is got, after respectively washing 4 times by running water and distilled water, constant weight is dried in 67 DEG C of baking ovens, subsequently it is freezingly milled and sieved, be prepared into 37 order pomelo peel particles, count by weight subsequently, choose the sodium hydroxide solution of the mass concentration 0.85mol/L of 40 parts respectively, the absolute ethyl alcohol of the pomelo peel particle of 10 parts and 50 parts, 11h is soaked at being placed on 25 DEG C, taken out subsequently and centrifugal filtration, collecting precipitation to spend deionized water to pH be after 7.0, be placed on dry 22h in 72 DEG C of baking ovens, be prepared into pretreatment pomelo peel particle, finally by Chitosan powder and deionized water, be uniformly mixed by solid-liquid mass ratio 1:10, form chitin modified liquid, subsequently the pomelo peel particle of above-mentioned preparation is put into the Dewar bottle that volume is 1L, pass into nitrogen deaeration, after air is discharged completely, then detached by nitrogen in bottle, forming vacuum pressure is-0.05MPa, under negative pressure state, by pomelo peel particle and modified solution mass ratio 1:25, chitin modified liquid is added in Dewar bottle, ensures complete for pomelo peel particle submergence, treat submergence 12min, plasma modification device rf frequency is set, open radio-frequency power supply, add the discharge power of 250kw between outer electrode when processing, in process bottle, nitrogen forms plasma form, after plasma treatment 35min, removed and filtered, collect filter residue and spend deionized water 4 times, and being placed in 75 DEG C of dry 11h of baking oven, a kind of cross-linked chitosan modification pomelo peel can be prepared into and remove low-concentration heavy metal sorbing material in waste water.Getting a kind of cross-linked chitosan modification pomelo peel that 30mg obtains, to remove in waste water that low-concentration heavy metal sorbing material is carried on aperture be on the screen cloth of 16 μm, screen cloth is holded up and is placed in low concentration heavy metal water treatment pond, one is laid every 45cm, process 2h, the Mercury in Wastewater content 42mg/L of process of the present invention is down to 0.6mg/L, nickel content 35mg/L is down to 0.6mg/L, copper ion 30mg/L is down to 0.04mg/L, treatment effeciency is high, secondary pollution can not be produced, meet state sewage emission standard, can not secondary pollution be produced.
Claims (1)
1. cross-linked chitosan modification pomelo peel removes a preparation method for low-concentration heavy metal sorbing material in waste water, it is characterized in that concrete preparation process is:
(1) count by weight, choose the shitosan of 20 ~ 45 parts respectively, the mass fraction of 15 ~ 30 parts is the methanol aqueous solution of 40%, the mass fraction of 20 ~ 25 parts is the benzaldehyde solution of 10% and the acetone of 20 ~ 25 parts, under temperature is 85 ~ 90 DEG C of water bath with thermostatic control conditions, reflux 1h in there-necked flask, after backflow completes, it is filtered, collect filter residue;
(2) by the filter residue of above-mentioned collection at temperature is 25 ~ 30 DEG C, be soak 48h in the hydrochloric acid solution of 4% at mass fraction, after benzaldehyde to be removed, 3 ~ 5min is soaked again by the NaOH solution of 0.5mol/L, after pickling alkali has soaked, adopt deionized water cyclic washing to be 7.0 to pH, be placed on dry 10 ~ 12h in 55 ~ 60 DEG C of baking ovens subsequently, be prepared into modification of chitosan particle;
(3) 1:10 in mass ratio, be the aqueous acetic acid of 1% by the modification of chitosan particle of above-mentioned preparation and mass fraction, be uniformly mixed and dissolve completely to it, be prepared into chitosan gum lime set, 1:25 in mass ratio again, is added to epoxychloropropane in chitosan gel rubber, is uniformly mixed under 2600 ~ 2800r/min, and drip mass fraction be 10% sodium hydroxide solution regulate its pH to be 8.5 ~ 9.5, reaction 10 ~ 15h;
(4) after question response completes, dropping mass concentration is that the hydrochloric acid solution of 1.25mol/L regulates its pH to be 7.0, subsequently filter cake is collected to its suction filtration, by it by deionized water washing 3 ~ 5 times, and be placed in the dry 10 ~ 12h of 75 ~ 80 DEG C of baking ovens, taken out subsequently and milled and sieved, be prepared into 180 ~ 200 order Chitosan powder for subsequent use;
(5) fresh grapefruit skin is got, after respectively washing 3 ~ 5 times by running water and distilled water, constant weight is dried in 65 ~ 70 DEG C of baking ovens, subsequently it is freezingly milled and sieved, be prepared into 35 ~ 40 order pomelo peel particles, count by weight subsequently, choose the sodium hydroxide solution of the mass concentration 0.85mol/L of 30 ~ 55 parts respectively, the absolute ethyl alcohol of the pomelo peel particle of 5 ~ 10 parts and 40 ~ 60 parts, 10 ~ 12h is soaked at being placed on 20 ~ 30 DEG C, taken out subsequently and centrifugal filtration, collecting precipitation to spend deionized water to pH be after 7.0, be placed on dry 20 ~ 24h in 70 ~ 75 DEG C of baking ovens, be prepared into pretreatment pomelo peel particle,
(6) Chitosan powder prepared by step (4) and deionized water, be uniformly mixed by solid-liquid mass ratio 1:10, form chitin modified liquid, subsequently the pomelo peel particle of above-mentioned preparation is put into the Dewar bottle that volume is 1L, pass into nitrogen deaeration, after air is discharged completely, again nitrogen in bottle is detached, forming vacuum pressure is-0.05MPa, under negative pressure state, by pomelo peel particle and modified solution mass ratio 1:25, chitin modified liquid is added in Dewar bottle, ensures complete for pomelo peel particle submergence;
(7) submergence 10 ~ 15min is treated, plasma modification device rf frequency is set, open radio-frequency power supply, add the discharge power of 200 ~ 300kw between outer electrode when processing, in process bottle, nitrogen forms plasma form, after plasma treatment 30 ~ 40min, removed and filtered, collect filter residue and spend deionized water 3 ~ 5 times, and being placed in the dry 40 ~ 45h of 70 ~ 80 DEG C of baking ovens, a kind of cross-linked chitosan modification pomelo peel can be prepared into and remove low-concentration heavy metal sorbing material in waste water.
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| CN106179239A (en) * | 2016-07-12 | 2016-12-07 | 梁珑 | The preparation method and applications of pomelo peel modified amido functionalization adsorbent |
| CN107930595A (en) * | 2017-11-20 | 2018-04-20 | 成都新柯力化工科技有限公司 | A kind of porous modified pericarp gel and preparation method for lithium battery recycling |
| CN112516961A (en) * | 2020-11-09 | 2021-03-19 | 江西佳霖炭业科技有限公司 | Preparation method of coconut shell activated carbon with antibacterial function |
| CN114686332A (en) * | 2022-03-28 | 2022-07-01 | 山东工大食品科技有限公司 | Decolouring and impurity removing process for new Maotai-flavor liquor |
| CN114686332B (en) * | 2022-03-28 | 2024-01-23 | 山东工大食品科技有限公司 | Decoloring and impurity removing process for new Maotai-flavor white spirit |
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