CN104014299A - Particulate attapulgite adsorbent and preparation method thereof - Google Patents
Particulate attapulgite adsorbent and preparation method thereof Download PDFInfo
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- CN104014299A CN104014299A CN201410288153.0A CN201410288153A CN104014299A CN 104014299 A CN104014299 A CN 104014299A CN 201410288153 A CN201410288153 A CN 201410288153A CN 104014299 A CN104014299 A CN 104014299A
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Abstract
The invention relates to a particulate attapulgite adsorbent and a preparation method thereof. According to the technical scheme, the preparation method comprises the following steps: uniformly mixing water and attapulgite powder to obtain mud attapulgite, wherein are in the mass ratio of the water to the attapulgite powder is 1 to (0.5-1); drying the prepared mud attapulgite for 8 to 16 hours at 90 to 110 DEG C; crushing dried mud attapulgite to the particulate attapulgite with the particle size being 0.045 to 1.25 mm; calcining the prepared particulate attapulgite for 2 to 3 hours at 650 to 750 DEG C in a Muffle furnace to prepare the particulate attapulgite adsorbent. According to the particulate attapulgite adsorbent and the preparation method thereof, the process is simple; secondary pollution is avoided; the prepared particulate attapulgite adsorbent has the characteristics of large particle, easiness in sedimentation, easiness in recycling and high adsorption performance, and is applicable to industrial heavy metal cationic wastewater treatment.
Description
Technical field
The invention belongs to adsorbent technical field.Relate in particular to a kind of granular concave rod earth adsorbing and preparation method thereof.
Background technology
Effluent containing heavy metal ions is one of the world today's three large water environment pollution modes, after these effluent containing heavy metal ions entered environments, can not be biodegradable, in water body, run up to certain limit and will produce serious harm to water body one water plant one aquatic animal system, and can have influence on by food chain mankind itself's health.Existing heavy metal processing method mainly comprises the methods such as chemical precipitation, solvent extraction, ion-exchange, film separation, activated carbon and silica gel absorption, wherein chemical precipitation method is most widely used, but for low concentration wastewater, employing chemical precipitation method exists and invests greatly, operating cost is high and easily produce the problem of secondary pollution.And absorption method is because its material is cheaply easy to get, cost is low and the good research emphasis that becomes of removal effect, the most frequently used adsorbent is active carbon at present both at home and abroad, but active carbon exists, cost is high, absorption is easy to the saturated and difficult problem of regenerating, and the substitute products of therefore finding active carbon have received the concern of this area.
Attapulgite is as a kind of natural material, have advantages of that raw material cheapness, aboundresources and specific area are large, attapulgite has special fibre structure and crystal structure, makes it to have many special materializations and processing performance, has the good reputation of " kings of thousand soil " and " soil of general-purpose ".Because attapulgite has larger specific area, make it have stronger suction-operated, under quite low concentration, can form full-bodied suspension, its rheological property has determined that it can be used as dytory, suspending agent, thixotropic agent and binding agent (Hu Tao, Qian Yunhua. the application study of attapulgite [J]. Chinese Mining Industry, 2005,14 (10), 73).But there is the problem that is difficult for precipitation, is easy to cause secondary pollution in attapulgite powder in water.Improvement attapulgite character has received those skilled in the art's concern.
At present the method for modifying of solid material is mainly, through surfactant, it is carried out to surface modification, its surface electrical behavior is changed, thereby change its absorption property, but surfactant is soluble in water, causes secondary pollution.The people such as Huang Jianhua have studied with OTAC attapulgite modified, improve the hydrophobicity of attapulgite, thereby have increased the absorption property (Huang Jianhua to Organic Pollution, Wang Xingguo, the people such as Jin Qingzhe, ultrasonically-modified OTMAC-attapulgite adsorbing phenol, water technology, 2005,31(9), 61-64), but the preparation technology of OTMAC-attapulgite adsorbent is accompanied by Organic Pollution, the adsorbent of preparation is powder, is difficult to reclaim after absorption.
Summary of the invention
The present invention is intended to overcome prior art defect, and object is to provide that a kind of technique is simple, the preparation method of the granular concave rod earth adsorbing of non-secondary pollution with low cost; The granular concave rod earth adsorbing particle diameter of preparing by the method greatly, free settling reclaims and absorption property is good, is applicable to the processing of industrial heavy metal cation waste water.
To achieve these goals, the preparation method of the technical solution used in the present invention is:
Step 1, water is mixed with attapulgite powder, the mass ratio of water and attapulgite powder is 1 ︰ 0.5 ~ 1, makes mud shape attapulgite;
Step 2, by the mud shape attapulgite making dry 8 ~ 16h under 90 ~ 110 ℃ of conditions, being crushed to particle diameter is the granular concave rod soil of 0.45 ~ 1.25mm;
Step 3, then the granular concave rod soil making is placed in to Muffle furnace, under 650 ~ 750 ℃ of conditions, calcines 2 ~ 3h, make granular concave rod earth adsorbing.
The particle diameter of described attapulgite powder is for being less than 76 μ m.
Owing to adopting technique scheme, the present invention compared with prior art has following good effect:
The present invention be take attapulgite powder as raw material, water is mixed with attapulgite powder, the mass ratio of water and attapulgite powder is 1 ︰ 0.5 ~ 1, make mud shape attapulgite, then by the mud shape attapulgite making dry 8 ~ 16h under 90 ~ 110 ℃ of conditions, take out dried block attapulgite, be crushed to the particle that particle diameter is 0.45 ~ 1.25mm, then under 650 ~ 750 ℃ of conditions, calcine 2 ~ 3h, make the granular concave rod earth adsorbing of processing heavy metal cation waste water, therefore technique is simple.
The advantages such as attapulgite powder aboundresources used in the present invention, raw material cheapness, therefore the granular concave rod earth adsorbing cost making in the present invention is low.
Granular concave rod earth adsorbing prepared by the present invention, due to the high-temperature calcination through 650 ~ 750 ℃, granule strength is high, and specific area is large, has produced calcium, the magnesium plasma of capacitive simultaneously, produces OH in solution
-make solution alkalize, thereby can make heavy metal cation precipitate and separate out.
Granular concave rod earth adsorbing prepared by the present invention, particle diameter is 0.45 ~ 1.25mm.Because particle diameter is easy to greatly separation from water, adsorption capacity is large, and in the waste residue after absorption, content of beary metal is 10-50wt%, can be used for smelting heavy metal, produces secondary benefit.
Therefore, technique of the present invention simply and not produces secondary pollution, and prepared granular concave rod earth adsorbing has that particle diameter is large, free settling, easily reclaim and the good feature of absorption property, is applicable to industrial heavy metal cation wastewater treatment.
Accompanying drawing explanation
Fig. 1 is the SEM figure of a kind of granular concave rod earth adsorbing of preparing of the present invention;
Fig. 2 is the infrared spectrum comparison diagram of the granular concave rod earth adsorbing shown in Fig. 1 and attapulgite powder.
The specific embodiment
Below in conjunction with the specific embodiment and accompanying drawing, the invention will be further described, not the restriction to its protection domain:
The particle diameter of the attapulgite powder described in this specific embodiment, for being less than 76 μ m, repeats no more in embodiment.
embodiment 1
A kind of granular concave rod earth adsorbing and preparation method thereof.The concrete steps of its preparation method are:
Step 1, water is mixed with attapulgite powder, the mass ratio of water and attapulgite powder is 1 ︰ 0.5 ~ 0.7, makes mud shape attapulgite;
Step 2, by the mud shape attapulgite making dry 12 ~ 16h under 90 ~ 100 ℃ of conditions, being crushed to particle diameter is the granular concave rod soil of 0.45 ~ 1.25mm;
Step 3, then the granular concave rod soil making is placed in to Muffle furnace, under 650 ~ 700 ℃ of conditions, calcines 2.5 ~ 3h, make granular concave rod earth adsorbing.
With the prepared attapulgite adsorbent of the present embodiment 1, to concentration, be 20mg/L containing Pb
2+waste water carries out adsorption treatment, under the condition that the speed of agitator that is 1g/L, 250r/min at described granular concave rod earth adsorbing dosage and adsorption time are 2h, described containing Pb
2+pb in waste water
2+clearance be 95%.
embodiment 2
A kind of granular concave rod earth adsorbing and preparation method thereof.The concrete steps of its preparation method are:
Step 1, water is mixed with attapulgite powder, the mass ratio of water and attapulgite powder is 1 ︰ 0.6 ~ 0.8, makes mud shape attapulgite;
Step 2, by the mud shape attapulgite making dry 12 ~ 16h under 90 ~ 100 ℃ of conditions, being crushed to particle diameter is the granular concave rod soil of 0.45 ~ 1.25mm;
Step 3, then the granular concave rod soil making is placed in to Muffle furnace, under 650 ~ 700 ℃ of conditions, calcines 2.5 ~ 3h, make granular concave rod earth adsorbing.
With the prepared attapulgite adsorbent of the present embodiment 2, to concentration, be 20mg/L containing Cu
2+waste water carries out adsorption treatment, under the condition that the speed of agitator that is 1g/L, 250r/min at described granular concave rod earth adsorbing dosage and adsorption time are 2h, described containing Cu
2+cu in waste water
2+clearance be 96%.
embodiment 3
A kind of granular concave rod earth adsorbing and preparation method thereof.The concrete steps of its preparation method are:
Step 1, water is mixed with attapulgite powder, the mass ratio of water and attapulgite powder is 1 ︰ 0.7 ~ 0.9, makes mud shape attapulgite;
Step 2, by the mud shape attapulgite making dry 8 ~ 12h under 100 ~ 110 ℃ of conditions, being crushed to particle diameter is the granular concave rod soil of 0.45 ~ 1.25mm;
Step 3, then the granular concave rod soil making is placed in to Muffle furnace, under 700 ~ 750 ℃ of conditions, calcines 2 ~ 2.5h, make granular concave rod earth adsorbing.
With the prepared attapulgite adsorbent of the present embodiment 3, to concentration, be 20mg/L containing Cd
2+waste water carries out adsorption treatment, under the condition that the speed of agitator that is 1g/L, 250r/min at described granular concave rod earth adsorbing dosage and adsorption time are 2h, described containing Cd
2+cd in waste water
2+clearance be 85%.
embodiment 4
A kind of granular concave rod earth adsorbing and preparation method thereof.The concrete steps of its preparation method are:
Step 1, water is mixed with attapulgite powder, the mass ratio of water and attapulgite powder is 1 ︰ 0.8 ~ 1, makes mud shape attapulgite;
Step 2, by the mud shape attapulgite making dry 8 ~ 12h under 100 ~ 110 ℃ of conditions, being crushed to particle diameter is the granular concave rod soil of 0.45 ~ 1.25mm;
Step 3, then the granular concave rod soil making is placed in to Muffle furnace, under 700 ~ 750 ℃ of conditions, calcines 2 ~ 2.5h, make granular concave rod earth adsorbing.
With the prepared attapulgite adsorbent of the present embodiment 4, to concentration, be 30mg/L containing Pb
2+waste water carries out adsorption treatment, under the condition that the speed of agitator that is 1g/L, 250r/min at described granular concave rod earth adsorbing dosage and adsorption time are 2h, described containing Pb
2+pb in waste water
2+clearance be 94%.
This specific embodiment compared with prior art has following good effect:
This specific embodiment be take attapulgite powder as raw material, water is mixed with attapulgite powder, the mass ratio of water and attapulgite powder is 1 ︰ 0.5 ~ 1, make mud shape attapulgite, again by the mud shape attapulgite making dry 8 ~ 16h under 90 ~ 110 ℃ of conditions, take out dried block attapulgite, be crushed to the particle that particle diameter is 0.45 ~ 1.25mm, then under 650 ~ 750 ℃ of conditions, calcine 2 ~ 3h, make the granular concave rod earth adsorbing of processing heavy metal cation waste water, therefore technique is simple.
The advantages such as the attapulgite powder aboundresources that this specific embodiment is used, raw material cheapness, therefore the granular concave rod earth adsorbing cost making in this specific embodiment is low.
Granular concave rod earth adsorbing prepared by this specific embodiment, due to the high-temperature calcination through 650 ~ 750 ℃, granule strength is high, and specific area is large, has produced calcium, the magnesium plasma of capacitive simultaneously, produces OH in solution
-make solution alkalize, thereby make heavy metal cation precipitate and separate out.
Granular concave rod earth adsorbing prepared by this specific embodiment, particle diameter is 0.45 ~ 1.25mm.Because particle diameter is easy to greatly separation from water, adsorption capacity is large, and in the waste residue after absorption, content of beary metal is 10-50wt%, can be used for smelting heavy metal, produces secondary benefit.
Fig. 1 is the prepared a kind of granular concave rod earth adsorbing of embodiment 1, can find out, rough surface, forms more cavernous structure, because adsorbed water, zeolite water and the constitution water in attapulgite sloughed in high-temperature calcination, causes intracell duct to increase.Fig. 2 is that the prepared granular concave rod earth adsorbing of Fig. 1 is compared with undressed attapulgite powder, the 1649cm of prepared granular concave rod earth adsorbing
-1water peak narrows down, and shows to dewater in attapulgite calcination process 3554cm
-1mg-OH characteristic peak in absorption spectrum, disappear, show that variation has occurred prepared granular concave rod earth adsorbing chain layer structure, interlamellar spacing increases, thereby improves absorption property.
Therefore, this specific embodiment technique simply and not produces secondary pollution, and prepared granular concave rod earth adsorbing has that particle diameter is large, free settling, easily reclaim and the good feature of absorption property, is applicable to industrial heavy metal cation wastewater treatment.
Claims (3)
1. a preparation method for granular concave rod earth adsorbing, is characterized in that described preparation method is:
Step 1, water is mixed with attapulgite powder, the mass ratio of water and attapulgite powder is 1 ︰ 0.5 ~ 1, makes mud shape attapulgite;
Step 2, by the mud shape attapulgite making dry 8 ~ 16h under 90 ~ 110 ℃ of conditions, being crushed to particle diameter is the granular concave rod soil of 0.45 ~ 1.25mm;
Step 3, then the granular concave rod soil making is placed in to Muffle furnace, under 650 ~ 750 ℃ of conditions, calcines 2 ~ 3h, make granular concave rod earth adsorbing.
2. the preparation method of granular concave rod earth adsorbing according to claim 1, is characterized in that the particle diameter of described attapulgite powder is for being less than 76 μ m.
3. a granular concave rod earth adsorbing, is characterized in that described adsorbent is according to the prepared granular concave rod earth adsorbing of preparation method of granular concave rod earth adsorbing described in any one in claim 1 ~ 2.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105148835A (en) * | 2015-10-27 | 2015-12-16 | 武汉科技大学 | Particle-type 13X molecule sieve/attapulgite-loaded nanometer iron-nickel material and preparation method thereof |
| CN106732346A (en) * | 2017-03-13 | 2017-05-31 | 南京信息工程大学 | A kind of preparation method of decoloring material of dyeing waste water |
| CN106943988A (en) * | 2017-04-12 | 2017-07-14 | 明光市国星凹土有限公司 | A kind of preparation method of attapulgite adsorption particle |
| CN106980005A (en) * | 2017-05-25 | 2017-07-25 | 安徽宏远职业卫生技术服务有限公司 | A kind of water quality detection agent detected for heavy metal element |
| CN110302743A (en) * | 2019-06-24 | 2019-10-08 | 上海交通大学 | The preparation method of Adsorption of Radioactive nucleic and the concave convex rod bead of heavy metal ion |
| CN114804962A (en) * | 2022-04-07 | 2022-07-29 | 云南天腾化工有限公司 | Novel anti-caking agent for compound fertilizer and preparation method and application thereof |
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| CN101164911A (en) * | 2007-09-27 | 2008-04-23 | 袁长兵 | Method for producing concave-convex rod particle adsorption oxygen increasing agent |
| CN101306343A (en) * | 2007-11-14 | 2008-11-19 | 中国科学院南京土壤研究所 | Method for preparing water body dephosphorized granule adsorbent using attapulgite clay |
| CN102225327A (en) * | 2011-04-21 | 2011-10-26 | 郑玥 | Method for producing attapulgite palm oil de-coloring purifying agent |
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| CN87100693A (en) * | 1987-02-13 | 1988-08-24 | 浙江省地质科学研究所 | Active clay for oil and fat purification |
| CN101164911A (en) * | 2007-09-27 | 2008-04-23 | 袁长兵 | Method for producing concave-convex rod particle adsorption oxygen increasing agent |
| CN101306343A (en) * | 2007-11-14 | 2008-11-19 | 中国科学院南京土壤研究所 | Method for preparing water body dephosphorized granule adsorbent using attapulgite clay |
| CN102225327A (en) * | 2011-04-21 | 2011-10-26 | 郑玥 | Method for producing attapulgite palm oil de-coloring purifying agent |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105148835A (en) * | 2015-10-27 | 2015-12-16 | 武汉科技大学 | Particle-type 13X molecule sieve/attapulgite-loaded nanometer iron-nickel material and preparation method thereof |
| CN106732346A (en) * | 2017-03-13 | 2017-05-31 | 南京信息工程大学 | A kind of preparation method of decoloring material of dyeing waste water |
| CN106943988A (en) * | 2017-04-12 | 2017-07-14 | 明光市国星凹土有限公司 | A kind of preparation method of attapulgite adsorption particle |
| CN106980005A (en) * | 2017-05-25 | 2017-07-25 | 安徽宏远职业卫生技术服务有限公司 | A kind of water quality detection agent detected for heavy metal element |
| CN110302743A (en) * | 2019-06-24 | 2019-10-08 | 上海交通大学 | The preparation method of Adsorption of Radioactive nucleic and the concave convex rod bead of heavy metal ion |
| CN114804962A (en) * | 2022-04-07 | 2022-07-29 | 云南天腾化工有限公司 | Novel anti-caking agent for compound fertilizer and preparation method and application thereof |
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Application publication date: 20140903 |