CN101818028A - Process method for preparing aluminum trioxide-based polishing powder by solid-solid phase synthesis - Google Patents

Process method for preparing aluminum trioxide-based polishing powder by solid-solid phase synthesis Download PDF

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Publication number
CN101818028A
CN101818028A CN200910153569A CN200910153569A CN101818028A CN 101818028 A CN101818028 A CN 101818028A CN 200910153569 A CN200910153569 A CN 200910153569A CN 200910153569 A CN200910153569 A CN 200910153569A CN 101818028 A CN101818028 A CN 101818028A
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China
Prior art keywords
polishing powder
solid
product
precursor
aluminum nitrate
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CN200910153569A
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柴春芳
刘金库
连加松
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ZHEJIANG ULTRAFINE POWDER&CHEMICALS CO Ltd
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ZHEJIANG ULTRAFINE POWDER&CHEMICALS CO Ltd
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Priority to CN200910153569A priority Critical patent/CN101818028A/en
Publication of CN101818028A publication Critical patent/CN101818028A/en
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Abstract

The invention relates to a technical method for aluminum trioxide-based polishing powder, which is characterized by comprising the following steps of: preparing the aluminum trioxide-based polishing powder by adopting a solid-solid phase synthesis method, using solid aluminum nitrate as main raw materials, adding organic acid, which is 2.5 to 10 percent of the mass of the aluminum nitrate, serving as an oxidizer; adding surfactant, which is 0.1 to 1 percent of the total mass of the aluminum nitrate and the organic acid, serving as a dispersing agent, and uniformly grinding; after drying the grinded mixture at the temperature of between 70 and 100 DEG C for 2 to 6 hours, obtaining a precursor of the target product; putting the precursor into a muffle furnace, slowly heating to the temperature of between 950 and 1,300 DEG C, calcining for 0.5 to 2 hours, naturally cooling, and crushing by using air flow or performing ball milling to obtain the alumina product. The process method has the advantages of no application of solvent, no water liquor discharge, simple technical process, low energy consumption, and the like, and accords with the requirement on green chemistry. The product obtained by the technology can be applied to surface polishing of pearls, agates, artware, disk surfaces and other materials.

Description

A kind of processing method of aluminum trioxide-based polishing powder by solid-solid phase synthesis
Technical field
The invention belongs to the materials chemistry field, be specifically related to a kind of processing method of aluminum trioxide-based polishing powder by solid-solid phase synthesis.This polishing powder can be used for the surface finish of materials such as pearl, agate, artwork, CD to be handled.
Background technology
Along with high-tech development, polishing powder is widely used in the polishing field of high-tech area and high-accuracy functional material, as manufacturing of the photomask in photoelectricity information material, the unicircuit, high density recording disk glass substrate etc.In order to reach the desired configuration of surface of high-accuracy functional material, the rerum natura of polishing powder product is also had higher requirement, its preparation technology is also correspondingly changing.China's polishing powder industry also exists problems at aspects such as preparation technology, performance and application at present, therefore, explore the novel polishing powder of a class, study the emphasis that mutual relationship between their character, optimum matching, optimum process condition etc. just become the research of polishing powder industry technology in great detail.Simultaneously, the task of top priority that along with China constantly strengthens environmental consciousness and energy consciousness, explore that a class production technique is simple, production and use environmental protection, product performance are stable and production cost is low, consumption is a few class polishing powder has become the polishing powder industry.
α type aluminium sesquioxide super-fine material has stable, the advantages such as hardness is high, narrow size distribution of crystalline phase, be widely used in the strengthening and toughening of products such as various plastics, rubber, pottery, refractory materials, the wear resisting property that particularly improves ceramic compactness, smooth finish, cold and hot fatigability, fracture toughness property, creep-resistant property and macromolecular material product is particularly remarkable.In recent years, the aluminium sesquioxide material is applied in the polishing material field, many excellent properties have been shown, cerium oxide base polishing material with domestic and international main flow is compared, has hardness, easier conciliation such as size, narrow diameter distribution, the light and controlled amount of density, characteristics such as cost is lower if replace or partly replace the cerium oxide base polishing material of main flow with it, then can obtain better polishing effect, and raw material and low production cost, reach polishing powder amount that same polishing effect consumes still less, can bring economic benefit and social benefit thus, meet the economic strategy of the current Sustainable development of China.
Industrial preparation α-Al 2O 3The method of material mainly contains bayer's process, sintering process and connects the method for mixing, and there is matter crystal internal defect mostly in the product that these methods obtain, can not use as polishing powder.Sol-gel method, reverse microemulsion process, detonation method, hydrothermal synthesis method etc. are often adopted in the laboratory, but these methods only rest on the experimental exploring stage mostly, and process repeatability is poor, combined coefficient is low, the product crystalline form is single; The facility investment of some method and maintenance cost exceed and poor stability, are difficult to realize industrialization; The method that also has exists complex process, condition harshness, has used a large amount of organic solvents, produces problems such as severe contamination, is seriously fettering promoting the use of of aluminium sesquioxide based relief polishing powder.And, because the polishing powder industry is to the size distribution of polishing powder, hardness, suspension, indexs such as density all have special requirement, and different Application Areass requires also different, therefore, realize control to These parameters, must carry out major tuneup to existing aluminium sesquioxide production technique, each factor that influences These parameters is in depth inquired into, from physics, chemistry, chemical industry, material, many science such as surface and colloid angle is set out, deeply inquire into the internal mechanism that product forms, to preparation condition, processing parameter is summarized to product control of physical properties rule, in conjunction with practical production experience, explore a modern aluminium sesquioxide based relief polishing powder production technique, it is controlled to reach the product rerum natura, high efficiency of energy is utilized, the production process environmental protection, requirements such as product performance are stable.
Summary of the invention
The method that the purpose of this invention is to provide the synthetic aluminium sesquioxide based relief polishing powder of a kind of efficient low-consume.Adopt preparation method of the present invention, the aluminium sesquioxide based relief polishing powder that is obtained has characteristics such as uniform particle diameter, good dispersity and hardness height under hot conditions.Simultaneously, present method is not used any solvent, can save resource, reduces the pollution to environment, meets the Green Chemistry requirement.
The present invention adopts the solid phase combustion reactions to make aluminium sesquioxide based relief polishing powder product, and concrete steps are: to contain aluminium salt as the aluminium source, add organism as ignition dope, add tensio-active agent as dispersion agent, by obtaining precursor behind the mill-drying.Precursor high-temperature calcination with obtaining obtains last product.According to the requirement of different field to aspects such as the size of polishing powder, distribution of sizes, hardness, density, surface charge situation, suspensions, adjust proportion of raw materials, can realize artificial adjustments such as globule size, distribution and product shapes.
The present invention specifically realizes as follows:
1) take by weighing a certain amount of aluminum nitrate, the tensio-active agent that adds the 0.1-1% that accounts for the aluminum nitrate quality stirs as dispersion agent;
2) in system, add account for the aluminum nitrate quality 2.5~10% organic molecule as ignition dope, and fully grind, system is uniformly dispersed;
3) with said mixture at 70-100 ℃ down behind the oven dry 2-6h, obtain the precursor of target product;
4) with after the precursor drying, change in the crucible, put into retort furnace, slowly be warmed up to 950-1300 ℃, calcining 0.5-2h, naturally cooling behind micronizer mill pulverizing or ball mill ball milling, promptly obtains the aluminium sesquioxide based relief polishing powder.
Beneficial effect
Preparation method of the present invention has following advantage:
1, realizes the efficient low-consume production of aluminium sesquioxide based relief polishing powder, do not use any solvent, no discharging of waste liquid, energy consumption low in process of production, low production cost.
2, a series of stable performances, good dispersity, uniform particle diameter, pure phase aluminium sesquioxide based relief polishing powder that hardness is high have been obtained by the solid phase combustion reactions, the particle diameter of product and shape are artificially controlled, can be applied to fields such as crystal, glass, jewel, precise materials.
Embodiment
The present invention is further illustrated below by specific embodiment.
Embodiment 1:
Take by weighing aluminum nitrate 100g as the aluminium source, add the 0.1g polyoxyethylene glycol, after stirring, add the 10g glycine again as ignition dope, agitation grinding obtains precursor.Oven dry under 100 ℃ of conditions of precursor after 2 hours, was calcined 1 hour down at 1000 ℃ again.Naturally cooling is pulverized with ball mill, promptly obtains the aluminium sesquioxide based relief polishing powder, and the particle diameter of this product is about 100nm.
Embodiment 2:
Take by weighing aluminum nitrate 100g as the aluminium source, add 0.1g Triton x-100, after stirring, add the acid of 5g oxalic acid again as ignition dope, agitation grinding obtains precursor.Oven dry under 90 ℃ of conditions of precursor after 5 hours, was calcined 1 hour down at 950 ℃ again.Naturally cooling is pulverized with micronizer mill, promptly obtains the aluminium sesquioxide based relief polishing powder, and the particle diameter of this product is about 90nm.
Embodiment 3
Take by weighing aluminum nitrate 100g as the aluminium source, add 0.5g Triton x-100, after stirring, add the 10g citric acid again as ignition dope, agitation grinding obtains precursor.Oven dry under 70 ℃ of conditions of precursor after 6 hours, was calcined 0.5 hour down at 1000 ℃ again.Naturally cooling is pulverized with micronizer mill, promptly obtains the aluminium sesquioxide based relief polishing powder, and the particle diameter of this product is about 60nm.
Embodiment 4
Take by weighing aluminum nitrate 100g as the aluminium source, add 1g soil temperature-60, after stirring, add the 2.5g lauric acid again as ignition dope, agitation grinding obtains precursor.Oven dry under 90 ℃ of conditions of precursor after 5 hours, was calcined 2 hours down at 1300 ℃ again.Naturally cooling is pulverized with ball mill, promptly obtains the aluminium sesquioxide based relief polishing powder, and the particle diameter of this product is about 100nm.

Claims (4)

1. the preparation method of an aluminium sesquioxide based relief polishing powder, its spy are to adopt the method for solid-solid phase synthesis to be prepared, and concrete steps are:
Take by weighing a certain amount of aluminum nitrate, add account for aluminum nitrate quality 2.5-10% organic acid as ignition dope, the tensio-active agent that adds the 0.1-1% that accounts for the above two quality summations again grinds evenly as dispersion agent; Mixture after grinding behind oven dry 2-6h under 70-100 ℃, is obtained the precursor of target product; Precursor is put into retort furnace, slowly be warming up to 950-1300 ℃, calcining 0.5-2h, naturally cooling behind comminution by gas stream or ball milling, promptly obtains product.
2. the preparation method of aluminium sesquioxide based relief polishing powder as claimed in claim 1 is characterized in that described small-molecule substance ignition dope is an oxalic acid, glycine, citric acid, lauric acid or its mixture.
3. aluminium sesquioxide based relief polishing powder preparation method as claimed in claim 1 is characterized in that described tensio-active agent is nonionogenic tenside or cats product.
4. the preparation method of aluminium sesquioxide based relief polishing powder as claimed in claim 1 is characterized in that the pulverizing of product adopts ball mill or micronizer mill to realize.
CN200910153569A 2009-10-20 2009-10-20 Process method for preparing aluminum trioxide-based polishing powder by solid-solid phase synthesis Pending CN101818028A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103952083A (en) * 2014-04-09 2014-07-30 贵州亿科新材料有限公司 Method for producing polishing powder by hard kaolin
CN114940886A (en) * 2022-04-28 2022-08-26 浙江大学 Nano alumina abrasive particle, preparation method and application thereof, and silicon carbide polishing solution containing abrasive particle

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4011099A (en) * 1975-11-07 1977-03-08 Monsanto Company Preparation of damage-free surface on alpha-alumina
US20020055324A1 (en) * 2000-09-21 2002-05-09 Wacker Siltronic Gesellschaft Fur Halbleitermaterialien Ag Process for polishing silicon wafers
US6494928B1 (en) * 2001-05-25 2002-12-17 Minebea Co., Ltd. Polishing compound for sheet metal coating

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4011099A (en) * 1975-11-07 1977-03-08 Monsanto Company Preparation of damage-free surface on alpha-alumina
US20020055324A1 (en) * 2000-09-21 2002-05-09 Wacker Siltronic Gesellschaft Fur Halbleitermaterialien Ag Process for polishing silicon wafers
US6494928B1 (en) * 2001-05-25 2002-12-17 Minebea Co., Ltd. Polishing compound for sheet metal coating

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
尹晓光等: "α-Al2O3 纳米片的自燃烧法控制合成及其抛光性能", 《物理化学学报》 *
陆大年: "《表面活性剂化学及纺织助剂》", 31 March 2009, 中国纺织出版社 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103952083A (en) * 2014-04-09 2014-07-30 贵州亿科新材料有限公司 Method for producing polishing powder by hard kaolin
CN103952083B (en) * 2014-04-09 2016-04-27 贵州亿科新材料有限公司 A kind of hard kaoline produces the method for polishing powder
CN114940886A (en) * 2022-04-28 2022-08-26 浙江大学 Nano alumina abrasive particle, preparation method and application thereof, and silicon carbide polishing solution containing abrasive particle
CN114940886B (en) * 2022-04-28 2023-09-05 浙江大学 Nanometer alumina abrasive grain, preparation method and application thereof, and silicon carbide polishing solution containing abrasive grain

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Application publication date: 20100901