CN1608997A - Prepn process of nano aluminium hydroxide - Google Patents
Prepn process of nano aluminium hydroxide Download PDFInfo
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- CN1608997A CN1608997A CN 200410067540 CN200410067540A CN1608997A CN 1608997 A CN1608997 A CN 1608997A CN 200410067540 CN200410067540 CN 200410067540 CN 200410067540 A CN200410067540 A CN 200410067540A CN 1608997 A CN1608997 A CN 1608997A
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Abstract
The present invention is preparation process of nanometer aluminum hydroxide and belongs to the field of inorganic compound preparing technology. The preparation process includes homogeneous deposition and synthesis process and inhomogeneous deposition and azeotropic distillation process, and features that the aluminum salt solution and alkali solution as material are prepared into aluminum hydroxide powder through the steps of adding small amount of polymer protecting agent, homogeneous deposition reaction in a homogeneous emulsifier, regulating the stirring speed to obtain aluminum hydroxide suspension, cooling ageing, suction filtering, washing, azeotropic distillation of the solution obtained via adding n-butanol into the filter cake, stoving to obtain aluminum hydroxide colloid and aluminum hydroxide powder. The technological process is simple and the product has high purity and grain size of 25-100 nm.
Description
Technical Field
The invention relates to a preparation method of nano aluminum hydroxide, belonging to the technical field of preparation processes of inorganic compounds.
Background
With the further development of science and technology, the living standard of people is improved, and the plastic processed products and organic polymer materials of chemical building materials are more and more widely used in the fields of buildings, traffic, electrical appliances, communication and the like. The fire hazard caused by the inherent flammability of these materials has become a social problem of global concern, and at present, the flammability of the polymer is reduced mainly by adding a flame retardant to slow down the combustion speed of the polymer.
Among various flame retardant varieties, the halogen flame retardant is widely applied due to good flame retardant effect and no influence on the physical and chemical properties of materials. However, the polymer added with the halogen flame retardant has a large amount of smoke during combustion, and easily emits corrosive gases (such as HCl, HBr and the like) and harmful gases, thereby easily causing secondary damage. Therefore, the research on flame retardants in the world is moving toward non-halogenation. The aluminum hydroxide fire retardant, namely the alumina trihydrate, accounts for more than 80 percent of the inorganic fire retardant, can be used as a filler and a fire retardant in plastics, has triple functions of filling, fire retarding and smoke suppression, and has the advantages of no toxicity, no corrosion and strong price competitiveness. Is praised as a pollution-free flame retardant abroad. The temperature of the dehydration reaction of the aluminum hydroxide is 300-350 ℃, when the aluminum hydroxide is heated, the aluminum hydroxide releases crystal water and absorbs a large amount of heat, so that the temperature rise of the polymer material is inhibited, the thermal decomposition of the polymer material is delayed, the combustion speed is reduced, and the generated water vapor can dilute the combustible gas; the alumina produced by dehydration forms a coating layer which limits combustion, cuts off oxygen supply and prevents the flow of combustible gas, thus playing a role of flame retardance.
But the flame retardant efficiency of the aluminum hydroxide is low, the higher addition amount is required, and when the common aluminum hydroxide reaches the flame retardant share, the particle size is large, the interface bonding force is small, and the uniform dispersion in the polymer is difficult, so that the mechanical property of the polymer material is greatly reduced; the nanometer aluminum hydroxide has small particle size and large specific surface area, enhances the interaction with the matrix material, can be more uniformly dispersed in the matrix material, and can effectively improve the mechanical property of the matrix material while exerting the flame retardant effect. Therefore, the ultrafine formation of the aluminum hydroxide powder is a future development direction.
In recent years, a great deal of research work is done on the aspects of preparation and application of superfine or nano aluminum hydroxide flame retardants at home and abroad. In US4492682 and US3268295, it is proposed to use the carbolysis method to inject carbon dioxide gas into a sodium aluminate solution under vigorous stirring to obtain a gel, which is then washed, filtered and then redispersed in another solution for heat treatment to obtain ultrafine aluminium hydroxide with an average particle size of less than 10 nm. However, the method has long decomposition time of carbon, and when the volume of the solution is only 0.5 liter, the decomposition process of carbon still needs 15 to 30 minutes, so that the efficiency is low, and the obtained gel is not uniform. Chinese patent CN1116185A discloses a method for directly preparing superfine aluminum hydroxide by a one-step method under the condition of a rotary bed high gravity field, and superfine aluminum hydroxide with the particle size of 25-100nm can be obtained. However, the aluminum hydroxide particles obtained by the method have uneven particle size distribution, complex process and higher industrial cost.
Disclosure of Invention
The invention aims to provide a preparation method of nano aluminum hydroxide, which has simple conditions, uniform particle size distribution and easily controlled particle size.
The invention relates to a preparation method of nano aluminum hydroxide, which mainly comprises a homogeneous precipitation method synthesis method and a heterogeneous precipitation azeotropic distillation method, and is characterized by comprising the following specific process steps:
a. firstly, preparing an aluminum sulfate aqueous solution added with a high-molecular protective agent, wherein the high-molecular protective agent is any one of polyethylene glycol or polyvinyl alcohol; the adding amount of the aluminum sulfate is 1 to 3 percent of the mass of the aluminum sulfate;
b. placing the aluminum sulfate aqueous solution in a homogeneous emulsification reactor, heating, and stirring for 30 minutes at a certain rotating speed;
c. slowly dripping alkaline solution into the reactor, continuously stirring, controlling the rotating speed at 3000-7000rpm, and controlling the reaction temperature at 25-45 ℃ to obtain an aluminum hydroxide suspension; the alkaline solution is any one of sodium hydroxide, ammonia water and ammonium carbonate;
d. cooling, aging and filtering the obtained aluminum hydroxide suspension, and washing the obtained filter cake with deionized water; in the process, the aging temperature is 20 ℃ and the time is 12 hours;
e. adding an azeotropic solution n-butyl alcohol solution into the obtained filter cake, stirring and pulping, then carrying out azeotropic distillation until the water is completely removed, and continuing distillation to evaporate the azeotropic solvent n-butyl alcohol; and drying the obtained colloid to finally obtain loose nano aluminum hydroxide particles.
The adding amount of the azeotropic solvent n-butanol in the azeotropic solution n-butanol solution is based on the mass of the sodium hydroxide colloid filter cake, namely 0.58-0.68 ml of the azeotropic solvent n-butanol is added into each gram of the sodium hydroxide colloid filter cake; the drying temperature of the obtained aluminum hydroxide colloid is 100-130 ℃, and the drying time is 6-12 hours.
The concentration of the aluminum sulfate solution is most suitable to be 1-2 mol/l; the alkaline solution is preferably sodium hydroxide solution, and the concentration of the alkaline solution is 0.5-1.0 mol/l.
In the method, the basic reaction formula for preparing the nano aluminum hydroxide is as follows:
in the method, the function of adding the macromolecular protective agent which is polyethylene glycol or polyvinyl alcohol is to prevent the nano aluminum hydroxide colloid particles from agglomerating. The n-butanol azeotropic solvent is used for the purpose of making the aluminum hydroxide particles easily smaller and uniform in particle size.
The method has the advantages of simple process flow, easy operation, low investment and low cost. The particle diameter of the prepared nano aluminum hydroxide is in the range of 25-100 nm. The product has uniform particle size distribution and high purity. In addition, the flame retardant and the filling performance of the product are far superior to those of other common aluminum hydroxide products.
Detailed description of the invention
The embodiments of the present invention will now be described in detail as follows:
example 1
34.2 g of Al2(SO4)3The solid was dissolved in 100 ml of deionized water to give 1mol/l Al2(SO4)3Adding 0.5 g of polyethylene glycol into the solution, and stirringStirring for 30 minutes. Another 12 g NaOH was dissolved in 600 ml deionized water to form an alkaline solution of NaOH with a concentration of 0.5 mol/l. Adding the aluminum sulfate solution into a homogeneous emulsification reactor, slowly dropwise adding the prepared NaOH solution while stirring, controlling the rotating speed of the stirrer to be 6000rpm, and controlling the reaction temperature to be 25 ℃ to obtain an aluminum hydroxide suspension; then cooling, aging at 20 ℃ for 12 hours, carrying out suction filtration, and washing the obtained filter cake with deionized water until no sulfate ions are detected; the filter cake and n-butanol azeotropic solution prepared in advance are prevented in a container together, and stirring and pulping are carried out; then, carrying out azeotropic distillation until the water is completely removed, and continuing distillation to evaporate the azeotropic solvent n-butanol; then drying the obtained colloid for 8 hours at 130 ℃ to finally obtain the aluminum hydroxide powder with the average grain diameter of 25 nm.
Example 2
The process of this example is the same as example 1 above. 34.2 g of Al2(SO4)3The solid was dissolved in 100 ml of deionized water to give 1mol/l Al2(SO4)3The solution was stirred for 30 minutes with 0.5 g of polyethylene glycol. Another 12 g NaOH was dissolved in 600 ml deionized water to form an alkaline solution of NaOH with a concentration of 0.5 mol/l. Adding the aluminum sulfate solution into a homogeneous emulsification reactor, slowly dropwise adding the prepared NaOH solution while stirring, controlling the rotating speed of the stirrer to be 3000rpm, and controlling the reaction temperature to be 45 ℃ to obtain an aluminum hydroxide suspension; then cooling, aging at 20 ℃ for 12 hours, carrying out suction filtration, and washing the obtained filter cake with deionized water until no sulfate ions are detected; putting the filter cake and a n-butanol azeotropic solution prepared in advance into a container together, and stirring and pulping; then, carrying out azeotropic distillation until the water is completely removed, and continuing distillation to evaporate the azeotropic solvent n-butanol; then drying the obtained colloid for 8 hours at 130 ℃ to finally obtain the aluminum hydroxide powder with the average grain diameter of 50 nm.
Example 3
The process of this example is the same as example 1 above. The difference is that when the materials react in the homogeneous emulsification reactor, the rotating speed of the stirrer is 7000rpm, the reaction temperature is controlled at 30 ℃, and finally the aluminum hydroxide powder with the average grain diameter of 30nm is obtained.
In the above examples, the amount of n-butanol as an azeotropic solvent in the n-butanol azeotropic solution is based on the mass of the aluminum hydroxide colloidal filter cake, that is, 0.61 ml of n-butanol as an azeotropic solvent is added per gram of the aluminum hydroxide colloidal filter cake.
Claims (3)
1. A method for preparing nano aluminum hydroxide mainly comprises a homogeneous precipitation method synthesis method and a heterogeneous precipitation azeotropic distillation method, and is characterized by comprising the following specific process steps:
a. firstly, preparing an aluminum sulfate aqueous solution added with a high-molecular protective agent, wherein the high-molecular protective agent is any one of polyethylene glycol or polyvinyl alcohol; the adding amount of the aluminum sulfate is 1 to 3 percent of the mass of the aluminum sulfate;
b. placing the aluminum sulfate aqueous solution in a homogeneous emulsification reactor, heating, and stirring for 30 minutes at a certain rotating speed;
c. slowly dripping alkaline solution into the reactor, continuously stirring, controlling the rotating speed at 3000-7000rpm, and controlling the reaction temperature at 25-45 ℃ to obtain an aluminum hydroxide suspension; the alkaline solution is any one of sodium hydroxide, ammonia water and ammonium carbonate;
d. cooling, aging and filtering the obtained aluminum hydroxide suspension, and washing the obtained filter cake with deionized water; in the process, the aging temperature is 20 ℃ and the time is 12 hours;
e. adding an azeotropic solution n-butyl alcohol solution into the obtained filter cake, stirring and pulping, then carrying out azeotropic distillation until the water is completely removed, and continuing distillation to evaporate the azeotropic solvent n-butyl alcohol; and drying the obtained colloid to finally obtain loose nano aluminum hydroxide particles.
2. The method for preparing nano aluminum hydroxide according to claim 1, wherein the amount of n-butanol as azeotropic solvent in the n-butanol solution of azeotropic solution is based on the mass of the sodium hydroxide colloid filter cake, that is, 0.58-0.68 ml of n-butanol as azeotropic solvent is added per gram of sodium hydroxide colloid filter cake; the drying temperature of the obtained aluminum hydroxide colloid is 100-130 ℃, and the drying time is 6-12 hours.
3. The method for preparing nano aluminum hydroxide according to claim 1, wherein the concentration of the aluminum sulfate solution is 1-2 mol/l; the alkaline solution is preferably sodium hydroxide solution, and the concentration of the alkaline solution is 0.5-1.0 mol/l.
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| CN100337922C (en) * | 2005-10-18 | 2007-09-19 | 浙江大学 | Method of preparing ultrafine aluminium hydroxide by coprecipitation sublimation |
| CN100411990C (en) * | 2006-01-23 | 2008-08-20 | 中国铝业股份有限公司 | Method for preparing aluminium hydroxide micropowder |
| CN100427397C (en) * | 2006-09-05 | 2008-10-22 | 中国铝业股份有限公司 | Preparation method of flake ultrafine aluminium hydroxide |
| CN1868885B (en) * | 2006-05-12 | 2010-07-21 | 广西民族大学 | Self-dispersion type nanometer gamma A100H and its preparation method and use |
| CN102120596B (en) * | 2010-01-08 | 2012-11-07 | 北京世纪地和科技有限公司 | Method for preparing aluminum hydroxide by utilizing precipitation method |
| CN102101685B (en) * | 2009-12-16 | 2012-11-28 | 国家纳米科学中心 | Aluminium hydroxide nanometer strip and preparation method thereof |
| CN103359763A (en) * | 2013-07-04 | 2013-10-23 | 鸿福晶体科技(安徽)有限公司 | Chemical preparation method for spherical hollow alumina powder for producing gemstone by using flame fusion method |
| CN103395809A (en) * | 2013-07-23 | 2013-11-20 | 浙江万里学院 | Method for synthesizing nanometer gama-Al2O3 by adopting solvent replacement/azeotropic distillation drying method and applications thereof |
| CN103754913A (en) * | 2014-01-28 | 2014-04-30 | 复旦大学 | Simple preparation method of aluminum hydroxide nanoparticle material |
| CN104961146A (en) * | 2015-06-26 | 2015-10-07 | 吉林大学 | Nanometer sheet aluminum hydroxide gel and preparation method thereof |
| CN109534379A (en) * | 2019-01-09 | 2019-03-29 | 上海大学(浙江·嘉兴)新兴产业研究院 | A kind of nano-level sphere γ-Al2O3The low cost preparation method of powder |
| CN110092385A (en) * | 2019-04-01 | 2019-08-06 | 浙江工业大学之江学院 | A kind of preparation method of zeopan hydrogel |
| CN110368327A (en) * | 2019-08-14 | 2019-10-25 | 广州益凡医疗器械有限公司 | A kind of plaque removes gel and preparation method thereof |
| CN111184860A (en) * | 2020-02-21 | 2020-05-22 | 中牧实业股份有限公司 | Improved aluminum hydroxide adjuvant and preparation method thereof |
| CN112110463A (en) * | 2019-06-19 | 2020-12-22 | 吉林大学 | Al (OH) based on aluminum-gallium-based alloy3Powder preparation method |
| CN113735152A (en) * | 2020-05-29 | 2021-12-03 | 中国石油化工股份有限公司 | Method for removing alcohol entrained in aluminum hydroxide slurry |
| CN114735961A (en) * | 2022-02-23 | 2022-07-12 | 武汉源锦建材科技有限公司 | Solid-liquid dual-purpose alkali-free accelerator and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100337922C (en) * | 2005-10-18 | 2007-09-19 | 浙江大学 | Method of preparing ultrafine aluminium hydroxide by coprecipitation sublimation |
| CN100411990C (en) * | 2006-01-23 | 2008-08-20 | 中国铝业股份有限公司 | Method for preparing aluminium hydroxide micropowder |
| CN1868885B (en) * | 2006-05-12 | 2010-07-21 | 广西民族大学 | Self-dispersion type nanometer gamma A100H and its preparation method and use |
| CN100427397C (en) * | 2006-09-05 | 2008-10-22 | 中国铝业股份有限公司 | Preparation method of flake ultrafine aluminium hydroxide |
| CN102101685B (en) * | 2009-12-16 | 2012-11-28 | 国家纳米科学中心 | Aluminium hydroxide nanometer strip and preparation method thereof |
| CN102120596B (en) * | 2010-01-08 | 2012-11-07 | 北京世纪地和科技有限公司 | Method for preparing aluminum hydroxide by utilizing precipitation method |
| CN103359763A (en) * | 2013-07-04 | 2013-10-23 | 鸿福晶体科技(安徽)有限公司 | Chemical preparation method for spherical hollow alumina powder for producing gemstone by using flame fusion method |
| CN103395809A (en) * | 2013-07-23 | 2013-11-20 | 浙江万里学院 | Method for synthesizing nanometer gama-Al2O3 by adopting solvent replacement/azeotropic distillation drying method and applications thereof |
| CN103395809B (en) * | 2013-07-23 | 2017-03-01 | 宁波江东晟创工业产品设计有限公司 | One kind is using solvent displacement/azeotropic point distillation seasoning synthesis nanometer γ Al2O3Method and its application |
| CN103754913B (en) * | 2014-01-28 | 2016-08-17 | 复旦大学 | A kind of simple method for preparing of aluminum hydroxide nanoparticle material |
| CN103754913A (en) * | 2014-01-28 | 2014-04-30 | 复旦大学 | Simple preparation method of aluminum hydroxide nanoparticle material |
| CN104961146A (en) * | 2015-06-26 | 2015-10-07 | 吉林大学 | Nanometer sheet aluminum hydroxide gel and preparation method thereof |
| CN109534379A (en) * | 2019-01-09 | 2019-03-29 | 上海大学(浙江·嘉兴)新兴产业研究院 | A kind of nano-level sphere γ-Al2O3The low cost preparation method of powder |
| CN110092385A (en) * | 2019-04-01 | 2019-08-06 | 浙江工业大学之江学院 | A kind of preparation method of zeopan hydrogel |
| CN110092385B (en) * | 2019-04-01 | 2022-07-15 | 浙江工业大学之江学院 | Preparation method of magnesium aluminum silicate hydrogel |
| CN112110463A (en) * | 2019-06-19 | 2020-12-22 | 吉林大学 | Al (OH) based on aluminum-gallium-based alloy3Powder preparation method |
| CN110368327A (en) * | 2019-08-14 | 2019-10-25 | 广州益凡医疗器械有限公司 | A kind of plaque removes gel and preparation method thereof |
| CN111184860A (en) * | 2020-02-21 | 2020-05-22 | 中牧实业股份有限公司 | Improved aluminum hydroxide adjuvant and preparation method thereof |
| CN111184860B (en) * | 2020-02-21 | 2022-05-06 | 中牧实业股份有限公司 | Improved aluminum hydroxide adjuvant and preparation method thereof |
| CN113735152A (en) * | 2020-05-29 | 2021-12-03 | 中国石油化工股份有限公司 | Method for removing alcohol entrained in aluminum hydroxide slurry |
| CN113735152B (en) * | 2020-05-29 | 2023-09-05 | 中国石油化工股份有限公司 | Method for removing entrained alcohol in aluminum hydroxide slurry |
| CN114735961A (en) * | 2022-02-23 | 2022-07-12 | 武汉源锦建材科技有限公司 | Solid-liquid dual-purpose alkali-free accelerator and preparation method and application thereof |
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Assignee: Shanghai Huahui Curtain Wall Manufacturing Co., Ltd. Assignor: Shanghai University Contract fulfillment period: 2007.9.10 to 2012.12.31 contract change Contract record no.: 2008310000105 Denomination of invention: Process for preparing nano aluminium hydroxide Granted publication date: 20061122 License type: Exclusive license Record date: 2008.10.6 Assignee: Xiandeng Electric Equipment Co., Ltd., Zhejiang Assignor: Shanghai University Contract fulfillment period: 2007.4.18 to 2015.4.17 contract change Contract record no.: 2008330001469 Denomination of invention: Process for preparing nano aluminium hydroxide Granted publication date: 20061122 License type: Exclusive license Record date: 20081029 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2007.4.18 TO 2015.4.17; CHANGE OF CONTRACT Name of requester: ZHEJIANG PROVINCE XIANDENG ELECTRICAL EQUIPMENT CO Effective date: 20081029 Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2007.9.10 TO 2012.12.31; CHANGE OF CONTRACT Name of requester: SHANGHAI HUAHUI WALL MAKING ENGINEERING CO., LTD. Effective date: 20081006 |