CN103449558A - Method for adsorption treatment of cationic dye wastewater by using modified alkali residues - Google Patents
Method for adsorption treatment of cationic dye wastewater by using modified alkali residues Download PDFInfo
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- CN103449558A CN103449558A CN2013104070352A CN201310407035A CN103449558A CN 103449558 A CN103449558 A CN 103449558A CN 2013104070352 A CN2013104070352 A CN 2013104070352A CN 201310407035 A CN201310407035 A CN 201310407035A CN 103449558 A CN103449558 A CN 103449558A
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Abstract
The invention discloses a method for adsorption treatment of cationic dye wastewater by using modified alkali residues. The method comprises the following steps of (1) smashing the alkali residues into 20 to 40 meshes, washing with water, drying at the temperature of 80-105 DEG C, and grinding till powder can pass through a 100-140 mesh sieve, thus obtaining the alkali residue powder for standby application; (2) mixing the alkali residue powder and a sodium dodecyl sulfate solution with the critical micelle concentration (CMC) of 0.5-2 in a proportion of 5g/100mL, controlling the rotating speed at 160-180r/min at the temperature of 30-60 DEG C, vibrating for 6 to 12 hours, filtering obtained slurry so as to separate out solids, washing the solids, drying and grinding till the powder can pass through the 100-140 mesh sieve, thus obtaining an adsorbent for standby application; and (3) adding the adsorbent to the cationic dye wastewater in a proportion of 0.1-0.25g/100mL, controlling the temperature at 30-50 DEG C, and fully reacting for 5-360min, thus finishing the dye removal process, wherein the adsorption removal rate under the optimal condition can reach above 97%. The method can be used for solving the problems of high cost, long period, poor operational stability and the like in a conventional dye wastewater treatment method and recycling waste residues in ammonia base factories so as to achieve the effect of treating waste by waste.
Description
Technical field
The invention belongs to sewage disposal and industrial solid castoff resource utilization field, particularly utilize the method for surfactant-modified ammonia alkali factory waste residue as sorbent treatment cationic dyestuff waste water.
Background technology
Waste water from dyestuff is mainly derived from DYE PRODUCTION, dyestuff intermediate production and dyestuff and uses industry, its Production Flow Chart is long, product recovery rate is low, waste water has that complicated components is changeable, generation is large, COD concentration is high, colourity dark (extension rate can reach tens thousand of times), hazardous and noxious substances content is high, biodegradability is poor, dyestuff in waste water can absorb light, reduce water transparency, consume in a large number oxygen in water body, cause water hypoxia, destroying self purification of water body, is one of current unmanageable organic waste water.The treatment process of domestic contrast maturation has the treatment technologies such as biological activity sludge treatment method, physicochemical treatment method and membrane processing method at present, wherein, absorption method is owing to can not introducing new pollutent, energy consumption lower and can be from waste water the concentration and separation organic pollutant, thereby get more and more people's extensive concerning.For the selection of sorbent material, domestic existing a lot of research, such as gac, slag, wilkinite, flyash, zeolite, activated alumina etc.Although wherein the cost such as slag, flyash is low, its loading capacity is little, and required throwing ash amount is large; Although gac, zeolite have higher loading capacity, its price is relatively costly.
Alkaline residue is the waste residue produced in ammonia-soda process soda ash process.The current every production of " solvay soda process " technique 1t soda ash, need to discharge the solid alkaline residue 0.3t of water content 60% left and right.A large amount of alkaline residues can not get rational disposal and utilization for a long time, not only occupies a large amount of soils, and can cause the severe contamination of above and below ground, peripheral region, slag mountain, destroys the eubiosis.Its main component has: CaCO
3, CaCl
2, Mg (OH)
2, Fe
2o
3, Al
2o
3deng.At present, the main method of comprehensive utilization of alkaline residue comprises two aspects: the one, and for building engineering field, the raw material that can be used as material of construction is produced the building materials such as cement, brick; The 2nd, as chemical industry light industry raw material, through suitable technique, can make precipitated chalk, fume desulfurizing agent etc.(the journal of Shandong university such as Li Xia, 1672-3961 (2010) 02-0099-06) with dilute hydrochloric acid, alkaline residue is carried out to acidleach, metallic compound stripping by water-soluble in alkaline residue and indissoluble, make the alkaline residue leach liquor of the metal ions such as calcic, magnesium, and generate new looks oxyhydroxide under alkaline condition, as sorbent material adsorption treatment anionic dye waste water.The method takes full advantage of the advantage of the metal ions such as calcium, magnesium to pollutant removal, but the removal of dyestuff has very large dependency to pH, needs the scope of the strict pH of control, is unfavorable for the industrial applications of alkaline residue.
Summary of the invention
The object of the present invention is to provide and a kind ofly be applicable to the removal of waste water from dyestuff and take the ammonia alkali factory waste residue as starting material, the surface modifying method that the tensio-active agent of take is properties-correcting agent.Water outlet after present method is processed is hardly containing dye substance, and the alkaline residue surface of the adsorbing dyestuff dye substance of having combined closely, can not exist ecological risk to cause secondary pollution, and present method meets the environmental protection concept of the treatment of wastes with processes of wastes against one another.
The technical solution that realizes the object of the invention is:
A kind of method of utilizing modification alkaline residue adsorption treatment cationic dyestuff waste water, comprise the following steps:
(1) by alkaline residue fragmentation, washing, oven dry, levigate after, with surfactant soln, mix, the slurries that vibration obtains are separated by filtration out solid, after the solid washing is dried, grind and are screened to the order number needed, and obtain sorbent material;
(2) sorbent material is added in the reactor that cationic dyestuff waste water is housed;
(3) make the abundant hybrid reaction of sorbent material and waste water from dyestuff;
(4) sorbent material is separated to the water after finally being processed with the cationic dyestuff waste water solid.
Wherein, in step (1), alkaline residue is crushed to 20 ~ 40 orders, after washing, under 80 ~ 105 ℃, dries 24h, and grinding is screened to 100 ~ 140 orders and obtains sorbent material.
In step (1), tensio-active agent used is sodium lauryl sulphate, and the concentration of solution is 0.5 ~ 2CMC.
In step (1), the ratio of alkaline residue and sodium dodecyl sulfate solution is 5g/100mL.
In step (1), the hybrid reaction temperature is 30 ~ 60 ℃, and hunting speed is 160 ~ 180 r/min, and duration of oscillation is 6 ~ 12h.
In step (2), cationic dyestuff waste water adopts the methylene blue solution dye wastewater, and concentration is controlled at 20 ~ 30mg/L.
In step (2), the ratio that adds of sorbent material is 0.1 ~ 0.25g/100mL waste water.
In step (3), fully hybrid reaction is controlled temperature at 30～50 ℃, and the reaction times is 5～360min.
In step (4), solid-liquid separation adopts the method for centrifugation or filtration.
Principle of the present invention is: according to characterization test, the surface of alkaline residue is cellular, and specific surface area is about 31m
2/ g, have abundant adsorption site; The surface of alkaline residue is electronegativity, can electrostatic interaction Adsorption cationic dyestuff; Adopt the alkaline residue after surfactant-modified, before the wettability in solution and dispersiveness obviously are better than modification, can make alkaline residue and dyestuff fully act on; Alkaline residue after modification, the electronegativity on surface strengthens, and has then strengthened the interaction force between alkaline residue and dyestuff.
The present invention compared with prior art, its remarkable advantage is: according to the alkaline residue of modification of the present invention, before wettability in solution and dispersiveness obviously are better than modification, and the surface there is strong electronegativity, can well interact with dyestuff, compare unmodified alkaline residue, process the waste water of same concentration, at room temperature, need not change the pH of waste water from dyestuff, a small amount of sorbent material can reach desirable effect, can improve processing efficiency simultaneously.The present invention utilizes ammonia alkali factory alkaline residue, has not only realized the requirement of refuse " zero release " and " resource utilization ", and has obtained high dye decolored rate (the Wastewater Dyes percent of decolourization can reach more than 97%).New way has been opened up in the comprehensive utilization that the present invention is ammonia alkali factory alkaline residue, turns waste into wealth, and has opened up the potential value of environmental protection of alkaline residue, meets the environmental protection concept of the treatment of wastes with processes of wastes against one another, has Practical significance widely.
Below in conjunction with accompanying drawing, the present invention is described in further detail.
The accompanying drawing explanation
The graph of a relation of adsorption time and dye decolored rate in Fig. 1 embodiment of the present invention 1.
The graph of a relation of dosage and dye decolored rate in Fig. 2 embodiment of the present invention 1.
The graph of a relation of water inlet dye strength and dye decolored rate in Fig. 3 embodiment of the present invention 1.
Embodiment
The following examples can make the present invention of those skilled in the art comprehend.
A kind of method of utilizing modification alkaline residue adsorption treatment cationic dyestuff waste water, comprise the following steps:
(1) alkaline residue is crushed to 20 ~ 40 orders, after washing, under 80 ~ 105 ℃, dries 24h, be ground to 100 ~ 140 mesh sieves and obtain the alkaline residue powder, standby;
(2) the alkaline residue powder is mixed according to the ratio of 5g/100mL with 0.5 ~ 2CMC sodium dodecyl sulfate solution, at 30 ~ 60 ℃ of temperature, hunting speed is 160 ~ 180 r/min, duration of oscillation is 6 ~ 12h, the slurries that obtain are separated by filtration out solid, its washing oven dry were ground to 100～140 mesh sieves, obtained sorbent material, standby;
(3) sorbent material is added in cationic dyestuff waste water according to the ratio of 0.1 ~ 0.25g/100mL, controls temperature at 30～50 ℃, fully contact reacts 5～360min;
(4) adopt the method for centrifugation or filtration to realize solid-liquid separation.
Embodiment 1
In order to determine the top condition of alkaline residue absorption Wastewater Dyes, first with simulated wastewater, carry out the adsorption test of series of influence factors.Configure waste water from dyestuff with methylene blue, sorbent material is mixed with simulated wastewater, in the Erlenmeyer flask of packing into, in constant-temperature shaking incubator, vibrate, abundant hybrid reaction, reacted mud mixture, through the centrifuging and taking supernatant liquor, utilizes the concentration of dyestuff in the determined by ultraviolet spectrophotometry supernatant liquor.Percent of decolourization is calculated as follows:
Percent of decolourization (%)=(C
0-C)/C
0* 100%, C wherein
0for adsorbing the concentration of front solution, C is the concentration of the rear solution of absorption.
The experimental technique of each influence factor is as follows:
Adsorption time: the initial influent concentration of fixed dye waste water, the sorbent material dosage, the constant temperature oscillator rotating speed, pH, at room temperature, measure the absorption situation of different adsorption time sorbent materials to dyestuff, determines saturated adsorption time.
The sorbent material dosage: the initial influent concentration of fixed dye waste water, adsorption time, the constant temperature oscillator rotating speed, pH, at room temperature, change the sorbent material dosage, measures its impact on absorption.
The initial influent concentration of waste water from dyestuff: the fixed adsorbent dosage, adsorption time, the constant temperature oscillator rotating speed, pH, at room temperature, change initial influent concentration, measures its impact on absorption.
1. the configuration of the preparation of sorbent material and solution
Alkaline residue is crushed to 20 orders, dries under 105 ℃ after washing, be ground to 100 mesh sieves and obtain the alkaline residue powder; The alkaline residue powder is mixed according to the ratio of 5g/100mL with the 1CMC sodium dodecyl sulfate solution, and at 30 ℃ of temperature, hunting speed is 170 r/min, duration of oscillation is 6h, and the slurries that obtain are separated by filtration out solid, and its washing oven dry were ground to 100 mesh sieves, obtain sorbent material, standby.The dye solution that is 1000mg/L with the methylene blue configuration concentration is standby.
2. the impact of different affecting factors on dye decolored rate
(1) impact of adsorption time on dye decolored rate
Get the simulated wastewater 100mL that 10 parts of concentration are 20mg/L, in the Erlenmeyer flask with cover of packing into, add respectively the 0.2g sorbent material simultaneously, 30 ℃ of room temperatures, rotating speed is under 200r/min, adsorbs respectively 5min, 10min, 20min, 30min, 60min, 120min, 180min, 240min, 300min, the mixed solution after 360min is measured the concentration of dyestuff in filtrate after 0.45 μ m filter membrane.The speed of finding modification alkaline residue removal dyestuff is very fast, and in 5min, percent of decolourization reaches more than 90%.Reach balance after 60min, percent of decolourization is 98.18%.Under this condition, maximum adsorption capacity is 9.82mg/g.(shown in accompanying drawing 1)
(2) impact of sorbent material dosage on dye decolored rate
Getting 4 parts of concentration is 20mg/L, simulated wastewater 100mL, in the Erlenmeyer flask with cover of packing into, add respectively 0.1g simultaneously, 0.15g, 0.2g, the 0.25g sorbent material, 30 ℃ of room temperatures, rotating speed is under 200r/min, adsorption time 2h, and mixed solution is measured the concentration of dyestuff in filtrate after 0.45 μ m filter membrane.Discovery is along with the increase of dosage, and percent of decolourization increases, but amplification is little, and when dosage is 0.2g/100mL, the percent of decolourization of dyestuff has reached 98%.(shown in accompanying drawing 2)
(3) impact of the initial influent concentration of waste water from dyestuff on percent of decolourization
Get 6 parts of concentration and be respectively 20mg/L, 40mg/L, 60mg/L, 80mg/L, 100mg/L, 120mg/L, simulated wastewater 100mL, pack in Erlenmeyer flask with cover, add respectively the 0.2g sorbent material simultaneously, 30 ℃ of room temperatures, rotating speed is under 200r/min, adsorption time 2h, and mixed solution is measured the concentration of dyestuff in filtrate after 0.45 μ m filter membrane.Discovery is along with the increase of dyestuff starting point concentration, and loading capacity is also in continuous increase.(shown in accompanying drawing 3)
Embodiment 2
A kind of method of utilizing modification alkaline residue adsorption treatment cationic dyestuff waste water, comprise the following steps:
(1) alkaline residue is crushed to 40 orders, after washing, under 105 ℃, dries 24h, be ground to 100 mesh sieves and obtain the alkaline residue powder;
(2) the alkaline residue powder is mixed according to the ratio of 5g/100mL with the 0.8CMC sodium dodecyl sulfate solution, at 30 ℃ of temperature, hunting speed is 160r/min, duration of oscillation is 6h, the slurries that obtain are separated by filtration out solid, and its washing oven dry were ground to 100 mesh sieves, obtain sorbent material;
(3) by sorbent material, the ratio according to 0.1g/100mL is added in the waste water from dyestuff that concentration is 20mg/L, and the control rotating speed is 200r/min, controls temperature at 30 ℃, and fully, after contact reacts 2h, mixed solution is measured the concentration of dyestuff in supernatant liquor after centrifugation.The percent of decolourization of waste water from dyestuff is up to 88.21%.
Embodiment 3
(1) alkaline residue is crushed to 20 orders, after washing, under 80 ℃, dries 24h, be ground to 100 mesh sieves and obtain the alkaline residue powder;
(2) the alkaline residue powder is mixed according to the ratio of 5g/100mL with the 1CMC sodium dodecyl sulfate solution, under temperature 60 C, hunting speed is 170r/min, duration of oscillation is 12h, the slurries that obtain are separated by filtration out solid, and its washing oven dry were ground to 140 mesh sieves, obtain sorbent material;
(3) by sorbent material, the ratio according to 0.2g/100mL is added in the waste water from dyestuff that concentration is 30mg/L, and the control rotating speed is 200r/min, controls temperature at 50 ℃, and fully after contact reacts 2h, mixed solution is measured the concentration of dyestuff in filtrate after 0.45 μ m filter membrane.The percent of decolourization of waste water from dyestuff is up to 99.62%.
Embodiment 4
(1) alkaline residue is crushed to 20 orders, after washing, under 100 ℃, dries 24h, be ground to 100 mesh sieves and obtain the alkaline residue powder;
(2) the alkaline residue powder is mixed according to the ratio of 5g/100mL with the 0.5CMC sodium dodecyl sulfate solution, under temperature 60 C, hunting speed is 180r/min, duration of oscillation is 6h, the slurries that obtain are separated by filtration out solid, and its washing oven dry were ground to 100 mesh sieves, obtain sorbent material;
(3) by sorbent material, the ratio according to 0.2g/100mL is added in the waste water from dyestuff that concentration is 20mg/L, and the control rotating speed is 200r/min, controls temperature at 40 ℃, and fully after contact reacts 2h, mixed solution is measured the concentration of dyestuff in filtrate after 0.45 μ m filter membrane.The percent of decolourization of waste water from dyestuff is up to 94.97%.
Claims (9)
1. a method of utilizing modification alkaline residue adsorption treatment cationic dyestuff waste water, is characterized in that comprising the following steps:
(1) by alkaline residue fragmentation, washing, oven dry, levigate after, with surfactant soln, mix, the slurries that vibration obtains are separated by filtration out solid, after the solid washing is dried, grind and are screened to the order number needed, and obtain sorbent material;
(2) sorbent material is added in the reactor that cationic dyestuff waste water is housed;
(3) make the abundant hybrid reaction of sorbent material and waste water from dyestuff;
(4) sorbent material is separated to the water after finally being processed with the cationic dyestuff waste water solid.
2. method according to claim 1, it is characterized in that: in step (1), alkaline residue is crushed to 20 ~ 40 orders, after washing, under 80 ~ 105 ℃, dries 24h, grinds to be screened to 100 ~ 140 orders and to obtain sorbent material.
3. method according to claim 1, it is characterized in that: in step (1), tensio-active agent used is sodium lauryl sulphate, and the concentration of solution is 0.5 ~ 2CMC.
4. method according to claim 1, it is characterized in that: in step (1), the ratio of alkaline residue and sodium dodecyl sulfate solution is 5g/100mL.
5. method according to claim 1, it is characterized in that: in step (1), the hybrid reaction temperature is 30 ~ 60 ℃, and hunting speed is 160 ~ 180 r/min, and duration of oscillation is 6 ~ 12h.
6. method according to claim 1 is characterized in that: in step (2), cationic dyestuff waste water adopts the methylene blue solution dye wastewater, and concentration is controlled at 20 ~ 30mg/L.
7. method according to claim 1, it is characterized in that: in step (2), the ratio that adds of sorbent material is 0.1 ~ 0.25g/100mL(waste water).
8. method according to claim 1 is characterized in that: in step (3), fully hybrid reaction is controlled temperature at 30～50 ℃, and the reaction times is 5～360min.
9. method according to claim 1 is characterized in that: in step (4), solid-liquid separation adopts the method for centrifugation or filtration.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105585063A (en) * | 2014-10-22 | 2016-05-18 | 连云港中科博创科技有限公司 | A method of adsorbing nitrogen in waste water by utilizing modified caustic dross |
| CN106830250A (en) * | 2017-03-20 | 2017-06-13 | 合肥智慧龙图腾知识产权股份有限公司 | A kind of composite for dyeing and printing sewage treatment and its preparation method and application |
| CN108358371A (en) * | 2018-04-08 | 2018-08-03 | 哈尔滨工业大学（威海） | A kind of cationic dye wastewater separation method |
| CN109603744A (en) * | 2019-01-31 | 2019-04-12 | 中冶华天工程技术有限公司 | The modified useless brick of salt prepares the methods and applications of dyeing waste water adsorbent |
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2013
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US5389259A (en) * | 1992-08-24 | 1995-02-14 | Zimpro Environmental Inc. | Preparation treatment of volatile wastewater components |
| CN103241794A (en) * | 2013-05-17 | 2013-08-14 | 南京理工大学 | Method for removing phosphorus pollutants in sewage with modified alkali slag |
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|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105585063A (en) * | 2014-10-22 | 2016-05-18 | 连云港中科博创科技有限公司 | A method of adsorbing nitrogen in waste water by utilizing modified caustic dross |
| CN106830250A (en) * | 2017-03-20 | 2017-06-13 | 合肥智慧龙图腾知识产权股份有限公司 | A kind of composite for dyeing and printing sewage treatment and its preparation method and application |
| CN108358371A (en) * | 2018-04-08 | 2018-08-03 | 哈尔滨工业大学（威海） | A kind of cationic dye wastewater separation method |
| CN109603744A (en) * | 2019-01-31 | 2019-04-12 | 中冶华天工程技术有限公司 | The modified useless brick of salt prepares the methods and applications of dyeing waste water adsorbent |
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Inventor after: Sun Xiuyun Inventor after: Wang Lianjun Inventor after: Ma Fangbian Inventor after: Han Weiqing Inventor after: Li Jiansheng Inventor after: Shen Jinyou Inventor after: Liu Xiaodong Inventor after: Yan Yubo Inventor before: Sun Xiuyun Inventor before: Ma Bianfang Inventor before: Han Weiqing Inventor before: Li Jiansheng Inventor before: Shen Jinyou Inventor before: Liu Xiaodong Inventor before: Yan Yubo |
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Application publication date: 20131218 |