CN110586051B - Reusable large-size hollow adsorbent and preparation method and application thereof - Google Patents
Reusable large-size hollow adsorbent and preparation method and application thereof Download PDFInfo
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- B01D15/08—Selective adsorption, e.g. chromatography
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/3491—Regenerating or reactivating by pressure treatment
Abstract
The invention discloses a large-size hollow adsorbent capable of being recycled, and a preparation method and application thereof, and belongs to the technical field of chemical adsorbent materials. The method comprises the following steps: firstly, drying and sieving the cementing material; then placing soluble spherical particles as ball cores in a ball forming mill or a sugar coating machine, spraying a binder solution on the surfaces of the ball cores, and continuously adding a cementing material into the ball forming mill or the sugar coating machine to ensure that the cementing material is uniformly coated on the surfaces of the ball core materials; when the sphere diameter of the sample particles reaches the required size, taking out, and sieving and grading; maintaining for 0.5-2d to ensure that the sample initially obtains certain strength; removing the spherical core of the sample by adopting a solvent dissolution method or a low-temperature heat treatment method; and finally, curing the sample without the spherical cores in water for 1-7 days to obtain the porous adsorption material with large size, high strength and hollow structure. The method has the advantages of simple process, easily obtained raw materials, good reproducibility, high oil absorption efficiency of the prepared adsorbing material and reusability.
Description
Technical Field
The invention belongs to the technical field of chemical adsorbent materials, and particularly relates to a large-size hollow adsorbent capable of being recycled, and a preparation method and application thereof.
Background
Lubricating oil is widely used in transmission parts of automobiles, ships, various industrial equipment, and various machines. As the world's largest consumption country of lubricating oil, about 3000 million tons of waste lubricating oil are produced every year in China. However, the waste lubricating oil is difficult to handle because of its very complex composition and the large amount of organic and inorganic substances contained therein. At present, the treatment mode of the waste lubricating oil is relatively extensive, the main methods comprise discarding, burning, recycling and the like, and the recycling rate of the waste engine oil is only 20%. Furthermore, the used oil is not allowed to be regenerated and should be delivered to qualified waste oil treatment enterprises for treatment. In the national records of dangerous wastes, the used oil belongs to dangerous wastes.
The adsorption treatment technology is an important waste oil resource treatment technology, is commonly used for decoloring waste lubricating oil, and has long been an important position in the field of oil treatment. The technology utilizes lipophilic materials or porous materials, such as argil, oil absorption resin, activated carbon and the like, to remove polar substances such as colloid, asphaltene, acids, soaps, nitrogen-containing compounds, sulfur-containing compounds and the like in the waste oil and pollutants such as aromatic hydrocarbon and the like, so that the selection of an adsorption material is crucial in the adsorption process. However, the common oil-absorbing materials have many defects, such as poor oil-absorbing performance of argil and easy dust pollution; although the oil-absorbing resin has a good oil-absorbing effect, the cost is high; the activated carbon is expensive in cost, generally poor in oil absorption performance, and more importantly, the material is poor in reusability and not beneficial to cost control.
In the application of the adsorption technology, the adsorption material can lose the capacity of continuous adsorption after saturated adsorption. And after adsorbing the harmful substance, it itself becomes a toxic harmful substance and needs to be handled in a proper way. The inorganic material with a porous structure is used in the oil absorption field, and the adsorbent is reused by a combustion method, so that the cost can be effectively reduced, and the risk that the adsorbent is toxic after adsorbing the waste lubricating oil can be avoided. Compared with common porous structures, the hollow ceramsite shows huge application prospects in the adsorption field due to the huge hollow structure of the hollow ceramsite. Patent CN201210462747.X discloses a light hollow ceramsite and a preparation method thereof, wherein the light hollow ceramsite is composed of a ceramic material and a template material, the ceramic material is composed of waste paper papermaking dry sludge, fly ash and clay, and the template material is polyphenyl foam particles; the obtained light hollow ceramsite is spherical or quasi-spherical in shape, the middle cavity is also spherical or quasi-spherical, and the middle cavity is separated from the outside by a ceramic structure with the wall thickness of 0.5-2.5 mm; the light hollow ceramsite can be used as a suspended biological membrane ceramic filter material in sewage treatment. However, the process needs high-temperature calcination to sinter the ceramic material to obtain a certain strength, more importantly, different raw material systems need to be redesigned, and a sample is easy to crack and low in yield due to nonuniform shrinkage in the sintering process.
The present application has been made for the above reasons.
Disclosure of Invention
In view of the problems or defects of the prior art, the invention aims to provide a preparation technology of a reusable large-size hollow adsorbent, and the prepared adsorbent and application thereof. The method can obtain the high-strength reusable hollow adsorbent only by removing the ball core material at low temperature or without heat treatment.
In order to achieve one of the above objects of the present invention, the present invention adopts the following technical solutions:
a preparation method of a recyclable large-size hollow adsorbent comprises the following steps:
(1) drying and sieving the cementing material for later use;
(2) placing soluble spherical particle materials in a pelletizer or a sugar coating machine, taking the spherical particle materials as a ball core, and spraying a binder solution on the surface of the ball core to obtain a binder-treated ball core material; adding the gelled material dried and sieved in the step (1) into the ball forming mill or the sugar coating machine to prepare a layer of ball core material uniformly coated with the gelled material;
(3) putting the ball core material uniformly coated with the layer of the cementing material prepared in the step (2) into a ball forming mill or a sugar coating machine, repeating the steps of spraying the binder and coating the cementing material in the step (2) until the ball diameter of the obtained ball core material sample reaches the required size, and then sieving, grading and taking out;
(4) and (3) maintaining the ball core material obtained by sieving and grading in the step (3) for 0.5-2d under a steam condition or in a humid environment to obtain a primary maintenance sample, removing the ball core of the primary maintenance sample by adopting a solvent dissolution method or a low-temperature heat treatment method, and continuing maintaining for 1-7d under the steam condition or in the humid environment to obtain the porous adsorption material with large size, high strength and hollow structure.
Further, according to the technical scheme, the cementing material in the step (1) is any one of cement, gypsum and the like.
Further, in the above technical scheme, the drying temperature of the cementing material in the step (1) is 80-120 ℃, and more preferably 100 ℃.
Further, according to the above technical solution, the spherical particle material in the step (2) may be a water-soluble material, or may be a water-insoluble material, and the water-soluble material is preferably any one of urea particles, compound fertilizer particles, and the like; the water-insoluble material may be any of polystyrene particles and the like.
Further, in the above technical solution, the particle size of the spherical particle material in step (2) may not be limited, and the particle size may be selected according to the size of the actually required hollow structure.
Further, in the above technical scheme, the binder solution in step (2) is a solution of any one or a combination of dispersible latex powder, sesbania powder, CMC, guar gum, polyvinyl alcohol, and the like; the concentration of the binder solution is 0.5-2.5 wt%.
Preferably, the binder solution is obtained by adding one or a combination of dispersible latex powder, sesbania powder, CMC, guar gum and polyvinyl alcohol into water, heating in a water bath and stirring until the binder is completely dissolved, and standing.
Further, in the above technical solution, the removing the core of the primary cured sample by using the solvent dissolution method in the step (4) specifically means that the primary cured sample is soaked in water or an organic solvent until the core is completely dissolved out.
Preferably, in the above technical solution, the organic solvent is any one of an ethanol solution of ammonia water, an aqueous acetone solution, ethyl acetate, Methyl Methacrylate (MMA), and the like.
Further, in the above technical solution, the step (4) of removing the core of the primary cured sample by the low-temperature heat treatment method specifically means that the sample is subjected to heat treatment at 300-550 ℃ for 10-30min, so that the core material is completely thermally decomposed.
The second purpose of the invention is to provide a recyclable large-size hollow adsorbent prepared by the method.
Specifically, in the above technical solution, the size of the adsorbent is not limited, and the particle size thereof can be selected according to the size of the actually required hollow structure. For example, the particle size of the adsorbent may be 8 to 10mm, and the hollow pore diameter thereof may be 3 to 5 mm; the particle size of the adsorbent can also be 5-8mm, the hollow pore size can be 2-3mm, and the like.
The third purpose of the invention is to provide the application of the recyclable large-size hollow adsorbent prepared by the method, which can be used for adsorbing the waste lubricating oil.
The fourth purpose of the invention is to provide a recycling method of the large-size hollow adsorbent prepared by the method, specifically, the hollow adsorbent after saturated adsorption is desorbed by a heat treatment method or a negative pressure suction method to obtain a regenerated hollow adsorbent, and then the regenerated hollow adsorbent is continuously used for adsorbing the waste lubricating oil.
Further, in the above technical scheme, the heat treatment method specifically includes heating the saturated and adsorbed hollow adsorbent from room temperature to 400-600 ℃ for constant temperature heat treatment for 10-30min, and then naturally cooling.
Preferably, in the above technical solution, the rate of the heat treatment may be 1-10 ℃/min, more preferably 5 ℃/min.
Further, in the above technical solution, the negative pressure suction method specifically sucks the saturated and adsorbed hollow adsorbent at 0.08-0.10MPa and 80-120 ℃, and the suction condition is preferably 0.09MPa and 100 ℃.
Compared with the prior art, the preparation method and the application of the recyclable large-size hollow adsorbent have the following beneficial effects:
(1) the method has the advantages of simple process, easily obtained raw materials, good reproducibility, low price, environmental friendliness and capability of obtaining the high-efficiency hollow adsorbent with various particle size ranges.
(2) The hollow adsorbent prepared by the method has high oil absorption efficiency, the weight of the adsorbent can reach 62.2 percent after the adsorbent is used for absorbing waste lubricating oil for 30min, and the weight of the adsorbent can reach 75.8 percent after 24 h.
(3) After saturated adsorption, the hollow adsorbent prepared by the method can be reused by a heat treatment or negative pressure suction method, so that the use cost of the adsorbent can be effectively reduced, the risk of toxicity of the adsorbent due to adsorption of waste lubricating oil is avoided, and the environment-friendly effect is obvious.
(4) The hollow adsorbent prepared by the method has good effect of repeatedly absorbing the waste lubricating oil. After the absorbent is subjected to oil absorption-heat treatment repeatedly for 5 times, the oil absorption weight gain is 72.1% after 24 hours; after the absorbent is repeatedly sucked in the oil absorption-negative pressure way for 5 times, the oil absorption weight gain is 76.3 percent within 24 hours; furthermore, the adsorbent has high strength and is not broken under a pressure of 100N.
Drawings
In FIG. 1, a) and b) are an appearance picture and an optical microscope picture of a hollow adsorbent sample having a particle size of 5 to 8mm and a hollow pore size of 2 to 3mm prepared in example 2, respectively.
Detailed Description
The present invention will be described in further detail below with reference to examples. The present invention is implemented on the premise of the technology of the present invention, and the detailed embodiments and specific procedures are given to illustrate the inventive aspects of the present invention, but the scope of the present invention is not limited to the following embodiments.
Various modifications to the precise description of the invention will be readily apparent to those skilled in the art from the information contained herein without departing from the spirit and scope of the appended claims. It is to be understood that the scope of the invention is not limited to the procedures, properties, or components defined, as these embodiments, as well as others described, are intended to be merely illustrative of particular aspects of the invention. Indeed, various modifications of the embodiments of the invention which are obvious to those skilled in the art or related fields are intended to be covered by the scope of the appended claims.
For a better understanding of the invention, and not as a limitation on the scope thereof, all numbers expressing quantities, percentages, and other numerical values used in this application are to be understood as being modified in all instances by the term "about". Accordingly, unless expressly indicated otherwise, the numerical parameters set forth in the specification and attached claims are approximations that may vary depending upon the desired properties sought to be obtained. At the very least, each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.
The pelletizer used in each of the following examples was a disk pelletizer.
The standard curing in the following examples refers to curing under standard curing conditions recognized in the prior art, i.e., curing at a temperature of 20 ℃. + -. 5 ℃ and a humidity of not less than 95%.
The method comprises the following steps: firstly, drying a cementing material (such as cement, gypsum and the like) at about 100 ℃, and enabling all powder to pass through a 200-mesh sieve for later use; then, soluble spherical particles such as urea, compound fertilizer, polystyrene and the like are taken as a ball core (the selection of the particle size can be determined according to the size of an actually required hollow structure), the spherical particles are placed in a disc type ball forming mill or a sugar coating machine, 0.5-2.5wt% of aqueous solution of dispersible latex powder, sesbania powder, CMC, guar gum, polyvinyl alcohol and the like is taken as a binder, the aqueous solution is sprayed on the surface of the ball core in a spraying mode, and the cementing material is continuously added into the ball forming mill, so that the cementing material is uniformly coated on the surface of the ball core material. When the sphere diameter of the sample particles reaches the required size, taking out the sample, and sieving and grading the sample; then, the prepared sample is maintained for 0.5-2d under a certain condition (steam maintenance or wet environment maintenance) so that the sample initially obtains a certain strength; then removing the core of the sample by a solvent dissolving method (the solvent used by the water-soluble substances such as urea, compound fertilizer and the like is water, and the water-insoluble materials such as polystyrene adopt ethanol solution of ammonia water, acetone solution, ethyl acetate, MMA and the like) or a low-temperature (300-550 ℃) heat treatment method; and finally, curing the sample without the spherical cores in water for 1-7 days to obtain the porous adsorption material with large size, high strength and hollow structure.
Example 1
The preparation method of the hollow adsorbent with the particle size of 8-10mm and the hollow pore diameter of 3-5mm in the embodiment specifically comprises the following steps:
(1) weighing 1kg of ordinary portland cement, drying at about 100 ℃, and enabling all powder to pass through a 200-mesh sieve for later use;
(2) weighing 500g of urea spherulites (the particle size is 3-5mm), and adding the urea spherulites into a granulator; starting a granulator, taking a 0.5 wt% CMC aqueous solution as a binder, and spraying the binder on the surface of urea particles;
(3) gradually adding the dried and sieved cement powder, repeating the steps of spraying the binder and adding the cement powder until the sphere diameter of most samples reaches 8mm, and screening out particles with the diameter of 8-10mm by adopting a mesh screen;
(4) carrying out standard maintenance on the obtained sample in a standard maintenance box for 24 hours;
(5) soaking the cured sample particles in water, repeatedly washing to completely dissolve out urea spherical core, and continuously curing in water at 20 + -5 deg.C for 6d to obtain hollow adsorbent with particle diameter of about 8-10mm and hollow pore diameter of 3-5 mm.
Example 2
The preparation method of the hollow adsorbent with the particle size of 5-8mm and the hollow pore diameter of 2-3mm in the embodiment specifically comprises the following steps:
(1) weighing 1kg of gypsum powder, drying at about 100 ℃, and enabling the powder to pass through a 200-mesh sieve for later use;
(2) weighing 500g of compound fertilizer spherulites (with the particle size of 2-3mm) and adding the compound fertilizer spherulites into a granulator; starting a ball forming mill, taking a 0.5 wt% guar gum aqueous solution as a binder, and spraying the binder on the surface of urea particles;
(3) gradually adding the dried and sieved gypsum powder, repeating the steps of spraying the adhesive and adding the cement powder until the sphere diameter of most samples reaches 5mm, and screening out particles of 5-8mm by adopting a mesh screen;
(4) carrying out standard maintenance on the obtained sample in a standard maintenance box for 24 hours;
(5) soaking the maintained sample particles in water, repeatedly washing to completely dissolve out urea spherical core, taking out, and maintaining for 6 days to obtain hollow adsorbent with particle diameter of 5-8mm and hollow pore diameter of 2-3 mm.
Example 3
The preparation method of the hollow adsorbent with the particle size of 8-10mm and the hollow pore diameter of 3-5mm in the embodiment specifically comprises the following steps:
(1) weighing 1kg of ordinary portland cement, drying at about 100 ℃, and enabling all powder to pass through a 200-mesh sieve for later use;
(2) weighing 20g of polystyrene spherulites (the particle size is 3-5mm), and adding the polystyrene spherulites into a granulator; starting a pelletizer, taking 1.0 wt% of polyvinyl alcohol aqueous solution as a binder, and spraying the binder on the surface of polystyrene particles;
(3) gradually adding the dried and sieved cement powder, repeating the steps of spraying the binder and adding the cement powder until the sphere diameter of most samples reaches 8mm, and screening out particles with the diameter of 8-10mm by adopting a mesh screen;
(4) carrying out standard maintenance on the obtained sample in a standard maintenance box for 24 hours;
(5) and (3) soaking the cured sample particles in 20% acetone aqueous solution until the polystyrene spherical cores are completely dissolved, and continuously curing in water at the temperature of 20 +/-5 ℃ for 6 days to obtain the hollow adsorbent with the particle size of about 8-10mm and the hollow pore diameter of 3-5 mm.
Example 4
The preparation method of the hollow adsorbent with the particle size of 5-8mm and the hollow pore diameter of 2-3mm in the embodiment specifically comprises the following steps:
(1) weighing 1kg of ordinary portland cement, drying at about 100 ℃, and enabling all powder to pass through a 200-mesh sieve for later use;
(2) weighing 20g of polystyrene spherulites (the particle size is 2-3mm), and adding the polystyrene spherulites into a granulator; starting a pelletizer, taking 1.5 wt% of water solution of redispersible latex powder as a binder, and spraying the binder on the surfaces of polystyrene particles;
(3) gradually adding the dried and sieved cement powder, repeating the steps of spraying the binder and adding the cement powder until the sphere diameter of most samples reaches 5mm, and screening out particles of 5-8mm by adopting a mesh screen;
(4) carrying out standard maintenance on the obtained sample in a standard maintenance box for 24 hours;
(5) and (3) placing the cured sample particles in a muffle furnace for heat treatment at 350 ℃ for 20min, cooling the sample, and then continuing curing in water at the temperature of 20 +/-5 ℃ for 6d to obtain the hollow adsorbent with the particle size of about 5-8mm and the hollow pore diameter of 2-3 mm.
Application example 1
The hollow adsorbent prepared in example 1 is applied to adsorbing waste lubricating oil, and the specific experiment is as follows:
(a) 20g of the hollow adsorbent obtained in example 1 was weighed, immersed in 150 ℃ waste lubricating oil, sieved to remove excess waste lubricating oil after 30min, and weighed after absorbing oil for 30 min. The results show that the weight gain of the sample can reach 56.5%. The weight gain of the sample after 24h was measured by the same method and reached 72.3%.
(b) And (3) heating the sample subjected to oil absorption for 24 hours in the step (a) to 500 ℃ at the speed of 5 ℃/min, carrying out heat treatment for 15min, naturally cooling, and repeating the step (a) to carry out an oil absorption experiment. After the sample is subjected to repeated oil absorption-heat treatment for 5 times, the oil absorption weight gain is 76.6% after 24 hours, and the sample is not damaged under the pressure of 100N.
(c) Placing the sample subjected to oil absorption for 24 hours in the step (a) in a vacuum drying oven, sucking out the waste lubricating oil in the sample under the conditions of 0.09MPa and 100 ℃, and then reusing the sample for the experiment of adsorbing the waste lubricating oil. After the absorbent is repeatedly sucked in the oil absorption-negative pressure way for 5 times, the oil absorption weight gain is 71.4 percent within 24 hours.
Application example 2
The hollow adsorbent prepared in example 2 is applied to adsorbing waste lubricating oil, and the specific experiment is as follows:
(a) 20g of the hollow adsorbent obtained in example 2 was weighed, immersed in 150 ℃ waste lubricating oil, sieved to remove excess waste lubricating oil after 30min, and weighed after absorbing oil for 30 min. The results show that the weight gain of the sample can reach 62.2%. The weight gain of the sample after 24h was measured by the same method and reached 75.8%.
(b) And (3) heating the sample subjected to oil absorption for 24 hours in the step (a) to 500 ℃ at the speed of 5 ℃/min, carrying out heat treatment for 15min, naturally cooling, and repeating the step (a) to carry out an oil absorption experiment. After the sample is subjected to repeated oil absorption-heat treatment for 5 times, the oil absorption weight gain is 73.3% after 24 hours, and the sample is not damaged under the pressure of 100N.
(c) Placing the sample subjected to oil absorption for 24 hours in the step (a) in a vacuum drying oven, sucking out the waste lubricating oil in the sample under the conditions of 0.09MPa and 100 ℃, and then reusing the sample for the experiment of adsorbing the waste lubricating oil. After the absorbent is repeatedly sucked in the oil absorption-negative pressure way for 5 times, the oil absorption weight gain is 75.8 percent within 24 hours.
Application example 3
The hollow adsorbent prepared in example 3 is applied to adsorbing waste lubricating oil, and the specific experiment is as follows:
(a) 20g of the hollow adsorbent obtained in example 3 was weighed, immersed in 150 ℃ waste lubricating oil, sieved to remove excess waste lubricating oil after 30min, and weighed after absorbing oil for 30 min. The results show that the weight gain of the sample can reach 58.5%. The weight gain of the sample after 24h was measured in the same way and reached 74.6%.
(b) And (3) heating the sample subjected to oil absorption for 24 hours in the step (a) to 500 ℃ at the speed of 5 ℃/min, carrying out heat treatment for 15min, naturally cooling, and repeating the step (a) to carry out an oil absorption experiment. After the sample is subjected to repeated oil absorption-heat treatment for 5 times, the oil absorption weight gain is 78.9% after 24 hours, and the sample is not damaged under the pressure of 100N.
(c) Placing the sample subjected to oil absorption for 24 hours in the step (a) in a vacuum drying oven, sucking out the waste lubricating oil in the sample under the conditions of 0.09MPa and 100 ℃, and then reusing the sample for the experiment of adsorbing the waste lubricating oil. After the absorbent is repeatedly sucked in the oil absorption-negative pressure way for 5 times, the oil absorption weight gain is 76.3 percent within 24 hours.
Application example 4
The hollow adsorbent prepared in example 4 is applied to adsorbing waste lubricating oil, and the specific experiment is as follows:
(a) 20g of the hollow adsorbent obtained in example 4 was weighed, immersed in 150 ℃ waste lubricating oil, sieved to remove excess waste lubricating oil after 30min, and weighed after absorbing oil for 30 min. The results show that the weight gain of the sample can reach 50.6%. The weight gain of the sample after 24h was measured by the same method and reached 69.5%.
(b) And (3) heating the sample subjected to oil absorption for 24 hours in the step (a) to 500 ℃ at the speed of 5 ℃/min, carrying out heat treatment for 15min, naturally cooling, and repeating the step (a) to carry out an oil absorption experiment. After the sample is subjected to repeated oil absorption-heat treatment for 5 times, the oil absorption weight gain is 72.1% after 24 hours, and the sample is not damaged under the pressure of 100N.
(c) Placing the sample subjected to oil absorption for 24 hours in the step (a) in a vacuum drying oven, sucking out the waste lubricating oil in the sample under the conditions of 0.09MPa and 100 ℃, and then reusing the sample for the experiment of adsorbing the waste lubricating oil. After the absorbent is repeatedly sucked in the oil absorption-negative pressure way for 5 times, the oil absorption weight gain is 69.4 percent after 24 hours.
Claims (7)
1. A preparation method of a recyclable hollow adsorbent is characterized by comprising the following steps: the method specifically comprises the following steps:
(1) drying and sieving the cementing material for later use; the cementing material is any one of cement and gypsum;
(2) placing soluble spherical particle materials in a pelletizer or a sugar coating machine, taking the spherical particle materials as a sphere core, and spraying a binder solution on the surface of the sphere core to obtain a binder-treated sphere core material; adding the gelled material dried and sieved in the step (1) into the ball forming mill or the sugar coating machine to prepare a layer of ball core material uniformly coated with the gelled material; the spherical particle material is any one of urea particles, compound fertilizer particles and polystyrene particles; the binder solution is an aqueous solution of any one or a combination of dispersible latex powder, sesbania powder, CMC, guar gum and polyvinyl alcohol;
(3) putting the ball core material uniformly coated with the layer of the cementing material prepared in the step (2) into a ball forming mill or a sugar coating machine, repeating the steps of spraying the binder and coating the cementing material in the step (2) until the ball diameter of the obtained ball core material sample reaches the required size, and then sieving, grading and taking out;
(4) maintaining the ball core material obtained by sieving and grading in the step (3) for 0.5-2d under a steam condition or a humid environment to obtain a primary maintenance sample, then removing the ball core of the primary maintenance sample by adopting a solvent dissolution method or a low-temperature heat treatment method, and continuing maintaining for 1-7d under the steam condition or the humid environment to obtain the hollow adsorbent; wherein: the method for removing the ball core of the primary maintenance sample by the low-temperature heat treatment method is to heat treat the sample at the temperature of 300-550 ℃ for 10-30min so as to completely thermally decompose the ball core material.
2. The method for producing a reusable hollow adsorbent according to claim 1, wherein: the concentration of the binder solution in the step (2) is 0.5-2.5 wt%.
3. The method for producing a reusable hollow adsorbent according to claim 1, wherein: the step (4) of removing the ball core of the primary cured sample by adopting a solvent dissolving method is to soak the primary cured sample in water or an organic solvent until the ball core is completely dissolved out.
4. The method for producing a reusable hollow adsorbent according to claim 3, wherein: the organic solvent is any one of ethanol solution of ammonia water, acetone water solution, ethyl acetate and methyl methacrylate.
5. The reusable hollow adsorbent produced by the method for producing a reusable hollow adsorbent according to any one of claims 1 to 4.
6. Use of the hollow adsorbent prepared by the method according to any one of claims 1 to 4, wherein: used for adsorbing the waste lubricating oil.
7. A method for recycling a hollow adsorbent produced by the method according to any one of claims 1 to 4, wherein: the hollow adsorbent after saturated adsorption is desorbed by a heat treatment method or a negative pressure suction method to obtain a regenerated hollow adsorbent, and then the regenerated hollow adsorbent is continuously used for adsorbing the waste lubricating oil.
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1409542A (en) * | 1971-09-01 | 1975-10-08 | Agency Ind Science Techn | Method for manufacture of hollow body |
WO2011031883A2 (en) * | 2009-09-09 | 2011-03-17 | Cls Industrial Purification, Llc | Zeolytic sulfur guard |
CN105817213A (en) * | 2016-05-23 | 2016-08-03 | 大连工业大学 | Adsorbent based on hollow mesoporous silica, preparing method of adsorbent and application of adsorbent in recycling gold |
CN106459729A (en) * | 2014-05-23 | 2017-02-22 | 松本油脂制药株式会社 | Thermal expansion microspheres, manufacturing method and use thereof |
CN108404970A (en) * | 2018-03-05 | 2018-08-17 | 中国科学院山西煤炭化学研究所 | A kind of apple shape hollow molecules sieve microballoon and its preparation method and application |
CN110183244A (en) * | 2019-06-19 | 2019-08-30 | 长安大学 | A kind of hollow mullite spheroidal material and preparation method thereof |
-
2019
- 2019-09-20 CN CN201910892660.8A patent/CN110586051B/en active Active
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1409542A (en) * | 1971-09-01 | 1975-10-08 | Agency Ind Science Techn | Method for manufacture of hollow body |
WO2011031883A2 (en) * | 2009-09-09 | 2011-03-17 | Cls Industrial Purification, Llc | Zeolytic sulfur guard |
CN106459729A (en) * | 2014-05-23 | 2017-02-22 | 松本油脂制药株式会社 | Thermal expansion microspheres, manufacturing method and use thereof |
CN105817213A (en) * | 2016-05-23 | 2016-08-03 | 大连工业大学 | Adsorbent based on hollow mesoporous silica, preparing method of adsorbent and application of adsorbent in recycling gold |
CN108404970A (en) * | 2018-03-05 | 2018-08-17 | 中国科学院山西煤炭化学研究所 | A kind of apple shape hollow molecules sieve microballoon and its preparation method and application |
CN110183244A (en) * | 2019-06-19 | 2019-08-30 | 长安大学 | A kind of hollow mullite spheroidal material and preparation method thereof |
Non-Patent Citations (2)
Title |
---|
A one-step synthesis of hollow periodic mesoporous organosilica spheres with radially oriented mesochannels;Ning Ma;《CHEMICAL COMMUNICATIONS》;20160128;第52卷;全文 * |
水泥石吸水吸油体积变形性能及其机理;杨瑞芳;《硅酸盐学报》;20170228;第45卷;摘要 * |
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