CN108479728B - Composite drying agent based on quicklime waste residues and preparation method thereof - Google Patents
Composite drying agent based on quicklime waste residues and preparation method thereof Download PDFInfo
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- CN108479728B CN108479728B CN201810236948.5A CN201810236948A CN108479728B CN 108479728 B CN108479728 B CN 108479728B CN 201810236948 A CN201810236948 A CN 201810236948A CN 108479728 B CN108479728 B CN 108479728B
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/28054—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 surface properties or porosity
Abstract
The invention discloses a composite drying agent based on quicklime waste residue and a preparation method thereof, belonging to the field of drying agent preparation, wherein the quicklime waste residue is firstly crushed, mixed with kaolin, added with ethanol, subjected to ball milling and dried to obtain a product A; dissolving the product A in absolute ethyl alcohol, adding polyvinylpyrrolidone, and performing ultrasonic oscillation to obtain a product B; mixing the product B with NaOH, N' -methylene bisacrylamide and ethylene glycol, placing the mixture in a high-temperature reaction kettle for reaction, and centrifuging to obtain a bottom product C; mixing the product C, polyvinyl alcohol and polyethylene glycol, placing the mixture in a high-temperature reaction kettle, and centrifuging to obtain a bottom product D; and the product D is dried in vacuum to obtain the composite drying agent based on the quicklime waste residue, the composite drying agent has good moisture absorption effect, mild reaction after water absorption, uniform size and good safety, the quicklime waste residue is used as a main component, the cost is low, the preparation method is simple, and the composite drying agent is suitable for large-scale production and saves resources.
Description
Technical Field
The invention relates to a composite drying agent, in particular to a composite drying agent based on quicklime waste residues and a preparation method thereof.
Background
The quick lime has good water absorption performance, but as a drying agent, because of strong water absorption, the quick lime can rapidly release heat after absorbing water, a large amount of heat is generated, explosion and fire hazard during storage are easily caused, the safety is poor, the quick lime waste residue also has good water absorption performance but is slightly inferior to the quick lime, polyethylene oxide with ultrahigh molecular weight synthesized by ethylene glycol has more hydroxyl groups, can be grafted on the surface of the quick lime waste residue under the action of a catalyst and a cross-linking agent, has good water solubility and good hygroscopicity, can carry out esterification reaction, is easy to associate electron acceptor groups or automatically oxidize, and a composite drying agent with good water absorption performance and long duration is prepared by wrapping the quick lime waste residue by a high-performance organic material.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides the composite drying agent based on the quicklime waste residue and the preparation method thereof, wherein the composite drying agent has the technical characteristics of no violent water absorption reaction, low cost, simple preparation method, suitability for large-scale production and the like.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the composite desiccant based on the quick lime waste residue comprises the broken quick lime waste residue and kaolin, wherein a shell is wrapped outside the quick lime waste residue and the kaolin, the shell comprises polyethylene oxide formed by polymerizing ethylene glycol, and the molecular weight of the polyethylene oxide is 400000-1000000.
A preparation and drying method of a composite drying agent based on quick lime waste residue comprises the following preparation steps:
step 1): crushing quicklime waste residues into particles with the diameter less than 5mm, wherein the mass ratio of the particles to kaolin is 100: 10-20 to obtain a material, wherein the mass ratio of the materials is as follows: steel ball: the mass ratio of the absolute ethyl alcohol is 2-3: 8: 3-5, then placing the mixture in a ball mill with the rotating speed of 400-500r/min for ball milling for 1-1.5h, and then placing the mixture in a freeze drying condition at the temperature of-45 ℃ to obtain a product A;
step 2): according to the mass parts, 40-60 parts of the product A are dissolved in 200-300 parts of absolute ethyl alcohol, 10-20 parts of polyvinylpyrrolidone is added, and ultrasonic oscillation is carried out for 20-30min to obtain a product B;
step 3): adding NaOH, N' -methylene bisacrylamide and ethylene glycol into the product B obtained in the step 2), placing the mixture in a high-temperature reaction kettle with the pressure of 0.2-0.3MPa, the temperature of 120-;
step 4): adding polyvinyl alcohol and polyethylene glycol into the product C obtained in the step 3), placing the mixture in a high-temperature reaction kettle with the pressure of 0.2-0.4MPa, the temperature of 150-;
step 5): and (3) placing the product D under the conditions of vacuum drying pressure of 45-85Pa and temperature of 15-25 ℃ for vacuum drying to obtain the composite drying agent based on the quicklime waste residue.
As an improvement, the product B in step 3): NaOH: n, N' -methylenebisacrylamide: the mass ratio of the ethylene glycol is 45-50: 1: 5: 10-20.
As an improvement, the product C in step 4): polyvinyl alcohol: the mass ratio of the polyethylene glycol is 100: 3-5: 20-40.
As a modification, the molecular weight of the polyvinylpyrrolidone in the step 2) is 3500-5500.
As an improvement, the molecular weight of the polyethylene glycol in the step 4) is 400-600.
As an improvement, in the step 3), the pressure in the high-temperature high-pressure reaction kettle is 0.2MPa, the temperature is 120 ℃, the stirring speed is 500r/min, and the reaction time is 30 min.
As an improvement, the pressure in the high-temperature high-pressure reaction kettle is 0.3MPa, the temperature is 180 ℃, the stirring speed is 750r/min, and the reaction time is 100 min.
Has the advantages that: the desiccant prepared by the invention overcomes the defect of violent reaction when calcium oxide absorbs water and is dried on the premise of not influencing the moisture absorption performance of quicklime; in the preparation of the drying agent, ethylene glycol is adsorbed on the surfaces of calcium oxide particles, low molecular weight polyethylene glycol is generated by polymerization, the polyethylene glycol combined on different calcium oxide particles is mutually agglomerated, and finally ultra-high molecular weight polyethylene oxide is formed on the surface of quicklime by polymerization, and polyethylene oxide molecules with ultra-high molecular weight have hydrophilicity; the quicklime waste residue is used as a main component, so that the raw material cost is reduced; the preparation method is efficient and suitable for large-scale production; the method has the advantages that quicklime waste residues with wide sources are selected as main components, so that the problem of quicklime waste residue treatment is effectively solved; the organic calcium oxide composite drying agent has the advantages of good moisture absorption effect, mild reaction after water absorption, uniform size and good safety.
Detailed Description
The present invention will be further described with reference to specific embodiments, but the embodiments of the present invention are not limited to the following examples.
Example 1
The utility model provides a compound drier based on quick lime waste residue, compound drier includes quick lime waste residue, the kaolin after the breakage, quick lime waste residue, the outer parcel of kaolin have the shell, the shell includes the polyethylene oxide that the ethylene glycol polymerization formed, polyethylene oxide molecular weight 400000.
A preparation and drying method of a composite drying agent based on quick lime waste residue comprises the following preparation steps:
step 1): crushing quicklime waste residues into particles with the diameter less than 5mm, wherein the mass ratio of the particles to kaolin is 100: 10, mixing to obtain a material, wherein the mass ratio of the materials: steel ball: the mass ratio of the absolute ethyl alcohol is 2: 8: 3, then placing the mixture in a ball mill with the rotating speed of 400r/min for ball milling for 1h, and then placing the mixture in a freeze drying mode at the temperature of minus 45 ℃ to obtain a product A;
step 2): according to the mass parts, 40 parts of the product A are dissolved in 200 parts of absolute ethyl alcohol, 10 parts of polyvinylpyrrolidone with the molecular weight of 3500 are added, and ultrasonic oscillation is carried out for 20min to obtain a product B;
step 3): adding NaOH, N' -methylene bisacrylamide and ethylene glycol into the product B obtained in the step 2), wherein the product B: NaOH: n, N' -methylenebisacrylamide: the mass ratio of the ethylene glycol is 45: 1: 5: 10, mixing, placing in a high-temperature reaction kettle with the pressure of 0.2MPa, the temperature of 120 ℃ and the stirring speed of 500r/min, reacting for 30min, and then placing in a centrifuge with the rotating speed of 5000r/min for centrifuging to obtain a bottom product C;
step 4): adding polyvinyl alcohol and polyethylene glycol with the molecular weight of 400 into the product C obtained in the step 3), wherein the product C: polyvinyl alcohol: the mass ratio of the polyethylene glycol is 100: 3: 20, mixing, placing in a high-temperature reaction kettle with the pressure of 0.2MPa, the temperature of 150 ℃ and the stirring speed of 750r/min, reacting for 60min, then placing in a centrifuge with the rotating speed of 5000r/min, centrifuging to obtain a bottom product D, wherein the preferable air pressure is 0.3MPa, the temperature is 180 ℃, and the stirring speed is 750r/min, and the reaction time is 100 min;
step 5): and (3) placing the product D under the conditions of vacuum drying pressure of 45Pa and temperature of 15 ℃ for vacuum drying to obtain the composite drying agent based on the quicklime waste residue.
Example 2
The utility model provides a compound drier based on quick lime waste residue, compound drier includes quick lime waste residue, the kaolin after the breakage, quick lime waste residue, the outer parcel of kaolin have the shell, the shell includes the polyethylene oxide that the ethylene glycol polymerization formed, the polyethylene oxide molecular weight is 700000.
A preparation and drying method of a composite drying agent based on quick lime waste residue comprises the following preparation steps:
step 1): crushing quicklime waste residues into particles with the diameter less than 5mm, wherein the mass ratio of the particles to kaolin is 100: 15 to obtain a material, according to the material: steel ball: the mass ratio of the absolute ethyl alcohol is 2.5: 8: 4, then placing the mixture in a ball mill with the rotating speed of 450r/min for ball milling for 1.3h, and then placing the mixture in a freeze drying way at the temperature of minus 45 ℃ to obtain a product A;
step 2): according to the mass parts, 50 parts of the product A are dissolved in 250 parts of absolute ethyl alcohol, 15 parts of polyvinylpyrrolidone with the molecular weight of 4500 are added, and ultrasonic oscillation is carried out for 25min to obtain a product B;
step 3): adding NaOH, N' -methylene bisacrylamide and ethylene glycol into the product B obtained in the step 2), wherein the product B: NaOH: n, N' -methylenebisacrylamide: the mass ratio of the ethylene glycol is 47: 1: 5: 15, mixing, placing in a high-temperature reaction kettle with the pressure of 0.25MPa, the temperature of 135 ℃ and the stirring speed of 500r/min, reacting for 45min, and then placing in a centrifuge with the rotating speed of 5000r/min for centrifuging to obtain a bottom product C;
step 4): adding polyvinyl alcohol and polyethylene glycol with the molecular weight of 500 into the product C obtained in the step 3), wherein the product C: polyvinyl alcohol: the mass ratio of the polyethylene glycol is 100: 4: 30, mixing, placing in a high-temperature reaction kettle with the pressure of 0.3MPa, the temperature of 165 ℃ and the stirring speed of 750r/min, reacting for 90min, and then placing in a centrifuge with the rotating speed of 6250r/min for centrifuging to obtain a bottom product D;
step 5): and (3) placing the product D under the conditions of vacuum drying pressure of 65Pa and temperature of 20 ℃ for vacuum drying to obtain the composite drying agent based on the quicklime waste residue.
Example 3
The utility model provides a compound drier based on quick lime waste residue, compound drier includes quick lime waste residue, the kaolin after the breakage, quick lime waste residue, the outer parcel of kaolin have the shell, the shell includes the polyethylene oxide that the ethylene glycol polymerization formed, polyethylene oxide molecular weight is 1000000.
A preparation and drying method of a composite drying agent based on quick lime waste residue comprises the following preparation steps:
step 1): crushing quicklime waste residues into particles with the diameter less than 5mm, wherein the mass ratio of the particles to kaolin is 100: 20 to obtain a material, according to the material: steel ball: the mass ratio of the absolute ethyl alcohol is 2-3): 8: 5, then placing the mixture in a ball mill with the rotating speed of 500r/min for ball milling for 1.5h, and then placing the mixture in a freeze drying mode at the temperature of minus 45 ℃ to obtain a product A;
step 2): according to the mass parts, 60 parts of the product A are dissolved in 300 parts of absolute ethyl alcohol, 20 parts of polyvinylpyrrolidone with the molecular weight of 5500 are added, and ultrasonic oscillation is carried out for 30min to obtain a product B;
step 3): adding NaOH, N' -methylene bisacrylamide and ethylene glycol into the product B obtained in the step 2), wherein the product B: NaOH: n, N' -methylenebisacrylamide: the mass ratio of the ethylene glycol is 50): 1: 5: 20, mixing, placing in a high-temperature reaction kettle with the pressure of 0.3MPa, the temperature of 150 ℃ and the stirring speed of 500r/min, reacting for 60min, then placing in a centrifuge with the rotating speed of 5000r/min, centrifuging to obtain a bottom product C, wherein the preferable air pressure is 0.2MPa, the temperature is 120 ℃, the stirring speed is 500r/min, and the reaction time is 30 min;
step 4): adding polyvinyl alcohol and polyethylene glycol with the molecular weight of 400-600 into the product C obtained in the step 3), wherein the product C: polyvinyl alcohol: the mass ratio of the polyethylene glycol is 100: 5: 40, mixing, placing in a high-temperature reaction kettle with the pressure of 0.4MPa, the temperature of 180 ℃ and the stirring speed of 750r/min, reacting for 120min, then placing in a centrifuge with the rotating speed of 7500r/min, centrifuging to obtain a bottom product D, wherein the preferable air pressure is 0.3MPa, the temperature is 180 ℃, and the stirring speed is 750r/min, and the reaction time is 100 min;
step 5): and (3) placing the product D under the conditions of vacuum drying pressure of 85Pa and temperature of 25 ℃ for vacuum drying to obtain the composite drying agent based on the quicklime waste residue.
Finally, it should be noted that the present invention is not limited to the above embodiments, and many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (2)
1. A preparation method of a composite drying agent based on quick lime waste residue is characterized by comprising the following preparation steps:
step 1): crushing quicklime waste residues into particles with the diameter less than 5mm, wherein the mass ratio of the particles to kaolin is 100: 10-20 to obtain a material, wherein the mass ratio of the materials is as follows: steel ball: the mass ratio of the absolute ethyl alcohol is 2-3: 8: 3-5, then placing the mixture in a ball mill with the rotating speed of 400-500r/min for ball milling for 1-1.5h, and then placing the mixture in a freeze drying condition at the temperature of-45 ℃ to obtain a product A;
step 2): according to the mass parts, 40-60 parts of the product A are dissolved in 200-300 parts of absolute ethyl alcohol, 10-20 parts of polyvinylpyrrolidone is added, and ultrasonic oscillation is carried out for 20-30min to obtain a product B; the molecular weight of the polyvinylpyrrolidone is 3500-5500;
step 3): adding NaOH, N' -methylene bisacrylamide and ethylene glycol into the product B obtained in the step 2), placing the mixture in a high-temperature reaction kettle with the pressure of 0.2-0.3MPa, the temperature of 120-; the product B: NaOH: n, N' -methylenebisacrylamide: the mass ratio of the ethylene glycol is 45-50: 1: 5: 10-20 parts of; the air pressure in the high-temperature high-pressure reaction kettle is 0.2MPa, the temperature is 120 ℃, the stirring speed is 500r/min, and the reaction time is 30 min;
step 4): adding polyvinyl alcohol and polyethylene glycol into the product C obtained in the step 3), placing the mixture in a high-temperature reaction kettle with the pressure of 0.2-0.4MPa, the temperature of 150-; and (3) a product C: polyvinyl alcohol: the mass ratio of the polyethylene glycol is 100: 3-5: 20-40 parts of; the molecular weight of the polyethylene glycol is 400-600;
step 5): putting the product D under the conditions of vacuum drying pressure of 45-85Pa and temperature of 15-25 ℃ for vacuum drying to obtain a composite drying agent based on quicklime waste residues;
the composite drying agent comprises crushed quicklime waste residue and kaolin, wherein a shell is wrapped outside the quicklime waste residue and the kaolin, the shell comprises polyethylene oxide formed by polymerizing ethylene glycol, and the molecular weight of the polyethylene oxide is 400000-1000000.
2. The method for preparing the composite drying agent based on the quicklime waste residue as claimed in claim 1, wherein in the step 4), the pressure in the high-temperature high-pressure reaction kettle is 0.3MPa, the temperature is 180 ℃, and the reaction time is 100min at the stirring speed of 750 r/min.
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| CN109395778B (en) * | 2018-11-13 | 2021-10-22 | 北京林业大学 | Niobium phytate supported nano metal catalytic system for levulinic acid and ester hydrogenation |
| CN110451543A (en) * | 2019-09-01 | 2019-11-15 | 浙江理工大学 | A kind of preparation method based on carbon nano tube modified modified quicklime desiccant |
| CN114130169A (en) * | 2021-12-10 | 2022-03-04 | 安徽前江超细粉末科技有限公司 | Method for improving safety of lime drying agent |
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| WO2010083337A3 (en) * | 2009-01-15 | 2010-11-25 | The Regents Of The University Of Califorinia | Composite nanostructures and methods for making and using them |
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