CN1285510C - Prepn process of nano aluminium hydroxide - Google Patents
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- CN1285510C CN1285510C CN 200410067540 CN200410067540A CN1285510C CN 1285510 C CN1285510 C CN 1285510C CN 200410067540 CN200410067540 CN 200410067540 CN 200410067540 A CN200410067540 A CN 200410067540A CN 1285510 C CN1285510 C CN 1285510C
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- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 24
- 230000008569 process Effects 0.000 title claims abstract description 9
- 229910021502 aluminium hydroxide Inorganic materials 0.000 title 1
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000243 solution Substances 0.000 claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 21
- 239000012065 filter cake Substances 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 239000012670 alkaline solution Substances 0.000 claims abstract description 9
- 239000000084 colloidal system Substances 0.000 claims abstract description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 7
- 238000001556 precipitation Methods 0.000 claims abstract description 7
- 239000000725 suspension Substances 0.000 claims abstract description 7
- 238000010533 azeotropic distillation Methods 0.000 claims abstract description 6
- 238000004945 emulsification Methods 0.000 claims abstract description 6
- 239000003223 protective agent Substances 0.000 claims abstract description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 4
- 238000001308 synthesis method Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 230000032683 aging Effects 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 229920002521 macromolecule Polymers 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 239000002002 slurry Substances 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims 1
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 abstract description 5
- 229920000642 polymer Polymers 0.000 abstract description 5
- 239000000047 product Substances 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000011049 filling Methods 0.000 abstract description 3
- 150000002484 inorganic compounds Chemical class 0.000 abstract description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000012266 salt solution Substances 0.000 abstract 1
- 239000003063 flame retardant Substances 0.000 description 15
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 9
- 239000007789 gas Substances 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002861 polymer material Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000026030 halogenation Effects 0.000 description 1
- 238000005658 halogenation reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000012796 inorganic flame retardant Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000009972 noncorrosive effect Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 150000004684 trihydrates Chemical class 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
本发明涉及一种纳米氢氧化铝的制备方法，属无机化合物制备工艺技术领域。本发明方法主要包括有均相沉淀法合成法和非均相沉淀共沸蒸馏法，该方法的特点是采用铝盐溶液和碱性溶液为原料，添加少量高分子保护剂如聚乙二醇或聚乙烯醇，在均质乳化反应器中发生均相沉淀反应，根据所需产物粒径调节搅拌速度，得到的氢氧化铝悬浊液经冷却、陈化、抽滤，洗涤，将所得滤饼加入正丁醇共沸溶剂的溶液，进行共沸蒸馏，烘干所得氢氧化铝胶体，最后制得纳米氢氧化铝粉体。本发明方法工艺流程简单、易于操作，所得的产物粒径分布均匀、纯度高，粒径在25-100nm范围内。另外该纳米氢氧化铝具有较好的阻燃性能和填充性能。The invention relates to a preparation method of nanometer aluminum hydroxide, which belongs to the technical field of inorganic compound preparation technology. The method of the present invention mainly includes the homogeneous precipitation synthesis method and the heterogeneous precipitation azeotropic distillation method. The characteristics of the method are that aluminum salt solution and alkaline solution are used as raw materials, and a small amount of polymer protective agent such as polyethylene glycol or polyethylene glycol is added. Polyvinyl alcohol, a homogeneous precipitation reaction occurs in a homogeneous emulsification reactor, the stirring speed is adjusted according to the desired product particle size, the obtained aluminum hydroxide suspension is cooled, aged, suction filtered, washed, and the obtained filter cake is A solution of n-butanol azeotropic solvent is added, azeotropic distillation is carried out, and the obtained aluminum hydroxide colloid is dried to obtain nanometer aluminum hydroxide powder. The method of the invention has simple technological process and is easy to operate, and the obtained product has uniform particle size distribution and high purity, and the particle size is in the range of 25-100nm. In addition, the nano-aluminum hydroxide has good flame retardancy and filling performance.
Description
技术领域technical field
本发明涉及一种纳米氢氧化铝的制备方法，属无机化合物制备工艺技术领域。The invention relates to a preparation method of nanometer aluminum hydroxide, which belongs to the technical field of inorganic compound preparation technology.
背景技术Background technique
随着科学技术的进一步发展，人们生活水平的提高，化学建材塑料加工品及有机高分子聚合材料越来越广泛地用于建筑、交通、电器、通讯等领域。这些材料固有的易燃性而带来的火灾隐患已成为全球关注的社会问题，现阶段主要是通过加入阻燃剂来降低聚合物易燃性，减缓其燃烧速度。With the further development of science and technology and the improvement of people's living standards, chemical building materials, plastic processed products and organic polymer materials are more and more widely used in construction, transportation, electrical appliances, communications and other fields. The fire hazards caused by the inherent flammability of these materials have become a social issue of global concern. At this stage, the main method is to reduce the flammability of polymers and slow down their burning speed by adding flame retardants.
在众多的阻燃剂品种中，卤素阻燃剂以其阻燃效果好、不影响材料物化性能而得到广泛应用。但是，加入卤素阻燃剂的聚合物在燃烧时发烟量大、易放出腐蚀性气体(如HCl、HBr等)和有害性气体，易造成二次危害。因此，当今世界的阻燃剂研究朝无卤化的方向发展。氢氧化铝阻燃剂即三水合氧化铝，占无机阻燃剂的80％以上，在塑料中可作填料和阻燃剂，具有填充、阻燃和抑烟三重功能，且无毒、无腐蚀、价格竞争力强。在国外被誉为无公害阻燃剂。氢氧化铝发生脱水反应的温度为300-350℃，当受热时，氢氧化铝会释放结晶水，吸收大量热量，从而抑制聚合物材料温度上升，延缓其热分解并降低燃烧速度，产生的水蒸气能稀释可燃性气体；脱水而产生的氧化铝形成一覆盖层，限制燃烧、切断氧气供给，阻止可燃气体的流动，从而起到阻燃作用。Among the many varieties of flame retardants, halogen flame retardants are widely used because of their good flame retardant effect and not affecting the physical and chemical properties of materials. However, polymers added with halogen flame retardants have a large amount of smoke when burned, and are prone to release corrosive gases (such as HCl, HBr, etc.) and harmful gases, which are likely to cause secondary hazards. Therefore, the research on flame retardants in today's world is developing towards the direction of non-halogenation. Aluminum hydroxide flame retardant is alumina trihydrate, which accounts for more than 80% of inorganic flame retardants. It can be used as filler and flame retardant in plastics. It has triple functions of filling, flame retardant and smoke suppression, and is non-toxic and non-corrosive. , Strong price competitiveness. It is known as a pollution-free flame retardant abroad. The dehydration reaction temperature of aluminum hydroxide is 300-350°C. When heated, aluminum hydroxide will release crystal water and absorb a large amount of heat, thereby inhibiting the temperature rise of the polymer material, delaying its thermal decomposition and reducing the burning speed, and the produced water The steam can dilute the combustible gas; the alumina produced by dehydration forms a covering layer, which restricts combustion, cuts off the oxygen supply, and prevents the flow of combustible gas, thereby playing a flame-retardant role.
但是氢氧化铝本身的阻燃效率较低，要求较高的添加量，普通氢氧化铝在达到阻燃份额时，因其颗粒粒度大，界面结合力小，难以在聚合物中均匀分散，使得聚合物材料的机械力学性能大大降低；而纳米氢氧化铝，由于粒径小、比表面积大，增强了与基体材料的相互作用，可以更均匀地分散在基体材料中，发挥阻燃效果的同时能有效地改善基体材料的机械力学性能。因此，氢氧化铝粉体的超细化是今后的发展方向。However, the flame retardant efficiency of aluminum hydroxide itself is low, requiring a higher amount of addition. When ordinary aluminum hydroxide reaches the flame retardant ratio, it is difficult to disperse evenly in the polymer because of its large particle size and small interfacial bonding force. The mechanical and mechanical properties of polymer materials are greatly reduced; and nano-aluminum hydroxide, due to its small particle size and large specific surface area, enhances the interaction with the matrix material, and can be more uniformly dispersed in the matrix material to exert the flame retardant effect. Can effectively improve the mechanical properties of the matrix material. Therefore, ultra-fine aluminum hydroxide powder is the future development direction.
近年来，国内外在超细或纳米氢氧化铝阻燃剂的制备和应用方面作了大量的研究工作。在美国专利US4492682和US3268295中，提出了利用碳分分解法在剧烈搅拌下，往铝酸钠溶液中通入二氧化碳气体得到凝胶，洗涤过滤后再分散到其他溶液中进行热处理，得到平均粒径小于10nm的超细氢氧化铝。但该方法碳分分解时间长，当溶液体积仅为0.5升时，碳分分解过程还需要15-30分钟时间，其效率较低，且得到的凝胶不均匀。中国专利CN1116185A中公开了一种在旋转床超重力场条件下一步法直接制备超细氢氧化铝的方法，可以得到颗粒为25-100nm的超细氢氧化铝。但此种方法得到的氢氧化铝颗粒粒度分布不均，且工艺复杂，工业化成本较高。In recent years, a lot of research work has been done on the preparation and application of ultrafine or nano aluminum hydroxide flame retardants at home and abroad. In U.S. Patents US4492682 and US3268295, it is proposed to use the carbon decomposition method to pass carbon dioxide gas into the sodium aluminate solution under vigorous stirring to obtain a gel. After washing and filtering, it is dispersed in other solutions for heat treatment to obtain the average particle size. Ultrafine aluminum hydroxide less than 10nm. However, this method takes a long time to decompose carbon. When the volume of the solution is only 0.5 liters, the process of decomposing carbon still needs 15-30 minutes. The efficiency is low, and the obtained gel is not uniform. Chinese patent CN1116185A discloses a method for directly preparing ultra-fine aluminum hydroxide in the next step under the condition of a rotating bed in a high-gravity field, and can obtain ultra-fine aluminum hydroxide with a particle size of 25-100 nm. However, the particle size distribution of aluminum hydroxide particles obtained by this method is uneven, and the process is complicated, and the industrialization cost is relatively high.
发明内容Contents of the invention
本发明的目的是提供一种条件简易、粒度分布均匀、粒径易控制的纳米氢氧化铝的制备方法。The object of the present invention is to provide a method for preparing nano aluminum hydroxide with simple conditions, uniform particle size distribution and easy control of particle size.
本发明一种纳米氢氧化铝的制备方法，包括有均相沉淀法合成法和非均相沉淀共沸蒸馏法，该制备方法的特征是具有以下具体工艺步骤：A kind of preparation method of nanometer aluminum hydroxide of the present invention comprises homogeneous phase precipitation synthesis method and heterogeneous phase precipitation azeotropic distillation method, and the feature of this preparation method is to have the following specific process steps:
a.首先制备添加有高分子保护剂的硫酸铝水溶液，高分子保护剂为聚乙二醇或聚乙烯醇中的任一种；其加入量为硫酸铝质量的1-3％；a. first prepare the aluminum sulfate aqueous solution that is added with macromolecule protective agent, macromolecule protective agent is any one in polyethylene glycol or polyvinyl alcohol; Its addition is 1-3% of aluminum sulfate quality;
b.将上述硫酸铝水溶液放置于均质乳化反应器中，加热，且在转速3000-7000rpm下搅拌30分钟；b. Place the above aluminum sulfate aqueous solution in a homogeneous emulsification reactor, heat, and stir for 30 minutes at a rotating speed of 3000-7000rpm;
c.缓慢滴入碱性溶液于反应器中，并不断搅拌，控制转速3000-7000rpm，控制反应温度25-45℃，得到氢氧化铝悬浊液；碱性溶液为氢氧化钠、氨水、碳酸铵中的任一种；c. Slowly drop the alkaline solution into the reactor, and keep stirring, control the speed at 3000-7000rpm, control the reaction temperature at 25-45°C to obtain aluminum hydroxide suspension; the alkaline solution is sodium hydroxide, ammonia water, carbonic acid any of ammonium;
d.将所得的氢氧化铝悬浊液冷却、陈化、抽滤，所得滤饼用去离子水洗涤；在此过程中，陈化处理温度为20℃，时间为12小时；d. cooling, aging, and suction filtering the obtained aluminum hydroxide suspension, and washing the obtained filter cake with deionized water; during this process, the aging treatment temperature was 20° C., and the time was 12 hours;
e.将上述所得滤饼中加入共沸溶液正丁醇溶液，并进行搅拌打浆，然后共沸蒸馏至水分被完全脱除，再继续蒸馏，蒸出共沸溶剂正丁醇；然后将所得的胶体进行烘干，最终得到疏松的纳米氢氧化铝颗粒。e. Add the azeotropic solution n-butanol solution to the filter cake obtained above, and stir and make a slurry, then azeotropically distill until the water is completely removed, then continue to distill, and steam the azeotropic solvent n-butanol; then the obtained The colloid is dried to obtain loose nano-aluminum hydroxide particles.
共沸溶液正丁醇溶液中的共沸溶剂正丁醇的加入量是按氢氧化铝胶体滤饼的质量为基准，即每克氢氧化铝胶体滤饼加入相当于0.58-0.68毫升的共沸溶剂正丁醇；所得氢氧化铝胶体的干燥温度为100-130℃，干燥时间为6-12小时。The amount of the azeotropic solvent n-butanol in the azeotropic solution n-butanol solution is based on the quality of the aluminum hydroxide colloidal filter cake, that is, every gram of aluminum hydroxide colloidal filter cake is added with an amount equivalent to 0.58-0.68 ml of azeotropic The solvent is n-butanol; the drying temperature of the obtained aluminum hydroxide colloid is 100-130° C., and the drying time is 6-12 hours.
硫酸铝溶液的浓度最适宜为1-2mol/l；所述碱性溶液最佳为氢氧化钠溶液，其浓度为0.5-1.0mol/l。The most suitable concentration of the aluminum sulfate solution is 1-2 mol/l; the most suitable alkaline solution is a sodium hydroxide solution with a concentration of 0.5-1.0 mol/l.
本发明方法中，制备纳米氢氧化铝的基本反应式如下：In the inventive method, the basic reaction formula of preparing nano aluminum hydroxide is as follows:
本发明方法中，加入高分子保护剂为聚乙二醇或聚乙烯醇的作用是防止纳米氢氧化铝胶体粒子发生团聚。采用正丁醇共沸溶剂是为了使氢氧化铝粒子容易变小，粒径均匀。In the method of the present invention, the function of adding polyethylene glycol or polyvinyl alcohol as the polymer protective agent is to prevent the aggregation of the nano aluminum hydroxide colloidal particles. The purpose of using n-butanol azeotropic solvent is to make the aluminum hydroxide particles smaller and uniform in particle size.
本发明方法的优点是工艺流程简单、易于操作、投资小、成本低。制备得到的纳米氢氧化铝的颗粒粒径在25-100nm范围内。产品粒度分布均匀、纯度高。另外，与聚烯烃类基体材料相溶性良好，产品的阻燃性能、填充性能均远优于其它普通氢氧化铝产品。The method of the invention has the advantages of simple technological process, easy operation, small investment and low cost. The particle size of the prepared nano aluminum hydroxide is in the range of 25-100nm. The particle size distribution of the product is uniform and the purity is high. In addition, it has good compatibility with polyolefin matrix materials, and its flame retardancy and filling performance are far superior to other ordinary aluminum hydroxide products.
具体实施方法Specific implementation method
现将本发明的实施例具体叙述如后：Embodiments of the present invention are now specifically described as follows:
实施例1Example 1
将34.2克Al2(SO4)3固体溶于100毫升去离子水中，构成浓度为1mol/l的Al2(SO4)3溶液，加入0.5克聚乙二醇，搅拌30分钟。另将12克NaOH溶于600毫升去离子水中，形成浓度为0.5mol/l的NaOH碱性溶液。将上述硫酸铝溶液加入到均质乳化反应器，缓慢滴加上述配置的NaOH溶液，边滴加边搅拌，搅拌器转速控制为6000rpm，控制反应温度为25℃，得到氢氧化铝悬浊液；然后经冷却，在20℃下陈化12小时，再进行抽滤，所得滤饼用去离子水洗涤，直至检不出硫酸根离子；将滤饼与事先制备好的正丁醇共沸溶液一起防在容器内，进行搅拌打浆；然后共沸蒸馏至水分被完全脱除，继续蒸馏，蒸出共沸溶剂正丁醇；然后将所得胶体在130℃下烘干8小时，最终得到平均粒径为25nm氢氧化铝粉体。34.2 g of Al 2 (SO 4 ) 3 solid was dissolved in 100 ml of deionized water to form an Al 2 (SO 4 ) 3 solution with a concentration of 1 mol/l, 0.5 g of polyethylene glycol was added, and stirred for 30 minutes. In addition, 12 grams of NaOH was dissolved in 600 milliliters of deionized water to form a NaOH alkaline solution with a concentration of 0.5 mol/l. Add the above-mentioned aluminum sulfate solution to the homogeneous emulsification reactor, slowly add the above-mentioned NaOH solution dropwise, stir while adding dropwise, control the speed of the stirrer to 6000rpm, and control the reaction temperature to 25°C to obtain an aluminum hydroxide suspension; Then, after cooling, aging at 20°C for 12 hours, and then suction filtration, the obtained filter cake was washed with deionized water until no sulfate ion was detected; the filter cake was mixed with the previously prepared n-butanol azeotropic solution Put it in the container, stir and beat; then azeotropic distillation until the water is completely removed, continue to distill, and distill out the azeotropic solvent n-butanol; then dry the obtained colloid at 130°C for 8 hours, and finally get the average particle size It is 25nm aluminum hydroxide powder.
实施例2Example 2
本实施例的工艺过程与上述实施例1相同。将34.2克Al2(SO4)3固体溶于100毫升去离子水中，构成浓度为lmol/l的Al2(SO4)3溶液，加入0.5克聚乙二醇，搅拌30分钟。另将12克NaOH溶于600毫升去离子水中，形成浓度为0.5mol/l的NaOH碱性溶液。将上述硫酸铝溶液加入到均质乳化反应器，缓慢滴加上述配置的NaOH溶液，边滴加边搅拌，搅拌器转速控制为3000rpm，控制反应温度为45℃，得到氢氧化铝悬浊液；然后经冷却，在20℃下陈化12小时，再进行抽滤，所得滤饼用去离子水洗涤，直至检不出硫酸根离子；将滤饼与事先制备好的正丁醇共沸溶液一起放在容器内，进行搅拌打浆；然后共沸蒸馏至水分被完全脱除，继续蒸馏，蒸出共沸溶剂正丁醇；然后将所得胶体在130℃下烘干8小时，最终得到平均粒径为50nm氢氧化铝粉体。The process of this embodiment is the same as that of the above-mentioned embodiment 1. 34.2 g of Al 2 (SO 4 ) 3 solid was dissolved in 100 ml of deionized water to form an Al 2 (SO 4 ) 3 solution with a concentration of 1 mol/l, 0.5 g of polyethylene glycol was added, and stirred for 30 minutes. In addition, 12 grams of NaOH was dissolved in 600 milliliters of deionized water to form a NaOH alkaline solution with a concentration of 0.5 mol/l. Add the above-mentioned aluminum sulfate solution to the homogeneous emulsification reactor, slowly add the above-mentioned NaOH solution dropwise, stir while adding dropwise, control the speed of the stirrer to 3000rpm, and control the reaction temperature to 45°C to obtain an aluminum hydroxide suspension; Then, after cooling, aging at 20°C for 12 hours, and then suction filtration, the obtained filter cake was washed with deionized water until no sulfate ion was detected; the filter cake was mixed with the previously prepared n-butanol azeotropic solution Put it in a container, stir and beat; then azeotropic distillation until the water is completely removed, continue to distill, and distill out the azeotropic solvent n-butanol; then dry the obtained colloid at 130°C for 8 hours, and finally get the average particle size It is 50nm aluminum hydroxide powder.
实施例3Example 3
本实施例的工艺过程与上述实施例1相同。所不同的是物料在均质乳化反应器中反应时，搅拌器转速为7000rpm，控制反应温度为30℃，最终得到平均粒径为30nm氢氧化铝粉体。The process of this embodiment is the same as that of the above-mentioned embodiment 1. The difference is that when the materials are reacted in the homogeneous emulsification reactor, the stirrer speed is 7000rpm, the reaction temperature is controlled at 30°C, and aluminum hydroxide powder with an average particle size of 30nm is finally obtained.
在上述实施例中，所采用的正丁醇共沸溶液中的共沸溶剂正丁醇的配置加入量按氢氧化铝胶体滤饼的质量为基准，即每克氢氧化铝胶体滤饼加入相当于0.61毫升的共沸溶剂正丁醇。In the foregoing examples, the configuration addition amount of the azeotropic solvent n-butanol in the n-butanol azeotropic solution adopted is based on the quality of the aluminum hydroxide colloidal filter cake, that is, every gram of aluminum hydroxide colloidal filter cake is added equivalent to In 0.61 ml of azeotropic solvent n-butanol.
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| CN102502735A (en) * | 2011-11-03 | 2012-06-20 | 沈阳铝镁设计研究院有限公司 | Method for producing alumina by using pulverized fuel ash |
| CN102502735B (en) * | 2011-11-03 | 2014-05-21 | 沈阳铝镁设计研究院有限公司 | Method for producing alumina by using pulverized fuel ash |
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