CN105219393A - The preparation method of lignin modification heavy metal deactivator - Google Patents
The preparation method of lignin modification heavy metal deactivator Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of lignin modification heavy metal deactivator, the method comprises the following steps: (11) are by wiring solution-forming soluble in water for a certain amount of xylogen, and regulator solution is to acid; (2) add iron protochloride and hydrogen peroxide successively by a certain percentage, leave standstill after reacting by heating for some time; (3) adjust solution to alkalescence, after add a certain amount of diethylenetriamine and formaldehyde successively, to stir, and reacting by heating for some time; (4) reaction drips hydrochloric acid soln product is fully separated out after terminating under whipped state, leaves standstill, obtains amination modifying xylogen after suction filtration; (5) wash unreacted medicament with water, after product is dried, grinding, namely obtain xylogen amination modifying heavy metal deactivator finished product.The inventive method technique is simple, production cost is low, excellent performance, applied widely, and the passivation repair process and the heavy metal ion-containing waste water that are adapted to all kinds of heavy-metal pollution soil adsorb, During Coagulation Process.
Description
Technical field
The present invention relates to heavy metal pollution of soil passivation treatment technology field, particularly a kind of preparation method utilizing xylogen amination modifying to prepare heavy metal deactivator.
Background technology
Along with industry developments such as mining, smelting, lead storage battery, leather, chemical industry, " three wastes " containing heavy metal enter into edatope by all means, cause serious pollution to soil.Heavy metal contamination has the advantages that pollution range is wide, the time length long, pollute disguise, cannot be biodegradable, not only larger harm is produced to the seed output and quality of farm crop, and pass through the continuous enrichment of transmission of food chain, the finally health risk at people's body accumulation.The national soil investigation publication issued according to Chinese Ministry of Environmental Protection in 2014, Ministry of Land and Resources is pointed out, the soil gross contamination exceeding standard rate of investigated in China 6,300,000 square kilometres is 16.1%, main based on inorganic pollutants such as cadmium, mercury, arsenic, copper, lead, chromium, zinc, nickel, points of contamination figure place accounts for 82.8% of all super punctuation bits.Current, heavy metal-polluted soil administering method conventional both at home and abroad mainly contains peripheral doses, chemical redemption and biological restoration three kinds of methods.Peripheral doses method comprises soil moved in improve the original displacement, deep ploughing is digged, and chemical repair method comprises passivation reparation, Soil leaching etc., and biological renovation method comprises animal reparation, plant extract etc.Wherein, passivation restoration of soil polluted by heavy metal have with low cost, repairing efficiency is short, the feature such as easy to implement, the conditional request that current China heavy-metal contaminated soil is repaired can be met well, be particularly useful for repairing big area mild or moderate heavy metal contamination agricultural land soil.
Current existing soil heavy metal passivant can be divided into following two classes: (1) mineral-type, comprises lime, ferrous sulfate, phosphoric acid salt (hydroxyapatite, phosphate fertilizer etc.), industrial by-product category (red mud, flying dust, rhombspar residue etc.), clay mineral class (zeolite, attapulgite, sepiolite, wilkinite etc.) etc.; (2) organic, comprise organic compost, stalk, municipal sludge, feces of livestock and poultry and synthesis chelating type organic etc.Wherein, organic passivator has increases soil fertility and convenience of drawing materials, economic advantage, has great importance in heavy metal pollution of soil reparation.Research shows, xylogen and modified product to soil free of toxic effects, non-secondary pollution.Meanwhile, xylogen has low biological degradability, and the soil ulmin that degraded produces has stronger heavy metal adsorption equally, therefore, is that Material synthesis soil heavy metal passivant has unique advantage in long-lasting with xylogen.In addition, xylogen is the main component of pulping and paper-making waste liquid, is one of pulp and paper industry major source material causing environmental pollution, the added value that soil heavy metal passivant not only can improve xylogen prepared by lignin modification, also can reduce the pollution of environment, turn waste into wealth.
Ge is round proposes the preparation method preparing lignin-base dithiocarbamate(s) heavy metal ion trapping agent using xylogen as raw material in the patent of invention of publication number CN102784622A, application number 201210248082.2, but prepared by this trapping agent desired reaction temperature is higher, the reaction times is longer, step is more, and efficiency is lower.Meanwhile, adopt in this trapping agent preparation process and there is more supervirulent dithiocarbonic anhydride not only high requirement is proposed to production technique as raw materials for production, and can work the mischief and risk to producers, surrounding enviroment.Zhao Tao, Pan Hong propose with alkali lignin and epoxy chloropropane for raw material synthesizing epoxy xylogen under certain condition in the patent of invention of publication number CN103408767A, application number 201310317674.X, and this epoxy lignin derivative and polyamine compounds are reacted the preparation method preparing aminated lignin.But this preparation method fails the modified sites of xylogen fully to expose, modification efficiency is lower, and properties-correcting agent only adopts diamine compounds, and the binding site of heavy metal is less.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of lignin modification heavy metal deactivator, with the xylogen in papermaking wastewater for main component, be not only the new way of the comprehensive utilization developing of trade waste, and can greatly reduce heavy-metal contaminated soil treatment cost.
The present invention solves the problems of the technologies described above with following technical scheme:
The preparation method of lignin modification heavy metal deactivator of the present invention, comprises the following steps:
The first step, take a certain amount of xylogen and be added to the water and be made into the lignin liquor that mass concentration is 2-10%, stirring regulator solution pH value after 0.5 hour is 3.5,
Second step, adds iron protochloride successively and mass concentration is the hydrogen peroxide of 30%, reacts after 1 hour and leave standstill 0.5 hour at 50 DEG C,
3rd step, adjustment solution ph is 9.5, then adds diethylenetriamine and formaldehyde successively, stirs, and is heated to 50-80 DEG C of reaction 1-4 hour,
4th step, under whipped state, dripping mass concentration after reaction terminates is that 10% hydrochloric acid soln regulates the pH value of above-mentioned reaction soln to be 7.0, and modified xylogen is fully separated out, and leaves standstill suction filtration after 2-3 hour, obtains amination modifying xylogen,
5th step, washes unreacted diethylenetriamine and formaldehyde with water, after product is dried 6 hours at 50 DEG C, be ground to below 100 orders, namely obtain xylogen amination modifying heavy metal deactivator finished product.
Described xylogen extracts from papermaking wastewater, obtains alkali lignin or sulfonated lignin by acid adding sedimentation and filtration.
Hydrogen peroxide and lignin liquor described in preparation process second step are 1 ︰ 200 by volume, and iron protochloride adds ratio according to iron ion and H
2o
2mass ratio is 1 ︰ 4-7.
Described in preparation process the 3rd step, the mass ratio of xylogen and diethylenetriamine is 1 ︰ 0.75-1.5.
Described in preparation process the 3rd step, the mol ratio of diethylenetriamine and formaldehyde is 1 ︰ 0.5-3.
The inventive method tool has the following advantages:
1) xylogen adopted is the main component of pulping and paper-making waste liquid, the added value that soil heavy metal passivant not only can improve xylogen prepared by lignin modification, also can reduce the pollution of environment, turn waste into wealth.
2) xylogen is carried out diethylenetriamine modification by the present invention, obtains aminated lignin, and its synthetic method is simple, and reaction conditions is gentleer, workable.Obtained heavy metal deactivator is neutral, and to soil free of toxic effects, non-secondary pollution, stable in properties, has very strong heavy metal adsorption, passivation ability.
3) passivating agent products that the present invention produces has wide range of applications, and not only can be used for heavy metal-polluted soil passivation, also can be used as heavy metal in water sorbent material.
Embodiment
Below in conjunction with specific embodiment, the inventive method is further described.
Embodiment 1
The preparation method of lignin modification heavy metal deactivator, operation steps is as follows:
The first step, takes 4.0g alkali lignin and adds in 200mL distilled water, stirs 0.5 hour, by hydrochloric acid conditioning solution pH value to 3.5,
Second step, adds iron protochloride successively and 1mL mass concentration is the hydrogen peroxide of 30%, and the dosage of iron protochloride presses m (Fe
2+): m (H
2o
2)=1 ︰ 4 adds, and reacts after 1 hour and leave standstill 0.5 hour at 50 DEG C,
3rd step, by NaOH solution regulator solution pH value to 9.5, adds the diethylenetriamine of 5g, then is that 1:0.5 adds 0.024mol formaldehyde by the mol ratio of diethylenetriamine and formaldehyde, stirs, and keeps solution 80 DEG C of reactions 1 hour,
4th step, reaction terminate after drip under whipped state mass concentration be 10% hydrochloric acid soln regulate the pH value of above-mentioned reaction soln to be 7.0, modified xylogen is fully separated out, leave standstill suction filtration after 2 hours, unreacted diethylenetriamine and formaldehyde is washed away with deionized water, after product is dried 6 hours at 50 DEG C, be ground to below 100 orders, namely obtain xylogen amination modifying heavy metal deactivator finished product.
The xylogen amination modified product nitrogen content of gained is 4.05%.
Embodiment 2
The preparation method of lignin modification heavy metal deactivator, operation steps is as follows:
The first step, takes 10.0g alkali lignin and adds in 200mL distilled water, stirs 0.5 hour, by hydrochloric acid conditioning solution pH value to 3.5,
Second step, adds iron protochloride successively and 1mL mass concentration is the hydrogen peroxide of 30%, and the dosage of iron protochloride presses m (Fe
2+): m (H
2o
2)=1 ︰ 6 adds, and reacts after 1 hour and leave standstill 0.5 hour at 50 DEG C,
3rd step, by NaOH solution regulator solution pH value to 9.5, adds 10g diethylenetriamine, then is that 1:3 adds 0.29mol formaldehyde by the mol ratio of diethylenetriamine and formaldehyde, stirs, and keeps solution 70 DEG C of reactions 3 hours,
4th step, reaction terminate after drip under whipped state mass concentration be 10% hydrochloric acid soln regulate the pH value of above-mentioned reaction soln to be 7.0, modified xylogen is fully separated out, leave standstill suction filtration after 2 hours, unreacted diethylenetriamine and formaldehyde is washed away with deionized water, after product is dried 6 hours at 50 DEG C, be ground to below 100 orders, namely obtain xylogen amination modifying heavy metal deactivator finished product.
The xylogen amination modified product nitrogen content of gained is 7.00%.
Embodiment 3
The preparation method of lignin modification heavy metal deactivator, operation steps is as follows:
The first step, takes 20.0g alkali lignin and adds in 200mL distilled water, stirs 0.5 hour, by hydrochloric acid conditioning solution pH value to 3.5,
Second step, adds iron protochloride successively and 1mL mass concentration is the hydrogen peroxide of 30%, and the dosage of iron protochloride presses m (Fe
2+): m (H
2o
2)=1 ︰ 7 adds, and reacts after 1 hour and leave standstill 0.5 hour at 50 DEG C,
3rd step, by NaOH solution regulator solution pH value to 9.5, adds 15g diethylenetriamine, then is that 1:2 adds 0.29mol formaldehyde by the mol ratio of diethylenetriamine and formaldehyde, stirs, and keeps solution 50 DEG C of reactions 4 hours,
4th step, reaction terminate after drip under whipped state mass concentration be 10% hydrochloric acid soln regulate the pH value of above-mentioned reaction soln to be 7.0, modified xylogen is fully separated out, leave standstill suction filtration after 3 hours, unreacted diethylenetriamine and formaldehyde is washed away with deionized water, after product is dried 6 hours at 50 DEG C, be ground to below 100 orders, namely obtain xylogen amination modifying heavy metal deactivator finished product.
The xylogen amination modified product nitrogen content of gained is 5.34%.
Embodiment 4
The preparation method of lignin modification heavy metal deactivator, step is as follows:
The first step, takes 16.0g sodium lignosulfonate and adds in 200mL distilled water, stirs 0.5 hour, by hydrochloric acid conditioning solution pH value to 3.5,
Second step, adds iron protochloride successively and 1mL mass concentration is the hydrogen peroxide of 30%, and the dosage of iron protochloride presses m (Fe
2+): m (H
2o
2)=1:5 adds, and reacts after 1 hour and leave standstill 0.5 hour at 50 DEG C,
3rd step, by NaOH solution regulator solution pH value to 9.5, adds 24g diethylenetriamine, then is that 1 ︰ 1 adds 0.23mol formaldehyde by the mol ratio of diethylenetriamine and formaldehyde, stirs, and keeps solution 60 DEG C of reactions 2 hours,
4th step, reaction terminate after drip under whipped state mass concentration be 10% hydrochloric acid soln regulate the pH value of above-mentioned reaction soln to be 7.0, modified xylogen is fully separated out, leave standstill suction filtration after 2 hours, unreacted diethylenetriamine and formaldehyde is washed away with deionized water, after product is dried 6 hours at 50 DEG C, be ground to below 100 orders, namely obtain xylogen amination modifying heavy metal deactivator finished product.
The xylogen amination modified product nitrogen content of gained is 3.88%.
Test example 1
Modified product heavy metal passivation ability is passed judgment on heavy metal amount of capacity in xylogen amination modifying heavy metal deactivator finished product adsorption aqueous solution of the present invention.In embodiment 1, amination modifying heavy metal deactivator finished product is to Cu in solution
2+, Pb
2+, Cd
2+, Zn
2+saturated extent of adsorption be respectively 10.48mg/g, 58.91mg/g, 25.13mg/g, 16.17mg/g.In embodiment 2, amination modifying heavy metal deactivator finished product is to Cu in solution
2+, Pb
2+, Cd
2+, Zn
2+saturated extent of adsorption be respectively 23.73mg/g, 76.62mg/g, 31.69mg/g, 21.85mg/g.In embodiment 3, amination modifying heavy metal deactivator finished product is to Cu in solution
2+, Pb
2+, Cd
2+, Zn
2+saturated extent of adsorption be respectively 12.40mg/g, 15.12mg/g, 19.52mg/g, 14.64mg/g.In embodiment 4, amination modifying heavy metal deactivator finished product is to Cu in solution
2+, Pb
2+, Cd
2+, Zn
2+saturated extent of adsorption be respectively 12.365mg/g, 18.84mg/g, 10.70mg/g, 5.71mg/g.Contrast Zhou Yan " environmental engineering journal " in October, 2013 deliver " aminated lignin to water in Cu (II), Cd (II) absorption " in literary composition aminated lignin to Cu
2+, Cd
2+loading capacity 6.2mg/g and 7.1mg/g there is significant advantage.
Test example 2
Cultivate to obtain analog composite heavy-metal contaminated soil, its heavy metal concentration is cadmium 21.51mg/g, plumbous 1968.85mg/g, zinc 2175.63mg/g, copper 1353.43mg/g.Get 10g air-dry simulation heavy-metal contaminated soil sample and be placed in the clean beaker of 250mL, the dosage of xylogen amination modifying heavy metal deactivator finished product of the present invention is soil quality 5%, guarantees that the water ratio of soil is 30%, stirs, maintenance 14 days.After 14 days, get the soil after reparation, adopt the toxicity leaching method of HJ/299-2007 and the Acid extractable of BCR method to determine the effect of passivator.Cadmium concentration reduction by 47.40% after interpolation passivator in toxicity leach liquor, lead concentration reduction by 79.31%, zinc concentration reduction by 62.36%, copper concentration reduce by 95.90%, the cadmium concentration reduction by 3.97% in Acid extractable, lead concentration reduction by 19.51%, zinc concentration reduction by 23.60%, copper concentration reduction by 28.76%.
Claims (5)
1. the preparation method of lignin modification heavy metal deactivator, is characterized in that, comprises the following steps:
The first step, take a certain amount of xylogen and be added to the water and be made into the lignin liquor that mass concentration is 2-10%, stirring regulator solution pH value after 0.5 hour is 3.5,
Second step, adds iron protochloride successively and mass concentration is the hydrogen peroxide of 30%, reacts after 1 hour and leave standstill 0.5 hour at 50 DEG C,
3rd step, adjustment solution ph is 9.5, then adds diethylenetriamine and formaldehyde successively, stirs, and is heated to 50-80 DEG C of reaction 1-4 hour,
4th step, under whipped state, dripping mass concentration after reaction terminates is that 10% hydrochloric acid soln regulates the pH value of above-mentioned reaction soln to be 7.0, and modified xylogen is fully separated out, and leaves standstill suction filtration after 2-3 hour, obtains amination modifying xylogen,
5th step, washes unreacted diethylenetriamine and formaldehyde with water, after product is dried 6 hours at 50 DEG C, be ground to below 100 orders, namely obtain xylogen amination modifying heavy metal deactivator finished product.
2. lignin modification heavy metal deactivator preparation method according to claim 1, is characterized in that: described xylogen extracts from papermaking wastewater, obtains alkali lignin or sulfonated lignin by acid adding sedimentation and filtration.
3. lignin modification heavy metal deactivator preparation method according to claim 1, is characterized in that: hydrogen peroxide and lignin liquor described in preparation process second step are 1 ︰ 200 by volume, and iron protochloride adds ratio according to iron ion and H
2o
2mass ratio is 1 ︰ 4-7.
4. lignin modification heavy metal deactivator preparation method according to claim 1, is characterized in that: described in preparation process the 3rd step, the mass ratio of xylogen and diethylenetriamine is 1 ︰ 0.75-1.5.
5. lignin modification heavy metal deactivator preparation method according to claim 1, is characterized in that: described in preparation process the 3rd step, the mol ratio of diethylenetriamine and formaldehyde is 1 ︰ 0.5-3.
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Inventor after: Wang Shuangfei Inventor after: Liu Ni Inventor after: Zhu Hongxiang Inventor after: Qin Cheng Rong Inventor after: Liu Xinliang Inventor before: Liu Ni Inventor before: Wang Shuangfei Inventor before: Zhu Hongxiang Inventor before: Qin Cheng Rong Inventor before: Liu Xinliang |