CN103447014A - Polyacrylic acid/13X molecular sieve adsorbent and method for preparing same - Google Patents
Polyacrylic acid/13X molecular sieve adsorbent and method for preparing same Download PDFInfo
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- CN103447014A CN103447014A CN2013104631408A CN201310463140A CN103447014A CN 103447014 A CN103447014 A CN 103447014A CN 2013104631408 A CN2013104631408 A CN 2013104631408A CN 201310463140 A CN201310463140 A CN 201310463140A CN 103447014 A CN103447014 A CN 103447014A
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Abstract
The invention relates to a polyacrylic acid/13X molecular sieve adsorbent and a method for preparing the polyacrylic acid/13X molecular sieve adsorbent. According to the technical scheme, the method for preparing the polyacrylic acid/13X molecular sieve adsorbent includes the steps of using a polyacrylic acid solution with the mass fraction of 13.5wt% and with the pH value ranging from 3.8 to 4.2 as a raw material, adding a 13X molecular sieve to the polyacrylic acid solution under the stirring condition to prepare mixed liquor of polyacrylic acid and the 13X modulator sieve, stirring the prepared mixed liquor of the polyacrylic acid and the 13X modulator sieve at the rotating speed ranging from 200r/min to 300r/min under the room temperature for 2 hours to 3 hours, then, directly placing the mixed liquor into a muffle furnace, roasting the stirred mixed liquor under the temperature ranging from 100 DEG C to 220 DEG C for 2 hours to 3 hours, and grinding the roasted mixed liquor into powder to prepare the polyacrylic acid/13X molecular sieve adsorbent. The method for preparing the polyacrylic acid/13X molecular sieve adsorbent is simple in procedure, the secondary pollution is not caused, and the prepared polyacrylic acid/13X molecular sieve adsorbent is large in grain diameter, can easily settle down, is good in adsorptive performance, and is suitable for processing waste water containing industrial basic dye.
Description
Technical field
The invention belongs to the adsorbent technical field.Relate in particular to a kind of polyacrylic acid/13X adsorbent of molecular sieve and preparation method thereof.
Background technology
The basic-dyeable fibre complicated component, colourity is high and toxicity is large, is one of major pollutants in China's water environment.The processing method of basic-dyeable fibre waste water is mainly activated sludge process, biomembrance process, photocatalytic method and physical-chemical process at present.Since entering the eighties, printing and dyeing industry neutral and alkali dyestuff adopts the polymer substance of difficult for biological degradation more, and the polymer substance biodegradability is poor, thereby activated sludge process and biomembrance process are restricted.Photocatalytic method because photochemical catalyst titanium dioxide exists that cost is high, poor heat stability, not responding to visible light and the defect that is difficult to separate, be restricted in actual applications.Physical-chemical process mainly contains absorption and the methods such as film separates, and the investment and the operating cost that due to film, separate are too high, therefore is difficult to apply on a large scale; Absorption method has been the method for extensive use in the basic-dyeable fibre wastewater treatment since 20 century 70s, though active carbon is wherein the most frequently used sorbing material, but exist, cost is high, charcoal absorption is easy to the problems such as saturated and regeneration difficulty, and the substitute products of therefore finding active carbon have received the concern of this area.
Solid material can make particle more disperse after surfactant-modified, and surface tension reduces, and surface electrical behavior changes, thereby absorption property is improved.J. the people such as Huang has studied attapulgite after surfactant OTAC (OTMAC) modification, surface is changed lipophile into by hydrophily, thereby increased absorption property (the J. Huang to organic pollution, X. Wang, Q. Jin, etal. Removal of phenol from aqueous solution by adsorption onto OTMAC-modified attapulgite. Journal of Environmental Management. 84 (2007) 229-236.), but OTMAC-attapulgite adsorbent adopts the wet method preparation, exist the use amount of modifier OTMAC large, and produce the shortcomings such as secondary pollution in preparation process.
Molecular sieve is the alumino-silicate of crystalline state, owing to thering is spacious skeleton structure, larger bug hole volume and a large amount of micropore uniformly, make its inside and outside there is very large specific area, can provide good adsorption reaction position for large molecule, but for processing some larger dye molecules in practical application, molecular sieve bore diameter is still large not, only depends on internal capillary can not reach the adsorption effect of expection.Molecular sieve is carried out to surface modification and can make the molecular sieve surface tension reduce, surface electrical behavior changes, thereby improves the absorption property of its surface to dye molecule.
Summary of the invention
The present invention is intended to overcome the prior art defect, and purpose is to provide that a kind of technique is simple, the preparation method of the polyacrylic acid of non-secondary pollution/13X adsorbent of molecular sieve; The polyacrylic acid prepared by the method/13X adsorbent of molecular sieve particle diameter is large, free settling, and absorption property is good, is applicable to the processing of industrial alkaline waste water from dyestuff.
To achieve these goals, the preparation process of the technical solution used in the present invention is:
Step 1, first prepare the polyacrylic acid solution that mass fraction is 13.5wt%, then regulate the pH value to 3.8 of polyacrylic acid solution ~ 4.2 with sodium hydroxide solution.
Step 3, the polyacrylic acid that makes/13X molecular sieve solution directly is placed in to Muffle furnace, under 100 ~ 220 ℃ of conditions, calcines 2 ~ 3h, be ground to powdery, make polyacrylic acid/13X adsorbent of molecular sieve.
Described polyacrylic acid solution is formulated by polyacrylic acid and distilled water.
Described sodium hydroxide solution is formulated by NaOH and distilled water.
Owing to adopting technique scheme, the present invention compared with prior art has following good effect:
It is primary raw material that polyacrylic acid and 13X molecular sieve are take in the present invention, add the 13X molecular sieve in the polyacrylic acid solution that is 3.8 ~ 4.2 to the pH value under stirring condition, make the mixed liquor of polyacrylic acid and 13X molecular sieve, again the mixed liquor of polyacrylic acid and 13X molecular sieve is stirred to 2 ~ 3h with the rotating speed of 200 ~ 300r/min at ambient temperature, then directly be placed in Muffle furnace and calcine 2 ~ 3h under 100 ~ 220 ℃ of conditions, be ground to powdery, make the adsorbent of processing basic-dyeable fibre waste water, therefore technique is simple.
Polyacrylic acid prepared by the present invention/13X adsorbent of molecular sieve adopts semidry method, with the existing wet method for preparing adsorbent, with dry method, compare, because preparing adsorbent, wet method can produce secondary pollution, the shortcoming of the adsorbent uneven components that dry method makes, therefore the present invention does not only produce secondary pollution, and the adsorbent composition is even.
Polyacrylic acid prepared by the present invention/13X adsorbent of molecular sieve, because polyacrylic acid is surperficial electronegative anion surfactant, therefore the surface negative charge that with polyacrylic acid, the 13X molecular sieve is carried out to the polyacrylic acid that makes after modification/13X adsorbent of molecular sieve increases, and the basic-dyeable fibre of effects on surface positively charged has absorption property preferably.Polyacrylic acid/13X adsorbent of molecular sieve granularity is large, is easy to separate from water, therefore can be by its recycling.
Polyacrylic acid prepared by the present invention/13X adsorbent of molecular sieve is compared with the 13X molecular sieve, the 13X sieve particle mainly is the octahedral bodily form, adhesion is arranged more, it is the typical crystal habit of X-type molecular sieve, and the part particle of the polyacrylic acid of preparation/13X adsorbent of molecular sieve manifests clustering phenomena, form larger particle, the meso-position radius of polyacrylic acid/13X adsorbent of molecular sieve is 15.817um, the meso-position radius of 13X molecular sieve is 4.506um, therefore in water after adsorpting dye molecule polyacrylic acid/13X adsorbent of molecular sieve be easier to sedimentation.In polyacrylic acid/13X adsorbent of molecular sieve, the crystal structure of 13X molecular sieve subsides, and forms amorphous state.
Therefore, technique of the present invention simply and not produces secondary pollution, and prepared polyacrylic acid/13X adsorbent of molecular sieve particle diameter is large, free settling, and absorption property is good, is applicable to industrial alkaline dye wastewater treatment.
The accompanying drawing explanation
The SEM figure that Fig. 1 is the 13X molecular sieve;
The SEM figure that Fig. 2 is a kind of polyacrylic acid of preparing of the present invention/13X adsorbent of molecular sieve;
The particle size distribution figure that Fig. 3 is the 13X molecular sieve shown in the another kind of polyacrylic acid for preparing of the present invention/13X adsorbent of molecular sieve and Fig. 1;
The X-diffraction pattern that Fig. 4 is the 13X molecular sieve shown in another polyacrylic acid of preparing of the present invention/13X adsorbent of molecular sieve and Fig. 1.
The specific embodiment
Below in conjunction with the specific embodiment and accompanying drawing, the invention will be further described, not to the restriction of its protection domain:
embodiment 1
A kind of polyacrylic acid/13X adsorbent of molecular sieve and preparation method thereof.The concrete steps of its preparation method are:
Step 1, first prepare the polyacrylic acid solution that mass fraction is 13.5wt%, then regulate the pH value to 3.8 of polyacrylic acid solution ~ 4.0 with sodium hydroxide solution.
Step 3, the polyacrylic acid that makes/13X molecular sieve solution directly is placed in to Muffle furnace, under 100 ~ 150 ℃ of conditions, calcines 2.5 ~ 3h, be ground to powdery, make polyacrylic acid/13X adsorbent of molecular sieve.
Carry out adsorption treatment with the alkaline bright yellow waste water from dyestuff that the prepared polyacrylic acid of the present embodiment/the 13X adsorbent of molecular sieve is 30mg/L to concentration, under the condition that is 30min at speed of agitator that described polyacrylic acid/13X adsorbent of molecular sieve dosage is 0.2g/L, 200r/min and adsorption time, the light yellow clearance of described waste water from dyestuff neutral and alkali is 89.0%.
A kind of polyacrylic acid/13X adsorbent of molecular sieve and preparation method thereof.The concrete steps of its preparation method are:
Step 1, first prepare the polyacrylic acid solution that mass fraction is 13.5wt%, then regulate the pH value to 3.8 of polyacrylic acid solution ~ 4.0 with sodium hydroxide solution.
Step 3, the polyacrylic acid that makes/13X molecular sieve solution directly is placed in to Muffle furnace, under 150 ~ 220 ℃ of conditions, calcines 2 ~ 2.5h, be ground to powdery, make polyacrylic acid/13X adsorbent of molecular sieve.
Carry out adsorption treatment with the methylene blue dye waste water that the prepared polyacrylic acid of the present embodiment/the 13X adsorbent of molecular sieve is 30mg/L to concentration, under the condition that is 30min at speed of agitator that described polyacrylic acid/13X adsorbent of molecular sieve dosage is 0.2g/L, 250r/min and adsorption time, the clearance of described waste water from dyestuff Methylene Blue is 93.8%.
embodiment 3
A kind of polyacrylic acid/13X adsorbent of molecular sieve and preparation method thereof.The concrete steps of its preparation method are:
Step 1, first prepare the polyacrylic acid solution that mass fraction is 13.5wt%, then regulate the pH value to 4.0 of polyacrylic acid solution ~ 4.2 with sodium hydroxide solution.
Step 3, the polyacrylic acid that makes/13X molecular sieve solution directly is placed in to Muffle furnace, under 100 ~ 150 ℃ of conditions, calcines 2.5 ~ 3h, be ground to powdery, make polyacrylic acid/13X adsorbent of molecular sieve.
Carry out adsorption treatment with the peacock green waste water from dyestuff that the prepared polyacrylic acid of the present embodiment/the 13X adsorbent of molecular sieve is 30mg/L to concentration, under the condition that is 30min at speed of agitator that described polyacrylic acid/13X adsorbent of molecular sieve dosage is 0.2g/L, 150r/min and adsorption time, the clearance of described waste water from dyestuff Malachite Green is 88.4%.
A kind of polyacrylic acid/13X adsorbent of molecular sieve and preparation method thereof.The concrete steps of its preparation method are:
Step 1, first prepare the polyacrylic acid solution that mass fraction is 13.5wt%, then regulate the pH value to 4.0 of polyacrylic acid solution ~ 4.2 with sodium hydroxide solution.
Step 3, the polyacrylic acid that makes/13X molecular sieve solution directly is placed in to Muffle furnace, under 150 ~ 220 ℃ of conditions, calcines 2 ~ 2.5h, be ground to powdery, make polyacrylic acid/13X adsorbent of molecular sieve.
Carry out adsorption treatment with the peacock green waste water from dyestuff that the prepared polyacrylic acid of the present embodiment/the 13X adsorbent of molecular sieve is 50mg/L to concentration, under the condition that is 30min at speed of agitator that described polyacrylic acid/13X adsorbent of molecular sieve dosage is 0.3g/L, 200r/min and adsorption time, the clearance of described waste water from dyestuff Malachite Green is 89.1%.
It is primary raw material that this specific embodiment be take polyacrylic acid and 13X molecular sieve, add the 13X molecular sieve in the polyacrylic acid solution that is 3.8 ~ 4.2 to the pH value under stirring condition, make the mixed liquor of polyacrylic acid and 13X molecular sieve, again the mixed liquor of polyacrylic acid and 13X molecular sieve is stirred to 2 ~ 3h with the rotating speed of 200 ~ 300r/min at ambient temperature, then directly be placed in Muffle furnace and calcine 2 ~ 3h under 100 ~ 220 ℃ of conditions, be ground to powdery, make the adsorbent of processing basic-dyeable fibre waste water, therefore technique is simple.
Polyacrylic acid prepared by this specific embodiment/13X adsorbent of molecular sieve adopts semidry method, with the existing wet method for preparing adsorbent, with dry method, compare, because preparing adsorbent, wet method can produce secondary pollution, the shortcoming of the adsorbent uneven components that dry method makes, therefore this specific embodiment does not only produce secondary pollution, and the adsorbent composition is even.
Polyacrylic acid prepared by this specific embodiment/13X adsorbent of molecular sieve, because polyacrylic acid is surperficial electronegative anion surfactant, therefore the surface negative charge that with polyacrylic acid, the 13X molecular sieve is carried out to the polyacrylic acid that makes after modification/13X adsorbent of molecular sieve increases, and the basic-dyeable fibre of effects on surface positively charged has absorption property preferably.Polyacrylic acid/13X adsorbent of molecular sieve granularity is large, is easy to separate from water, therefore can be by its recycling.
The SEM figure that Fig. 1 is the 13X molecular sieve can find out that the 13X sieve particle mainly is the octahedral bodily form, and adhesion is arranged more, is the typical crystal habit of X-type molecular sieve.Fig. 2 is the prepared polyacrylic acid of embodiment 1/13X adsorbent of molecular sieve, can find out, its part particle presents clustering phenomena, forms larger particle, therefore in water after adsorpting dye molecule polyacrylic acid/13X adsorbent of molecular sieve be easier to sedimentation.The meso-position radius of the prepared polyacrylic acid of the embodiment 2 shown in Fig. 3/13X adsorbent of molecular sieve is 15.817um, and the meso-position radius of 13X molecular sieve is 4.506um, the particle size that further illustrates polyacrylic acid/13X adsorbent of molecular sieve becomes large, free settling more during adsorpting dye molecule in water.The prepared polyacrylic acid of embodiment 3 shown in Fig. 4/13X adsorbent of molecular sieve is compared with the 1 3X molecular sieve with sharp-pointed crystal diffraction peak, the X-diffraction pattern is without diffraction maximum, explanation crystalline phase after polyacrylic acid modified has changed amorphous state into, and original crystal structure subsides.
Therefore, this specific embodiment technique simply and not produces secondary pollution, and prepared polyacrylic acid/13X adsorbent of molecular sieve particle diameter is large, free settling, and absorption property is good, is applicable to industrial alkaline dye wastewater treatment.
Claims (4)
1. the preparation method of polyacrylic acid/13X adsorbent of molecular sieve is characterized in that described preparation method is:
Step 1, first prepare the polyacrylic acid solution that mass fraction is 13.5wt%, then regulate the pH value to 3.8 of polyacrylic acid solution ~ 4.2 with sodium hydroxide solution;
Step 2, under stirring condition, in the polyacrylic acid solution of regulating after pH value, add the 13X molecular sieve, the 13X molecular sieve addition that every rising tune saves the polyacrylic acid solution after the pH value is 55 ~ 60g, obtains the mixed liquor of polyacrylic acid and 13X molecular sieve; Again the mixed liquor of polyacrylic acid and 13X molecular sieve is stirred to 2 ~ 3h with the rotating speed of 200 ~ 300r/min at ambient temperature, make polyacrylic acid/13X molecular sieve solution;
Step 3, the polyacrylic acid that makes/13X molecular sieve solution directly is placed in to Muffle furnace, under 100 ~ 220 ℃ of conditions, calcines 2 ~ 3h, be ground to powdery, make polyacrylic acid/13X adsorbent of molecular sieve.
2. the preparation method of polyacrylic acid/13X adsorbent of molecular sieve according to claim 1, is characterized in that described polyacrylic acid solution is formulated by polyacrylic acid and distilled water.
3. the preparation method of polyacrylic acid/13X adsorbent of molecular sieve according to claim 1, is characterized in that described sodium hydroxide solution is formulated by NaOH and distilled water.
4. polyacrylic acid/13X adsorbent of molecular sieve, is characterized in that described polyacrylic acid/13X adsorbent of molecular sieve is the polyacrylic acid prepared according to the preparation method of the described polyacrylic acid of any one/13X adsorbent of molecular sieve in claim 1 ~ 3/13X adsorbent of molecular sieve.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104907053A (en) * | 2015-05-12 | 2015-09-16 | 安徽鑫昆净化设备有限公司 | Composite adsorbent and preparation method thereof |
| WO2024021342A1 (en) * | 2022-07-29 | 2024-02-01 | 正大能源材料(大连)有限公司 | Adsorbent, and preparation method therefor and use thereof |
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| JP2012250211A (en) * | 2011-06-06 | 2012-12-20 | Dainichiseika Color & Chem Mfg Co Ltd | Adsorbent composition, adsorbent, and method for applying the same |
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Patent Citations (4)
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| US20050281734A1 (en) * | 2002-08-12 | 2005-12-22 | Postech Foundation | Method for manufacturing mesoporous alumina molecular sieve and alumina nanotube and use of the alumina nanotube for storage of h2 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104907053A (en) * | 2015-05-12 | 2015-09-16 | 安徽鑫昆净化设备有限公司 | Composite adsorbent and preparation method thereof |
| WO2024021342A1 (en) * | 2022-07-29 | 2024-02-01 | 正大能源材料(大连)有限公司 | Adsorbent, and preparation method therefor and use thereof |
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