CN104815619A - Oilseed rape straw/hydrotalcite composite material and preparation method and application thereof - Google Patents
Oilseed rape straw/hydrotalcite composite material and preparation method and application thereof Download PDFInfo
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- CN104815619A CN104815619A CN201510219127.7A CN201510219127A CN104815619A CN 104815619 A CN104815619 A CN 104815619A CN 201510219127 A CN201510219127 A CN 201510219127A CN 104815619 A CN104815619 A CN 104815619A
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- hydrotalcite
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Abstract
The invention relates to an oilseed rape straw/hydrotalcite composite material and a preparation method and application on water treatment aspect. Oilseed rape straws are added into NaOH solution in batches, magnetic stirring is performed to form even oilseed rape straw suspension liquid; hydrotalcite and distilled water are added into a container and stirred, then the oilseed rape straw suspension liquid is slowly added, centrifugal separation is performed after heating reaction, finally distilled water is used for flushing till the neutral situation is achieved, grinding and screening are performed after vacuum drying, and the oilseed rape straw/hydrotalcite composite material is prepared. The oilseed rape straw/hydrotalcite composite material has the advantages that the adopted raw materials, namely the hydrotalcite and the straws are natural materials and are low in price and wide in sources, the composite material prepared by utilizing the hydrotalcite and the straws is simple in process and is also an environment-friendly material, the efficient removal effect is achieved, waste water treatment efficiency is high, handling efficiency can be higher than 90%, and the oilseed rape straw/hydrotalcite composite material is low in cost, convenient to operate and easy to apply widely.
Description
Technical field
The invention belongs to water-treatment technology field, be specifically related to a kind of rape stalk/hydrotalcite composite material and preparation method thereof and the application in water treatment.
Background technology
In recent years, along with the increasing of china natural resources using degree, each Big Lakes eutrophication is day by day serious.Ecosystem degradation, wawter bloom frequently break out, and have a strong impact on the productive life of the mankind, and this becomes the great environmental problem of restriction Chinese society and national sustained economic development.
Phosphorus is the main polluted factors causing body eutrophication, and in eutrophication water, phosphorus pollution sources mainly enter the phosphorus of water body in outside (agricultural fertilizer, phosphorus-containing wastewater discharge beyond standards etc.).In common phosphorus removing method, what be most widely used is the physical-chemical process that process equipment is simple, disposal cost is low.Absorption method wherein based on environment mineral material is considered to one of effective administering method.Mineral material because of its wide material sources, to be cheaply easy to get, to regenerate easily, can to repeatedly use and the feature such as non-secondary pollution, in phosphorus treatment research, be subject to extensive concern.
Containing large humic acid in natural drink water, to plant kingdom, the animal kingdom, or even the mankind create impact.For in the acid-treated method of humic, active carbon adsorption fortune is with the most use.But remove merely the DeGrain of humic acid with charcoal absorption, active carbon adsorption has carried out improving or achieving good effect with other method of coupling by many experts.But separately should in this way, the removal of humic acid is unsatisfactory, and the binding operation with other technique is complicated, will consider whether active carbon can regenerate simultaneously.Therefore consider to adopt the agricultural crop straw absorption humic acid without carbonization, realize the efficient of humic acid and the removal of low cost.
Summary of the invention
The object of the invention is to provide a kind of rape stalk/hydrotalcite composite material and preparation method thereof, and its preparation technology is simple, and the composite of low in raw material price, it can either have efficient dephosphorization and humic acid can ensure environment friendly again.
For achieving the above object, the present invention adopts technical scheme as follows: a kind of preparation method of rape stalk/hydrotalcite composite material, includes following steps: rape stalk is added NaOH solution in batches, magnetic agitation, forms uniform rape stalk suspension; Add in container by hydrotalcite and distilled water, slowly add rape stalk suspension after stirring, centrifugation after temperature reaction, be finally washed till neutrality with distilled water, grinding is sieved after vacuum drying, prepares rape stalk/hydrotalcite composite material.
By such scheme, the mass fraction of described NaOH solution is 10 ~ 30%.
By such scheme, the mass ratio of described rape stalk and hydrotalcite is 0.6 ~ 1.4.
By such scheme, described in add the rape stalk magnetic agitation time be 20 ~ 40min.
By such scheme, described in the mixing time added after hydrotalcite and distilled water be 20 ~ 40min.
By such scheme, described temperature reaction temperature is 50 ~ 70 DEG C, and the reaction time is 4 ~ 8h.
By such scheme, described bake out temperature is 100 ~ 110 DEG C.
The application of above-mentioned rape stalk/hydrotalcite composite material in water treatment.
The present invention utilizes stalk/hydrotalcite composite material Phosphate Sorption and humic acid, makes composite efficient dephosphorization and humic acid can ensure again the environment friendly of material under field conditions (factors).This technology achieves the fully effectively utilization of natural mineral resource and agricultural stalk, for the removal of phosphorus in water body and humic acid provides new principle and method.
Beneficial effect of the present invention:
The raw material hydrotalcite that the present invention is used and stalk are natural materials, cheap, and wide material sources, utilize the composite that it is prepared, and process is simple, is again environmental friendliness shaped material; The present invention utilizes the suction-operated of hydrotalcite and stalk to remove phosphorus in water body and humic acid, reaches efficient removal effect; Have employed a kind of innovative approach-solution intercalation composite algorithm, prepare a kind of dephosphorization and the pretty good rape stalk/hydrotalcite composite material of humic acid effect; Administer sewage, treatment effeciency is high, and treatment effeciency can reach more than 90%, and cost is low, easy to operate, and is easy to extensive enforcement.
Accompanying drawing explanation
Fig. 1 is the XRD figure of embodiment 3 stalks/hydrotalcite composite material;
Fig. 2 is that embodiment 3 stalks/hydrotalcite composite material FTIR schemes;
Fig. 3 is the removal effect of embodiment 3 stalks/hydrotalcite composite material to phosphorus;
Fig. 4 is that embodiment 3 stalks/hydrotalcite composite material is to humic acid removal effect.
Detailed description of the invention
Following examples explain technical scheme of the present invention further, but not as limiting the scope of the invention.
The preparation of embodiment 1 stalk/hydrotalcite composite material
Be that 0.6:1 prepares composite by rape stalk and hydrotalcite mass ratio.Rape stalk is added in batches the NaOH solution of 120mL12% (mass fraction), magnetic agitation 0.5h, form uniform rape stalk suspension.Hydrotalcite and 120mL distilled water are added there-necked flask, rape stalk suspension is slowly added after stirring (500r/min) 0.5h, be warming up to 50 DEG C, centrifugation after reaction 6h, finally be washed till neutrality with distilled water, after 105 DEG C of vacuum drying 5h, ground 200 mesh sieves, prepare rape stalk/hydrotalcite composite material.
Embodiment 2
Be that 0.8:1 prepares composite by rape stalk and hydrotalcite mass ratio.Rape stalk is added in batches the NaOH solution of 120mL16% (mass fraction), magnetic agitation 0.5h, form uniform rape stalk suspension.Hydrotalcite and 120mL distilled water are added in there-necked flask, rape stalk suspension is slowly added after stirring (500r/min) 0.5h, be warming up to 55 DEG C, centrifugation after reaction 6h, finally be washed till neutrality with distilled water, after 105 DEG C of vacuum drying 5h, ground 200 mesh sieves, prepare rape stalk/hydrotalcite composite material.
Embodiment 3
Be that 1:1 prepares composite by rape stalk and hydrotalcite mass ratio.Rape stalk is added in batches the NaOH solution of 120mL20% (mass fraction), magnetic agitation 0.5h, form uniform rape stalk suspension.Hydrotalcite and 120mL distilled water are added in there-necked flask, rape stalk suspension is slowly added after stirring (500r/min) 0.5h, be warming up to 60 DEG C, centrifugation after reaction 6h, finally be washed till neutrality with distilled water, after 105 DEG C of vacuum drying 5h, ground 200 mesh sieves, prepare rape stalk/hydrotalcite composite material.
Shown in accompanying drawing 1, the XRD figure of the present embodiment stalk/hydrotalcite composite material.As seen from the figure, be positioned at 2 θ=22.97 °, 2 θ=34.80 °, 2 θ=43.10 ° and 2 θ=62.39 ° absworption peak be the characteristic absorption peak of hydrotalcite.The characteristic absorption peak of rape stalk is positioned at 2 θ=22.21 °.After rape stalk and hydrotalcite compound, 2 θ=22.21 °, the disappearance of 2 θ=30.73 ° these diffraction maximums illustrates that rape stalk and hydrotalcite there occurs interaction.
Shown in accompanying drawing 2, the present embodiment stalk/hydrotalcite composite material FTIR schemes.From hydrotalcite collection of illustrative plates, wave number is 3473cm
-1the absworption peak of place's correspondence is O-H stretching vibration peak, and wave number is 1638cm
-1for H-O-H flexural vibrations peak in hydrone, be positioned at 1372cm
-1the absworption peak of place's correspondence is hydrotalcite layers CO
3 2-anion vibrates.After hydrotalcite is combined with rape stalk, obvious change can be observed from the FTIR figure of its composite.Collection of illustrative plates shows 3452cm
-1the peak at place is to 3459cm
-1direction is moved, and peak shape broadens, and shows that hydrogen bond action is strengthened.In addition, 1056cm is positioned at
-1peak disappear, at 487cm
-1having there is new peak in place, illustrates and there occurs interaction between rape stalk and hydrotalcite.
Preparation, containing the potassium dihydrogen phosphate of variable concentrations, after adding composite, shakes up, is put in constant-temperature table, set temperature, rotating speed and time.Regular sampling, after the centrifugal 3min of 12000r/min, gets certain volume supernatant in colorimetric cylinder, measures the concentration of phosphorus in solution according to ammonium molybdate spectrophotometric method (GB/T11893-1989).Arrange simultaneously one do not add the blank sample similarity condition of stalk/hydrotalcite composite material under carry out Experimental comparison.Result shows, along with the carrying out in processing time, the concentration of potassium dihydrogen phosphate constantly reduces, composite to the maximum material removal rate of phosphorus up to 90%.With reference to shown in accompanying drawing 3, the present embodiment stalk/hydrotalcite composite material is to the removal effect of phosphorus.
Preparation, containing the humic acid solution of variable concentrations, after adding material, shakes up, is put in constant-temperature table, set temperature, rotating speed and time.Regular sampling, after the centrifugal 3min of 12000r/min, get certain volume supernatant in colorimetric cylinder, the sample according to getting different time sections carries out centrifugal, get the value that supernatant carries out measuring UV254 in quartz colorimetric utensil again, and from calibration curve, calculate the actual concentrations of HA.Result shows, after photocatalysis 175min, humic acid degradation rate reaches 70%, and therefore stalk/hydrotalcite composite material all has good absorption property to humic acid.
In stalk/hydrotalcite composite material dephosphorization process, total hardness and Al levels in solution before and after reaction are measured.Result shows, stalk/hydrotalcite composite material on total hardness in solution and Al levels without impact.
Embodiment 4
Be that 1.2:1 prepares composite by rape stalk and hydrotalcite mass ratio.Rape stalk is added in batches the NaOH solution of 120mL24% (mass fraction), magnetic agitation 0.5h, form uniform rape stalk suspension.Hydrotalcite and 120mL distilled water are added in there-necked flask, rape stalk suspension is slowly added after stirring (500r/min) 0.5h, be warming up to 65 DEG C, centrifugation after reaction 6h, finally be washed till neutrality with distilled water, after 105 DEG C of vacuum drying 5h, ground 200 mesh sieves, prepare rape stalk/hydrotalcite composite material.
Embodiment 5
Be that 1.4:1 prepares composite by rape stalk and hydrotalcite mass ratio.Rape stalk is added in batches the NaOH solution of 120mL28% (mass fraction), magnetic agitation 0.5h, form uniform rape stalk suspension.Hydrotalcite and 120mL distilled water are added in there-necked flask, rape stalk suspension is slowly added after stirring (500r/min) 0.5h, be warming up to 70 DEG C, centrifugation after reaction 6h, finally be washed till neutrality with distilled water, after 105 DEG C of vacuum drying 5h, ground 200 mesh sieves, prepare rape stalk/hydrotalcite composite material.
The concrete data of embodiment 1-5 performance characterization see the following form:
Different stalk/the hydrotalcite composite material of table 1 is to the removal effect of various pollutant
| Phosphorus | Humic acid | |
| Embodiment 1 | 94 | 76 |
| Embodiment 2 | 92 | 75 |
| Embodiment 3 | 90 | 74 |
| Embodiment 4 | 88 | 73 |
| Embodiment 5 | 86 | 69 |
Claims (9)
1. a preparation method for rape stalk/hydrotalcite composite material, includes following steps: rape stalk is added NaOH solution in batches, magnetic agitation, forms uniform rape stalk suspension; Add in container by hydrotalcite and distilled water, slowly add rape stalk suspension after stirring, centrifugation after temperature reaction, be finally washed till neutrality with distilled water, grinding is sieved after vacuum drying, prepares rape stalk/hydrotalcite composite material.
2. the preparation method of rape stalk/hydrotalcite composite material according to claim 1, is characterized in that the mass fraction of described NaOH solution is 10 ~ 30%.
3. the preparation method of rape stalk/hydrotalcite composite material according to claim 1, is characterized in that the mass ratio of described rape stalk and hydrotalcite is 0.6 ~ 1.4.
4. the preparation method of rape stalk/hydrotalcite composite material according to claim 1, adding the rape stalk magnetic agitation time described in it is characterized in that is 20 ~ 40min.
5. the preparation method of rape stalk/hydrotalcite composite material according to claim 1, the mixing time added described in it is characterized in that after hydrotalcite and distilled water is 20 ~ 40min.
6. the preparation method of rape stalk/hydrotalcite composite material according to claim 1, it is characterized in that described temperature reaction temperature is 50 ~ 70 DEG C, the reaction time is 4 ~ 8h.
7. the preparation method of rape stalk/hydrotalcite composite material according to claim 1, is characterized in that described bake out temperature is 100 ~ 110 DEG C.
8. rape stalk/the hydrotalcite composite material of any one of claim 1 ~ 7 preparation method gained.
9. the application of rape stalk/hydrotalcite composite material according to claim 8 in water treatment.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105170072A (en) * | 2015-09-30 | 2015-12-23 | 太仓碧奇新材料研发有限公司 | Preparation method of wheat straw and hydrotalcite composite material capable of adsorbing cobalt ions in electroplating water |
| CN105170096A (en) * | 2015-09-30 | 2015-12-23 | 太仓碧奇新材料研发有限公司 | Preparation method of sisal and talc powder composite for enriching europium ions in tailing wastewater |
| CN105251451A (en) * | 2015-09-30 | 2016-01-20 | 太仓碧奇新材料研发有限公司 | Preparing method for biomass composite for removing basic green in printing and dyeing wastewater |
| CN105585064A (en) * | 2015-09-30 | 2016-05-18 | 太仓碧奇新材料研发有限公司 | Preparation method for sulfonated coal composite material capable of enriching lanthanum ions in tailing wastewater |
| CN108404874A (en) * | 2018-02-11 | 2018-08-17 | 华南理工大学 | A kind of plant fiber/LDHs sorbing materials and preparation method and application |
| CN108675420A (en) * | 2018-05-23 | 2018-10-19 | 沈阳建筑大学 | A kind of stalk, the compound method for preparing magnetic flocculant of charcoal |
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| CN102614851A (en) * | 2012-04-09 | 2012-08-01 | 西北师范大学 | Preparation of palygorskite clay/plant stalk composite adsorbent and application of composite adsorbent in treating printing and dyeing wastewater |
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| US6632363B1 (en) * | 2001-05-02 | 2003-10-14 | Grotek, Inc. | Hydrophobic compositions and methods of use in water applications |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105170072A (en) * | 2015-09-30 | 2015-12-23 | 太仓碧奇新材料研发有限公司 | Preparation method of wheat straw and hydrotalcite composite material capable of adsorbing cobalt ions in electroplating water |
| CN105170096A (en) * | 2015-09-30 | 2015-12-23 | 太仓碧奇新材料研发有限公司 | Preparation method of sisal and talc powder composite for enriching europium ions in tailing wastewater |
| CN105251451A (en) * | 2015-09-30 | 2016-01-20 | 太仓碧奇新材料研发有限公司 | Preparing method for biomass composite for removing basic green in printing and dyeing wastewater |
| CN105585064A (en) * | 2015-09-30 | 2016-05-18 | 太仓碧奇新材料研发有限公司 | Preparation method for sulfonated coal composite material capable of enriching lanthanum ions in tailing wastewater |
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| CN105585064B (en) * | 2015-09-30 | 2018-02-06 | 太仓碧奇新材料研发有限公司 | The preparation method of the sulfonated coal composite of lanthanum ion in a kind of enrichment mine tailing wastewater |
| CN108404874A (en) * | 2018-02-11 | 2018-08-17 | 华南理工大学 | A kind of plant fiber/LDHs sorbing materials and preparation method and application |
| CN108675420A (en) * | 2018-05-23 | 2018-10-19 | 沈阳建筑大学 | A kind of stalk, the compound method for preparing magnetic flocculant of charcoal |
| CN108675420B (en) * | 2018-05-23 | 2022-05-10 | 沈阳建筑大学 | Method for preparing magnetic flocculant by compounding straw and biochar |
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