CN113003593A - Method for preparing micron-sized granular aluminum oxide by taking guar gum as template - Google Patents
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Abstract
The invention discloses a method for preparing micron-sized granular alumina by taking guar gum as a template, which comprises the following steps: adding aluminum chloride hexahydrate and ethyl acetoacetate into an ethanol aqueous solution at the same time, and dispersing to obtain a yellowish solution A; gradually dropwise adding a sulfanilamide solution into the solution A, and then dropwise adding a mixed solution of guar gum, ammonia water and deionized water into the solution to obtain a colloidal solution B; the solution B is moved to a microwave ultrasonic hydrothermal synthesizer for ultrasonic reaction, and a product solution C is obtained by collection; vacuum freeze drying the product C and collecting white solid D; sintering the white solid D and naturally cooling to room temperature to obtain micron-sized granular alumina; according to the method, the natural space structure in the guar gum is used for inducing the alumina crystal grains to grow along the specific orientation direction, the uniform and efficient growth of micron-grade alumina crystal grains in solution reaction is realized by means of microwave ultrasonic hydrothermal synthesis reaction, the method is simple and easy, the cost is low, the product purity is high, and the orientation is good.
Description
Technical Field
The invention belongs to the field of materials, and particularly relates to a method for preparing micron-sized granular alumina by taking guar gum as a template.
Background
Biomass materials refer to various organisms formed by photosynthesis, including all animals, plants, and microorganisms, and so on, which play an important role in the overall energy system. Through natural evolution for hundreds of millions of years, the biomass material generally forms microstructures with different shapes, colors and sizes, such as hexagonal multilayer nests of bees, hollow structures of guar gum and the like. [ S.Sathish, M.Geetha, A.Udayakumar, S.senthi Kumar, R.Asokamani.Granulation of Nano aluminum Powder for Improved mobility by Spray Drying [ J ]. Transactions of the Indian Institute of Metals,2018,65(5) ]
In the research of materials science, the microstructure of a substance determines the functionality of the substance. Therefore, in the current research on the preparation of alumina powder, various biomass material structures are generally used as the objects to be researched for building microstructures, but the research on the production of alumina powder by directly introducing biomass materials as template is less limited to generating specific material structures by regulating experimental conditions. [ Taheri Nassaj. Economical synthesis of nano-alumina powder using an aqueous sol-gel method [ J ]. Materials Letters,2020,62(19) ]
In order to prepare alumina powder with controllable appearance and stable property, scientific researchers develop a key on the development of production and preparation technologies and equipment, and in recent years, a plurality of preparation means such as a micro-emulsion method, a detonation method, a precipitation method, a sol-gel method and the like are successfully explored. Therefore, exploring a micro-nano alumina production technology with low cost and high practicability becomes an objective that many scientific researchers are dedicated to achieve. [ Bhattacharyya. Nano aluminum: A Review of Powder Synthesis method [ J ]. Refractories Manual,2016,65(1): 10-16.)
Disclosure of Invention
The invention aims to provide a method for preparing micron-sized granular alumina by taking guar gum as a template, which is simple and has low cost, high product purity and good orientation.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing micron-sized granular alumina by taking guar gum as a template is characterized by comprising the following steps:
the method comprises the following steps: adding 3.2-5.4 g of aluminum chloride hexahydrate and 6.2-7.8 g of ethyl acetoacetate into 30-50 mL of 1.5-2.0 mol/L ethanol aqueous solution at the same time, and dispersing to obtain a yellowish solution A;
step two: gradually dropwise adding 0.6-1.5 mol/L sulfanilamide solution into the yellowish solution A, stirring while dropwise adding until the yellowish solution just disappears, and dropwise adding guar gum with the mass ratio: ammonia water: deionized water (8-12): (1-3): (16-20) heating the mixed solution until the pH value is 8.2-9.2, and then magnetically stirring to obtain a colloidal solution B;
step three: and (3) filling the solution B with a polytetrafluoroethylene lining, moving the solution B into a microwave ultrasonic hydrothermal synthesizer, and setting the following components to react for 6-9 h in two stages: the temperature of the first stage is 60-100 ℃, the ultrasonic frequency is 20-40 KHz, and the reaction time is 1-2 h; the temperature of the second stage is 160-200 ℃, the ultrasonic frequency is 40-60 KHz, the reaction time is 5-7 h, and finally, a product solution C is collected;
step four: and (3) pouring out the upper layer turbid liquid of the product solution C, washing the obtained product, and then placing the product in a vacuum freeze dryer to react for 12-18 h in two stages according to the following system: the temperature of the first stage is-50 to-20 ℃, and the freezing time is 2 to 4 hours; the vacuum degree of the second stage is-20 to-10 Pa, the drying time is 10 to 14 hours, and finally white agglomerated solid D can be obtained by collection;
step five: uniformly mixing the solid D and 5.2-5.8 g of aluminum potassium fluoride, transferring the mixture into a muffle furnace, heating the mixture from room temperature to 400-600 ℃ at a heating rate of 6-10 ℃/min, keeping the temperature for 0.5-1 h, heating the mixture to 1100-1300 ℃ at a heating rate of 5-8 ℃/min, keeping the temperature for 0.5-2 h, naturally cooling the mixture to room temperature, and washing and drying the mixture to obtain micron-sized granular aluminum oxide.
Further, in the first step, a yellowish solution A is obtained by ultrasonic dispersion for 10-20 min at the temperature of 40-60 ℃.
Further, in the second step, heating and magnetically stirring at a stirring speed of 300-500 r/min at a temperature of 160-200 ℃ for 20-30 min to obtain a colloidal solution B.
Further, washing the product obtained in the fourth step with deionized water and ethanol sequentially for 8 times until the pH value is 7.0-8.0, and then freeze-drying.
And further, drying the aluminum oxide particles in an ultraviolet oven at the temperature of 60-80 ℃ for 12-18 h to obtain the micron-sized granular aluminum oxide.
And further, collecting the product in the fifth step, washing the product for 6 times by using deionized water and ethanol in sequence, and drying the product in an ultraviolet oven at the temperature of 60-80 ℃ for 12-18 hours to obtain the micron-sized granular aluminum oxide.
The invention prepared by the process method has the following beneficial effects:
according to the invention, the guar gum which is a biomass raw material with wide natural reserves is used as a template, and a micro-nano granular space structure which is naturally formed in the guar gum is used as a growth template of the alumina seed crystal. Compared with the chemical template agents such as polyethylene glycol and the like which are commonly used at present, the guar gum template agent has the advantages of easily available raw materials, environment-friendly and eco-friendly product, lower production and manufacturing cost, simple production process, capability of perfectly conforming to the national policy requirements on energy conservation and environmental protection, and potential for realizing large-scale production.
In addition, the existing micro-nano-grade alumina preparation technology is mainly completed by a one-step precipitation method such as a microemulsion method, a hydrothermal method and the like, and alumina seed crystals have the defects of low yield, poor growth orientation and the like. Meanwhile, the double precipitating agents with better chemical inertness are introduced, so that the occurrence of side reactions in the system is reduced, the stability of the preparation technology and the purity of the product are improved, and the method has better popularization value and application prospect technically.
The invention also has the following five beneficial effects:
firstly, adding precipitant ethyl acetoacetate and aluminum source aluminum chloride hexahydrate into an ethanol water solution, and successfully realizing the dissolution of a double-precipitant microemulsion system under the condition of skillfully controlling a heating centrifugal stirring process by utilizing the principle that a binding layer is formed by utilizing the intermiscibility of surfactant p-aminobenzenesulfonamide to ethyl acetoacetate and hydrophilic groups. Compared with a single precipitant, the two precipitants are introduced to effectively improve the precipitation efficiency of the product alumina seed crystal, improve the precipitation width of the reaction and the purity of the precipitated alumina seed crystal, and the improvement of the solution reaction efficiency is also beneficial to the uniform precipitation of the micro-nano alumina seed crystal.
The introduced ethyl acetoacetate and sulfanilamide contain various heterogeneous functional groups such as amino, carbonyl and the like, and various functional groups can be subjected to a bonding reaction of free chemical bonds with weakly alkaline guar gum, so that abundant attachment points are provided for the double precipitant in a micro-nano structure inside the guar gum, the double precipitant is ensured to successfully enter the template, and alumina seed crystals with specific orientation are separated, separated and grown at specific spatial points, the incidence rate of non-template precipitation reaction in the solution is reduced, and the yield of the micro-nano-scale oriented granular alumina seed crystals is improved.
And (III) a two-in-one microwave ultrasonic homogeneous reaction system is constructed, hydrothermal reaction and microwave ultrasonic reaction are organically combined, effective collision of reaction particles and uniform dispersion of products in the thermal motion process are promoted by controlling ultrasonic frequency, the reaction efficiency is improved while the process operation steps are simplified, and the target product loss possibly existing in the multi-step reaction process is reduced. Meanwhile, the temperature control step of the two-in-one microwave ultrasonic homogeneous reaction in the first stage effectively ensures the dissolution amount of guar gum in the reaction solution, provides a material basis for uniform precipitation and directional growth of alumina seed crystals attached to a template in the main reaction in the second stage, and ensures the yield of the micro-nano granular alumina seed crystals.
And (IV) designing a 'two-step' vacuum freeze-drying process, wherein the 'two-step' vacuum freeze-drying process can remove liquid water in the system in a sublimed form after solidifying compared with the conventional process in which the drying is carried out in an oven. And solid water is compared with liquid water, the internal hydrogen bond acting force is smaller, uncontrollable agglomeration of the micro-nano granular alumina seed crystals due to the strong interaction force of the hydrogen bonds is reduced, the dispersibility of the alumina seed crystals is improved, and therefore the alumina seed crystals are not required to be dispersed by subsequent physical methods such as ultrasonic dispersion and the like, the preparation flow is effectively shortened, the preparation cost is saved, and the production efficiency is improved.
And (V) introducing aluminum potassium fluoride in the 'two-step' muffle furnace reaction to provide guidance for the oriented growth of alumina seed crystals, efficiently promoting the crystal form transformation process of the alumina and the generation of micro-nano granular alumina under the combined action of a template agent, ammonia gas and fluoride, improving the reaction efficiency, and avoiding abnormal growth of crystal grains caused by long-time high-temperature solid-phase reaction.
Drawings
FIG. 1 is a scanning electron microscope test chart of micron-sized spherical alumina prepared in example 1 of the present invention
FIG. 2 is an X-ray diffraction pattern of micron-sized spherical alumina prepared in example 1 of the present invention
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are not intended to limit the invention thereto.
Example 1:
the method comprises the following steps: simultaneously adding 3.2g of aluminum chloride hexahydrate and 6.2g of ethyl acetoacetate into 30mL of ethanol aqueous solution with the concentration of 1.5mol/L, and performing ultrasonic dispersion at the temperature of 40 ℃ for 20min to obtain a yellowish solution A;
step two: gradually dropwise adding 0.6mol/L p-aminobenzene sulfonamide solution into the yellowish solution A, stirring while dropwise adding until the yellowish solution just disappears, and then dropwise adding guar gum with the mass ratio: ammonia water: deionized water 8: 1: 16 until the pH value is 8.2, and finally heating the mixed solution at the temperature of 160 ℃ and stirring at the stirring speed of 300r/min and magnetically stirring for 30min to obtain a colloidal solution B;
step three: and (3) filling the solution B with a polytetrafluoroethylene lining, moving the solution B into a microwave ultrasonic hydrothermal synthesizer, and setting the following components to react for 9 hours in two stages: the temperature of the first stage is 60 ℃, the ultrasonic frequency is 20KHz, and the reaction time is 2 h; the temperature of the second stage is 160 ℃, the ultrasonic frequency is 40KHz, the reaction time is 7h, and finally, the product solution C is collected;
step four: and (3) pouring the upper turbid liquid of the product solution C, washing the obtained product with deionized water and ethanol for 8 times in sequence until the pH value is 7.0, and then placing the product in a vacuum freeze dryer to react for 12 hours in two stages according to the following system: the temperature of the first stage is-50 ℃, and the freezing time is 2 h; the vacuum degree of the second stage is-20 Pa, the drying time is 10h, and finally white agglomerated solid D can be obtained by collection;
step five: uniformly mixing the solid D and 5.2g of aluminum potassium fluoride, transferring the mixture into a muffle furnace, heating the mixture from room temperature to 400 ℃ at the heating rate of 6 ℃/min, keeping the temperature for 1h, then heating the mixture to 1100 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 2h, then naturally cooling the mixture to room temperature, collecting a product after the reaction is finished, washing the product with deionized water and ethanol for 6 times in sequence, and finally drying the product in an ultraviolet oven at 60 ℃ for 18h to obtain micron-sized granular aluminum oxide.
Example 2:
the method comprises the following steps: simultaneously adding 4.5g of aluminum chloride hexahydrate and 7.0g of ethyl acetoacetate into 40mL of ethanol aqueous solution with the concentration of 1.8mol/L, and performing ultrasonic dispersion at the temperature of 50 ℃ for 15min to obtain a yellowish solution A;
step two: gradually dropwise adding 1.0mol/L p-aminobenzene sulfonamide solution into the yellowish solution A, stirring while dropwise adding until the yellowish solution just disappears, and then dropwise adding guar gum with the mass ratio: ammonia water: deionized water 10: 2: 20 until the pH value is 8.6, and finally heating and magnetically stirring the mixed solution at the temperature of 180 ℃ at the stirring speed of 400r/min for 25min to obtain a colloidal solution B;
step three: and (3) filling the solution B with a polytetrafluoroethylene lining, moving the solution B into a microwave ultrasonic hydrothermal synthesizer, and setting the following components to react for 7.5 hours in two stages: the temperature of the first stage is 80 ℃, the ultrasonic frequency is 30KHz, and the reaction time is 1.5 h; the temperature of the second stage is 180 ℃, the ultrasonic frequency is 50KHz, the reaction time is 6h, and finally, the product solution C is collected;
step four: and (3) pouring the upper-layer turbid liquid of the product solution C, washing the obtained product with deionized water and ethanol for 8 times in sequence until the pH value is 7.5, and then placing the product in a vacuum freeze dryer to react for 15 hours in two stages according to the following components: the temperature of the first stage is-30 ℃, and the freezing time is 3 h; the vacuum degree of the second stage is-15 Pa, the drying time is 12h, and finally white agglomerated solid D can be obtained by collection;
step five: uniformly mixing the solid D and 5.5g of aluminum potassium fluoride, transferring the mixture into a muffle furnace, heating the mixture from room temperature to 500 ℃ at the heating rate of 8 ℃/min, keeping the temperature for 0.8h, then heating the mixture to 1200 ℃ at the heating rate of 6 ℃/min, keeping the temperature for 1h, then naturally cooling the mixture to room temperature, collecting a product after the reaction is finished, washing the product with deionized water and ethanol for 6 times in sequence, and finally drying the product in an ultraviolet oven at 70 ℃ for 15h to obtain micron-sized granular aluminum oxide.
Example 3:
the method comprises the following steps: simultaneously adding 5.4g of aluminum chloride hexahydrate and 7.8g of ethyl acetoacetate into 50mL of 2.0mol/L ethanol aqueous solution, and performing ultrasonic dispersion at the temperature of 60 ℃ for 10min to obtain a yellowish solution A;
step two: gradually dropwise adding 1.5mol/L p-aminobenzene sulfonamide solution into the yellowish solution A, stirring while dropwise adding until the yellowish solution just disappears, and then dropwise adding guar gum with the mass ratio: ammonia water: deionized water 12: 3: the pH value of the mixed solution of 18 is 9.2, and finally the colloidal solution B is obtained by heating and magnetic stirring at the temperature of 200 ℃ and the stirring speed of 500r/min for 20 min;
step three: and (3) filling the solution B with a polytetrafluoroethylene lining, moving the solution B into a microwave ultrasonic hydrothermal synthesizer, and setting the following components to react for 6 hours in two stages: the temperature of the first stage is 100 ℃, the ultrasonic frequency is 40KHz, and the reaction time is 1 h; the temperature of the second stage is 200 ℃, the ultrasonic frequency is 60KHz, the reaction time is 5h, and finally, the product solution C is collected;
step four: and (3) pouring the upper layer turbid liquid of the product solution C, washing the obtained product with deionized water and ethanol for 8 times in sequence until the pH value is 8.0, and then placing the product in a vacuum freeze dryer to react for 18 hours in two stages according to the following system: the temperature of the first stage is-20 ℃, and the freezing time is 4 h; the vacuum degree of the second stage is-10 Pa, the drying time is 14h, and finally white agglomerated solid D can be obtained by collection;
step five: uniformly mixing the solid D and 5.8g of aluminum potassium fluoride, transferring the mixture into a muffle furnace, heating the mixture from room temperature to 600 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 0.5h, then heating the mixture to 1300 ℃ at the heating rate of 8 ℃/min, keeping the temperature for 0.5h, then naturally cooling the mixture to room temperature, collecting a product after the reaction is finished, washing the product with deionized water and ethanol for 6 times in sequence, and finally drying the product in an ultraviolet oven at 80 ℃ for 12h to obtain the micron-sized granular aluminum oxide.
Fig. 1 is a scanning electron microscope test chart of the micron-sized particulate alumina prepared in example 1. From fig. 1, it can be seen that the micron-sized alumina is uniformly dispersed, the agglomeration among the particles is less, the particles are in spherical orientation in appearance, and the abnormal growth of alumina grains does not occur, which indicates that example 1 successfully synthesizes micron-sized granular alumina by using guar gum as a template.
Figure 2 is an X-ray diffraction pattern of micron-sized particulate alumina prepared in example 1. From fig. 2 it can be seen that the X-ray diffraction pattern of the substance has sharp peaks, indicating a higher purity and crystallinity of the substance. Next, the diffraction angles of 25.58 °, 35.16 °, 43.47 °, 52.55 °, 57.56 °, 66.76 ° and 68.42 ° corresponded to characteristic peak positions of alumina, and it was verified that the produced substance was alumina.
The micron-sized particulate alumina product prepared using the dual precipitant from example 3 was collected, weighed, and calculated to yield comparative data as shown in table 1 below:
table 1 comparison of yields of example 3 and blank samples
The blank sample mentioned in the table above is micron-sized spherical alumina prepared by introducing only one precipitant, ethyl acetoacetate, in accordance with the method of example 3. Compared with a single precipitant, the precipitation efficiency of the product alumina seed crystal can be effectively improved by introducing the two precipitants, the precipitation width and the yield of the target product are improved, and the technology has certain guiding significance and popularization value for actual production.
The present invention is described in detail with reference to the above embodiments, and those skilled in the art will understand that: modifications and equivalents may be made to the embodiments of the invention without departing from the spirit and scope of the invention, which is to be covered by the claims.
Claims (6)
1. A method for preparing micron-sized granular alumina by taking guar gum as a template is characterized by comprising the following steps:
the method comprises the following steps: adding 3.2-5.4 g of aluminum chloride hexahydrate and 6.2-7.8 g of ethyl acetoacetate into 30-50 mL of 1.5-2.0 mol/L ethanol aqueous solution at the same time, and dispersing to obtain a yellowish solution A;
step two: gradually dropwise adding 0.6-1.5 mol/L sulfanilamide solution into the yellowish solution A, stirring while dropwise adding until the yellowish solution just disappears, and dropwise adding guar gum with the mass ratio: ammonia water: deionized water (8-12): (1-3): (16-20) heating the mixed solution until the pH value is 8.2-9.2, and then magnetically stirring to obtain a colloidal solution B;
step three: and (3) filling the solution B with a polytetrafluoroethylene lining, moving the solution B into a microwave ultrasonic hydrothermal synthesizer, and setting the following components to react for 6-9 h in two stages: the temperature of the first stage is 60-100 ℃, the ultrasonic frequency is 20-40 KHz, and the reaction time is 1-2 h; the temperature of the second stage is 160-200 ℃, the ultrasonic frequency is 40-60 KHz, the reaction time is 5-7 h, and finally, a product solution C is collected;
step four: and (3) pouring out the upper layer turbid liquid of the product solution C, washing the obtained product, and then placing the product in a vacuum freeze dryer to react for 12-18 h in two stages according to the following system: the temperature of the first stage is-50 to-20 ℃, and the freezing time is 2 to 4 hours; the vacuum degree of the second stage is-20 to-10 Pa, the drying time is 10 to 14 hours, and finally white agglomerated solid D can be obtained by collection;
step five: uniformly mixing the solid D and 5.2-5.8 g of aluminum potassium fluoride, transferring the mixture into a muffle furnace, heating the mixture from room temperature to 400-600 ℃ at a heating rate of 6-10 ℃/min, keeping the temperature for 0.5-1 h, heating the mixture to 1100-1300 ℃ at a heating rate of 5-8 ℃/min, keeping the temperature for 0.5-2 h, naturally cooling the mixture to room temperature, and washing and drying the mixture to obtain micron-sized granular aluminum oxide.
2. The method for preparing micron-sized granular aluminum oxide by using guar gum as a template according to claim 1, wherein in the first step, the micro-yellow solution A is obtained by ultrasonic dispersion at the temperature of 40-60 ℃ for 10-20 min.
3. The method for preparing micron-sized granular aluminum oxide by using guar gum as a template according to claim 1, wherein in the second step, the colloidal solution B is obtained by heating and magnetic stirring at a stirring speed of 300-500 r/min at a temperature of 160-200 ℃ for 20-30 min.
4. The method for preparing micron-sized granular aluminum oxide by using guar gum as a template according to claim 1, wherein in the fourth step, the obtained product is sequentially washed with deionized water and ethanol for 8 times until the pH value is 7.0-8.0, and then is freeze-dried.
5. The method for preparing micron-sized granular alumina by using guar gum as a template according to claim 1, wherein in the fifth step, the micron-sized granular alumina is obtained by drying in an ultraviolet oven at 60-80 ℃ for 12-18 h.
6. The method for preparing micron-sized granular alumina by using guar gum as a template according to claim 1, wherein the product is collected in the fifth step, washed by deionized water and ethanol for 6 times in sequence, and dried in an ultraviolet oven at 60-80 ℃ for 12-18 hours to obtain the micron-sized granular alumina.
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