CN102921371A - Manganese oxide adsorbent and preparation method thereof - Google Patents
Manganese oxide adsorbent and preparation method thereof Download PDFInfo
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- CN102921371A CN102921371A CN2012105219069A CN201210521906A CN102921371A CN 102921371 A CN102921371 A CN 102921371A CN 2012105219069 A CN2012105219069 A CN 2012105219069A CN 201210521906 A CN201210521906 A CN 201210521906A CN 102921371 A CN102921371 A CN 102921371A
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Abstract
The invention discloses a manganese oxide adsorbent and a preparation method thereof. The manganese oxide adsorbent comprises the following components in parts by weight; 100-150 parts of powder containing manganese oxide and 25-30 parts of binding agent, wherein the powder containing manganese oxide is composed of a manganese-containing compound and a lithium-containing compound in a weight ratio of (1:1)-(1:3). The preparation method comprises the steps of: 1, uniformly mixing the manganese-containing compound with the lithium-containing compound, heating to 100-200 DEG C and carrying out temperature preservation for 24-48 hours; 2, cooling the mixture to the room temperature, drying at the temperature of 60-100 DEG C, and then carrying out the temperature preservation for 5-8 hours at the temperature of 400-600 DEG C so as to obtain the powder containing manganese oxide; 3, uniformly mixing 100-150 parts of powder containing manganese oxide in the step 2 with 25-30 parts of binding agent; 4, carrying out extrusion forming or centrifugal forming on the obtained uniform mixture; and 5, dripping the formed material in ethanol or a solution of the ethanol and deionized water to obtain the manganese oxide adsorbent. The manganese oxide adsorbent disclosed by the invention is high in extraction efficiency and long in service life; and the preparation method is easy to implement, convenient, safe and low in energy consumption.
Description
Technical field
The present invention relates to a micron enclosure material field, particularly, relate to a kind of manganese oxide sorbents and preparation method thereof.
Background technology
Along with the development of new-energy automobile, the international market is to the demand sustainable growth of lithium product, increases with 7% ~ 11% speed every year on average.Upstream product as the new-energy automobile industrial chain, the development and use of lithium resource have become in the world scientific research department and the common hot issue of paying close attention to of industrial quarters, some lithium industry companies constantly seek to open up the approach of new resource and expansion product yield in the world, because land lithium abundant ore source is limited, production cost is high, and the mineral products taste descends.Can't satisfy present requirements, the salt lake is carried lithium and is replaced pegmatite to carry lithium having become foregone conclusion in the world, and bittern is put forward the main flow that lithium has become lithium industry, will occupy an leading position by longer-term in the lithium industrial development.
Salt lake bittern is considered to following important lithium source.Li in the bittern
+Often coexist with micro-form and a large amount of alkali metal, alkaline-earth metal ions.Because their chemical property is very close, so that therefrom the separation and Extraction lithium is very difficult.Lithium is extracted from bittern mainly with the form of lithium carbonate, lithium chloride in the world at present, the technology that adopts mainly contains solvent extraction, the precipitation method and absorption method etc.The salt lake bittern resource that China contains lithium mostly is the bittern of high Mg/Li ratio, the Mg of high-load
2+Existence so that separate Li
+Technology more complicated, there is no at present foreign technology can use for reference, and becomes the technical bottleneck that bittern is carried lithium.Absorption method has selective height, can process low concentration bittern, can adapt to the characteristics of cleaner production, and technique is simple, the rate of recovery is high, considers than additive method larger advantage is arranged from economy and environmental angle, is specially adapted to carry lithium from low-grade seawater or salt lake saline.The absorption method key is to seek the adsorbent that adsorptive selectivity is good, cyclic utilization rate is high, requires the absorption lithium ion ability of adsorbent strong, long service life.
Summary of the invention
The purpose of this invention is to provide a kind of adsorbent for extracting lithium ion and preparation method thereof, easy to operate, safety, energy consumption is low, the high adsorption capacity of gained adsorbent, long service life is easy to again the enforcement of lithium ion adsorbing and extracting.
In order to achieve the above object, the invention provides a kind of manganese oxide sorbents, wherein, this manganese oxide sorbents forms by counting by weight 100 ~ 150 parts the powder of manganese oxide and 25 ~ 30 parts binding agent.Preferably, this manganese oxide sorbents forms by counting by weight 120 ~ 140 parts the powder of manganese oxide and 25 ~ 28 parts binding agent.The powder of described manganese oxide by weight ratio be 1:1 ~ 1:3 contain manganese compound and lithium-containing compound forms.Adding lithium-containing compound mainly is in the adsorbent powder powder material, forms the LiMn2O4 compound.The suction-operated of this manganese oxide sorbents is based on the principle of ion-exchange, and namely lithium ion carries out ion-exchange in the hydrogen ion in the adsorbent and the bittern.The proportioning that contains manganese compound and lithium-containing compound among the present invention can make it form compound, carries out more fast ion-exchange, also just can improve adsorption rate.Binding agent mainly is the effect of playing support, can guarantee multiple adsorb, and material is not damaged, is conducive to industrial production, improves the service life of adsorbent.
Above-mentioned manganese oxide sorbents, wherein, the described manganese compound that contains is one or more mixture in manganese dioxide, mangano-manganic oxide, manganese sesquioxide managnic oxide, manganese carbonate, the manganese oxalate.
Above-mentioned manganese oxide sorbents, wherein, described lithium-containing compound is one or more the mixture in lithium hydroxide, lithium carbonate, lithium nitrate, the lithium oxalate.
Above-mentioned manganese oxide sorbents, wherein, described binding agent is one or more the mixture in phenolic resins, polyvinyl alcohol, polyvinyl chloride, polytetrafluoroethylene (PTFE), the Kynoar.
The present invention also provides a kind of method for preparing above-mentioned manganese oxide sorbents, and wherein, described method comprises:
Step 1, with weight ratio be 1:1 ~ 1:3 contain manganese compound and lithium-containing compound mixes, be heated to 100 ~ 200 ℃ in the aerial closed container, kept this temperature 24 ~ 48 hours.
Step 2 with the homogeneous mixture cool to room temperature that step 1 obtains, then after 60 ℃ ~ 100 ℃ dryings, is kept the powder that this temperature obtained manganese oxide in 5 ~ 8 hours again under 400 ~ 600 ℃; Preferably, can further make manganese oxide powder microballoon.
Step 3,100 ~ 150 parts of bonding agents with 25 ~ 30 parts of powder of counting by weight the manganese oxide of getting step 2 gained mix.
Step 4 is pushed the even mixture of step 3 gained or centrifugal forming obtains article shaped.
Step 5, described article shaped drop onto in the ethanol or the solution of ethanol and deionized water in, obtain described manganese oxide sorbents.
Manganese oxide sorbents provided by the invention and preparation method thereof has the following advantages:
This manganese oxide sorbents is adsorbed lithium ion from salt lake bittern amount is 25 ~ 32 mg/g, the rate of recovery of lithium ion can reach 82% ~ 92% in the bittern, namely, compared with prior art, the rate of adsorption of sorbing material provided by the invention is faster, adsorbance is larger, and adsorbing and extracting efficient is higher, and does not need multiple adsorb just can reach very high adsorbance.The material crystal formation does not change the adsorbent long service life before and after the absorption.Manufacture process of the present invention is simple, and the preparation method is easy to implement, and products obtained therefrom need not drying, and is more simple and practical.Reaction condition is gentle, stable, easy to operate, safety, and energy consumption is low, has very widely industrial applications prospect.
Description of drawings
Fig. 1 is the electromicroscopic photograph after the mixture that contains manganese compound and lithium-containing compound of the present invention tentatively heats.
Fig. 2 is the electromicroscopic photograph of the powder of manganese oxide of the present invention.
Fig. 3 is the electromicroscopic photograph of manganese oxide sorbents of the present invention.
The specific embodiment
Below in conjunction with accompanying drawing the specific embodiment of the present invention is further described.
Embodiment 1
With weight ratio be 1:1 contain manganese compound and lithium-containing compound mixes, then be heated to 200 ℃ under the aerial closed container, kept temperature 24 hours, and adopted the Hitachi-S3400N SEM that it is taken, electromicroscopic photograph as shown in Figure 1.
The gained mixture 60 ℃ of lower oven dry, was kept temperature 6 hours again under 500 ℃, obtain the powder of manganese oxide, adopt the Hitachi-S3400N SEM that it is taken, electromicroscopic photograph as shown in Figure 2.
Get the Powdered manganese oxide of the gained of counting by weight 140 parts and 25 parts of binding agents mix, at last by extrusion modling, article shaped is dropped in the solution of ethanol and deionized water, make manganese oxide sorbents.Adopt the Hitachi-S4800 SEM that manganese oxide sorbents is taken, electromicroscopic photograph as shown in Figure 3.
Manganese oxide sorbents is used for bittern absorption, make bittern pass through this manganese oxide sorbents until saturated, concentration with lithium ion in the bittern before and after the atomic absorption spectrophotometer test absorption, the adsorption concentration of testing this adsorbent that is applied can reach more than 92% of concentration in the former bittern, and adsorbance is 32 mg/g.
Embodiment 2
With weight ratio be 1:1.5 contain manganese compound and lithium-containing compound mixes, be heated to 100 ℃ under the then aerial closed container, kept temperature 48 hours.
The gained mixture 80 ℃ of lower oven dry, is kept temperature 5 hours again under 600 ℃, obtain the powder of manganese oxide.
Get the Powdered manganese oxide of the gained of counting by weight 120 parts and 28 parts of binding agents mix, by centrifugal forming, article shaped is dropped in the solution of ethanol at last, make manganese oxide sorbents.
Manganese oxide sorbents is used for bittern absorption, make bittern pass through this manganese oxide sorbents until saturated, concentration with lithium ion in the bittern before and after the atomic absorption spectrophotometer test absorption, the adsorption concentration of testing this adsorbent that is applied can reach more than 85% of concentration in the former bittern, and adsorbance is 28 mg/g.
Embodiment 3
With weight ratio be 1:3 contain manganese compound and lithium-containing compound mixes, be heated to 150 ℃ under the then aerial closed container, kept temperature 36 hours.
The gained mixture 100 ℃ of lower oven dry, is kept temperature 8 hours again under 400 ℃, obtain the powder of manganese oxide.
Get the Powdered manganese oxide of the gained of counting by weight 100 parts and 30 parts of binding agents mix, by centrifugal forming, article shaped is dropped in the solution of ethanol at last, make manganese oxide sorbents.
Manganese oxide sorbents is used for bittern absorption, make bittern pass through this manganese oxide sorbents until saturated, concentration with lithium ion in the bittern before and after the atomic absorption spectrophotometer test absorption, the adsorption concentration of testing this adsorbent that is applied can reach more than 80% of concentration in the former bittern, and adsorbance is 25 mg/g.
Although content of the present invention has been done detailed introduction by above preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple modification of the present invention with to substitute all will be apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (5)
1. a manganese oxide sorbents is characterized in that, this manganese oxide sorbents forms by counting by weight 100 ~ 150 parts the powder of manganese oxide and 25 ~ 30 parts binding agent; The powder of described manganese oxide by weight ratio be 1:1 ~ 1:3 contain manganese compound and lithium-containing compound forms.
2. manganese oxide sorbents as claimed in claim 1 is characterized in that, the described manganese compound that contains is one or more mixture in manganese dioxide, mangano-manganic oxide, manganese sesquioxide managnic oxide, manganese carbonate, the manganese oxalate.
3. manganese oxide sorbents as claimed in claim 1 is characterized in that, described lithium-containing compound is one or more the mixture in lithium hydroxide, lithium carbonate, lithium nitrate, the lithium oxalate.
4. manganese oxide sorbents as claimed in claim 1 is characterized in that, described binding agent is one or more the mixture in phenolic resins, polyvinyl alcohol, polyvinyl chloride, polytetrafluoroethylene (PTFE), the Kynoar.
5. a method for preparing such as the described manganese oxide sorbents of claim 1 ~ 4 is characterized in that, described method comprises:
Step 1, with weight ratio be 1:1 ~ 1:3 contain manganese compound and lithium-containing compound mixes, in closed container, be heated to 100 ~ 200 ℃, kept this temperature 24 ~ 48 hours;
Step 2 with the homogeneous mixture cool to room temperature that step 1 obtains, then after 60 ℃ ~ 100 ℃ dryings, is kept the powder that this temperature obtained manganese oxide in 5 ~ 8 hours again under 400 ~ 600 ℃;
Step 3,100 ~ 150 parts of bonding agents with 25 ~ 30 parts of powder of counting by weight the manganese oxide of getting step 2 gained mix;
Step 4 is pushed the even mixture of step 3 gained or centrifugal forming obtains article shaped;
Step 5, described article shaped drop onto in the ethanol or the solution of ethanol and deionized water in, obtain described manganese oxide sorbents.
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| CN2012103711862A CN102824759A (en) | 2012-09-29 | 2012-09-29 | Method for adsorbing lithium ions from salt lake brine through utilizing manganese oxide ion sieve adsorbent |
| CN2012105219069A CN102921371A (en) | 2012-09-29 | 2012-12-07 | Manganese oxide adsorbent and preparation method thereof |
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| CN201210521918.1A Active CN102935299B (en) | 2012-09-29 | 2012-12-07 | A kind of method using manganese oxide sorbing material to extract lithium ion |
| CN2012105219069A Pending CN102921371A (en) | 2012-09-29 | 2012-12-07 | Manganese oxide adsorbent and preparation method thereof |
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| CN201210521918.1A Active CN102935299B (en) | 2012-09-29 | 2012-12-07 | A kind of method using manganese oxide sorbing material to extract lithium ion |
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| CN103785345A (en) * | 2014-03-04 | 2014-05-14 | 武汉大学 | Supported manganese dioxide adsorbent and method for treating aniline waste water through same |
| CN108636341A (en) * | 2018-04-18 | 2018-10-12 | 南京工业大学 | A kind of forming method carrying lithium adsorbent |
| CN108854964A (en) * | 2018-07-11 | 2018-11-23 | 合肥帧讯低温科技有限公司 | A kind of water purification adsorbent material and preparation method |
| CN109012600A (en) * | 2018-09-17 | 2018-12-18 | 天津市职业大学 | A kind of activated carbon supported lithium ion sieve filler and its methods for making and using same |
| CN111644050A (en) * | 2020-05-06 | 2020-09-11 | 江苏卓高环保科技有限公司 | Formaldehyde removal purification material capable of releasing fragrance and application of formaldehyde removal purification material to formaldehyde removal purifier |
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| CN103785345A (en) * | 2014-03-04 | 2014-05-14 | 武汉大学 | Supported manganese dioxide adsorbent and method for treating aniline waste water through same |
| CN103785345B (en) * | 2014-03-04 | 2016-03-02 | 武汉大学 | A kind of support type manganese dioxide adsorbent and utilize the method for its pretreatment aniline waste water |
| CN108636341A (en) * | 2018-04-18 | 2018-10-12 | 南京工业大学 | A kind of forming method carrying lithium adsorbent |
| CN108854964A (en) * | 2018-07-11 | 2018-11-23 | 合肥帧讯低温科技有限公司 | A kind of water purification adsorbent material and preparation method |
| CN109012600A (en) * | 2018-09-17 | 2018-12-18 | 天津市职业大学 | A kind of activated carbon supported lithium ion sieve filler and its methods for making and using same |
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| Publication number | Publication date |
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| CN102824759A (en) | 2012-12-19 |
| CN102935299A (en) | 2013-02-20 |
| CN102935299B (en) | 2015-09-30 |
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Application publication date: 20130213 |