CN105836770B - A method of preparing high temperature boehmite - Google Patents

A method of preparing high temperature boehmite Download PDF

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CN105836770B
CN105836770B CN 201610172756 CN201610172756A CN105836770B CN 105836770 B CN105836770 B CN 105836770B CN 201610172756 CN201610172756 CN 201610172756 CN 201610172756 A CN201610172756 A CN 201610172756A CN 105836770 B CN105836770 B CN 105836770B
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boehmite
slurry
aluminum
temperature
water
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CN 201610172756
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CN105836770A (en )
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李广战
张丽
王智锦
李鹏飞
秦烟莱
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中铝山东有限公司
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本发明公开了一种耐高温勃姆石的制备方法,将含铝化合物与水化浆,加入引晶剂和洗涤助剂,混合均匀后装入高压釜中,控制升温速度为1~3℃/min,在150~250℃下,反应2~6h后降温,经分离洗涤、干燥后,得到耐高温勃姆石。 The present invention discloses a method for preparing a high temperature of boehmite, aluminum-containing compound with a hydrate slurry, added seeding agent and detergency builder mixed uniformly charged to the autoclave, temperature rise rate of the control 1 ~ 3 ℃ / min, at 150 ~ 250 ℃, reaction 2 ~ 6h cool, separated and washed, and dried to give boehmite temperature. 本发明制备方法简单,产能大,生产成本低,制备的勃姆石转化率高,颗粒分布集中,1%脱水温度达到350℃以上,化学纯度高,电导率≤25μs/cm。 The present invention is a simple method of preparation, large capacity, low cost, high conversion of boehmite prepared, the particle distribution centered, 1% dehydration temperature above 350 deg.] C, high chemical purity, conductivity ≤25μs / cm.

Description

一种耐高温勃姆石的制备方法 A method of preparing high temperature boehmite

技术领域 FIELD

[0001]本发明涉及材料制备合成技术领域,具体涉及一种耐高温勃姆石的制备方法。 Preparation [0001] The present invention relates to a composition technologies, and in particular relates to a method for preparing the boehmite temperature.

背景技术 Background technique

[0002] 勃姆石(Boehmite),又称薄水铝石、一水软铝石等,化学式为A100H或Al2〇3 • H20, 不溶于水,难溶于酸碱,其粉体具有非常广泛的应用价值。 [0002] boehmite (Boehmite), also called boehmite, a boehmite like, or the formula A100H Al2〇3 • H20, insoluble in water, insoluble in acid, which has a very wide powder application value.

[0003]勃姆石的制备方法,国内外很多专利文献都进行了报道,例如,us 4797139中所述的勃姆石是通过引晶处理的方法形成,并且局限于勃姆石微粒适应形成氧化铝磨料里的范围内,具有特别期望的球形状,使得其适用于研磨应用;R •鲍尔在公开号为CN 1942398A中公开了一种引晶勃姆石微粒材料及制备方法,指出以悬浮液的形式提供勃姆石前体和勃姆石^种,前体采用常规的ATH (三水合氧化铝),晶种为假勃姆石以及酸碱调节剂,然后对其进行热处理,以使勃姆石前体转化为各种长径比的勃姆石微粒;蔡卫权等在公开号为CN 1733607A中公开了一种微米级薄水铝石的制备方法,指出首先用H2〇2沉淀一定氧化铝浓度的铝酸钠溶液得到薄水铝石晶种,然后将其与一定氧化铝浓度的铝酸钠溶液进行种分,种分率可达50%以上;江琦等在Zl 20〇710〇31164.0中,公开了一种纳米 [0003] Preparation of boehmite, many domestic and foreign patent documents have been reported, e.g., us 4797139 in the boehmite is formed by the method of seeding process, and adapt limited boehmite particulate oxide is formed an aluminum abrasive in the range, particularly desirable spherical shape, make it suitable for abrasive applications; R • Powell Publication No. CN 1942398A discloses a crystalline boehmite particulate material and a method for preparing primers, indicated to a suspension in the form of liquid providing a boehmite precursor and boehmite ^ species precursor using conventional ATH (alumina trihydrate), the seed of the pseudo-boehmite and a pH adjusting agent, and then subjected to heat treatment, so that boehmite precursor into boehmite particulate of various aspect ratios; right guard Cai et Publication No. CN 1733607A discloses a method for preparing micron-sized boehmite, noting that some oxide precipitated first with H2〇2 aluminum concentration of sodium aluminate solution obtained boehmite seed, then some alumina concentration and sodium aluminate solution was seeded, seeded up to 50% or more; Zl 20〇710〇 in Jiang Qideng 31164.0 discloses a nano 体勃姆石的制备方法,即以异丙醇铝水解产物为前体,然后通过水热反应得到分散性好的纳米勃姆石;CN l〇2249270A中,公开了一种干法制备大粒径勃姆石的方法,首先将氢氧化铝在一定温度和压力下,转化为薄水铝石,然后磨至一定粒径,最后通过湿法进行纳米二氧化硅包覆处理, 得到低吸油率,广泛应用于电子材料领域的产品;CN 102815733A公开了一种纳米勃姆石及其制备方法,即一定组分的拟薄水铝石、无机酸/碱、助剂、去离子水等搅拌均匀,入高压釜进行水热反应,然后洗涤、喷雾干燥得到不同形貌的纳米勃姆石;CN 102092749A公开了一种薄水铝石的制备方法,即采用氢氧化铝为原料,水热处理过程中,加入薄水铝石等晶种控制产品的颗粒形貌,加入酸或碱性电解质降低产品的钠含量,从而得到一种超低钠的薄水铝石和氧化铝;CN 10183〇49lA公开了 Preparation of boehmite material, i.e., aluminum isopropoxide hydrolyzate precursor, and then obtain a good dispersibility Namibomu stone by hydrothermal reaction; l〇2249270A the CN, the dry process is disclosed a large grain method diameter boehmite, aluminum hydroxide at a first temperature and pressure, is converted to boehmite, and then ground to a certain particle size, and finally coated nanosilica treated by a wet process to obtain a low oil absorption rate , a material widely used in electronic products; CN 102815733A, discloses a method for its preparation Namibomu stone, i.e. quasi boehmite certain components, inorganic acids / bases, auxiliaries, water such as deionized stir , into the autoclave for a hydrothermal reaction, then washed, spray-dried to obtain different morphologies Namibomu stone; CN 102092749A discloses a process for preparing the boehmite, aluminum hydroxide as raw material, i.e., the hydrothermal treatment adding boehmite seed controlling particle morphology and the like products, addition of acid or alkaline electrolyte reduced the sodium content of the product, to thereby obtain boehmite alumina and an ultra-low sodium; discloses the CN 10183〇49lA 种高耐热勃姆石的制备方法,即首先将氢氧化铝在多350°C下转化为勃姆石,然后研磨至一定粒径,再采用湿法高速搅拌下进行表面纳米二氧化硅包覆处理,经除杂纯化后干燥得到低吸油率,高流动性的勃姆石产品。 The method of producing a high heat-boehmite, aluminum hydroxide by first conversion at 350 ° C a multi-boehmite, and then ground to a certain particle size, and then stirred at a high speed by a wet surface-nanosilica package plating process, after drying to obtain a low impurity purified oil absorption rate, high mobility boehmite product.

[0004] 综上,耐高温勃姆石的制备方法,相关资料很少。 [0004] In summary, the method for preparing high temperature boehmite, very little relevant information.

发明内容 SUMMARY

[0005] 本发明针对现有技术的不足,提供一种耐高温勃姆石的制备方法。 [0005] The present invention addresses deficiencies in the prior art, there is provided a method of preparing high temperature boehmite.

[0006] 为实现上述目的,本发明采用的技术方案是: [0006] To achieve the above object, the technical solution adopted by the invention is:

[0007] —种耐高温勃姆石的制备方法,将含铝化合物与水化浆,加入引晶剂和洗涤助剂, 混合均匀后装入高压釜中,控制升温速度为1〜3°C/min,在150〜25(TC下,反应2〜6h后降温,经分离洗涤、干燥后,得到耐高温勃姆石。 [0007] - Preparation of boehmite types of high temperature, the aluminum-containing compound with a hydrate slurry, added seeding agent and detergency builder mixed uniformly charged to the autoclave, controlled heating rate 1~3 ° C / min, in the (lower 150~25 TC, 2~6h after cooling the reaction, was separated, washed, and dried to give boehmite temperature.

[0008]进一步地,所述含铝化合物、引晶剂和洗涤助剂的质量比为1:0.05〜0.5:0.005〜 0.1。 [0008] Further, the aluminum compound, the mass ratio of the seeding agent and detergency builder is 1: 0.05~0.5: 0.005~ 0.1.

[0009] 进一步地,所述含铝化合物,包括碱石灰烧结法氢氧化铝、拟薄水铝石、p-氧化铝或拜耳石中的一种或多种。 [0009] Further, the aluminum compound include aluminum hydroxide, soda lime sintering method, one or more quasi-boehmite, bayerite alumina, or p-in.

[0010] 进一步地,所述水包括蒸馏水、高纯水、去离子水或反渗透水。 [0010] Preferably, the water comprises distilled water, high purity water, deionized or reverse osmosis water.

[0011] 进一步地,所述含铝化合物与水化浆的浆液液固比为1〜10。 [0011] Further, the aluminum-containing compound and hydrated pulp slurry of liquid to solid ratio of 1~10.

[0012] 进一步地,所述引晶剂,包括无定型铝胶、氧化铝溶胶或薄水铝石中的一种或多种。 [0012] Further, the seeding agent comprising one or more amorphous alumina gel, or alumina sol of boehmite.

[0013] 进一步地,所述引晶剂的含水率0 • 1〜95 % wt。 [0013] Further, the water content of the seeding agent 0 • 1~95% wt.

[0014] 进一步地,所述洗涤助剂为铵的碳酸盐,使衆液的pH值控制在7〜13之间。 [0014] Preferably, the adjuvant is washed with ammonium carbonate, the pH was controlled between all 7~13.

[0015] 进一步地,所述干燥温度为100〜220°C。 [0015] Further, the drying temperature is 100~220 ° C.

[0016] 进一步地,反应温度为180〜210°C,升温速度为1.5〜3°C/min,反应时间为2〜4h。 [0016] Further, the reaction temperature is 180~210 ° C, a heating rate of 1.5~3 ° C / min, the reaction time is 2~4h.

[0017] 本发明提供的一种耐高温勃姆石的制备方法,得到的勃姆石转化率高,颗粒分布集中,1 %脱水温度达到350°C以上,化学纯度高,电导率彡25us/cm;而且制备方法简单,产能大,生产成本低,广泛用作制备高纯氧化铝,高性能催化剂及载体、高效无毒阻燃剂以及电子材料等领域。 [0017] The method for producing a high temperature of the present invention provides boehmite, the boehmite conversion rate obtained particle distribution concentrated, 1% dehydration temperature above 350 ° C, high chemical purity, conductivity San 25us / cm & lt; preparation and the method is simple, large capacity, low cost, is widely used as the field of preparation of high purity alumina, high-performance catalyst and carrier, fire retardant and non-toxic and efficient electronic materials.

具体实施方式 detailed description

[0018] 本发明实施例提供一种耐高温勃姆石的制备方法,将含铝化合物与水化浆,加入引晶剂和洗涤助剂,混合均匀后装入高压釜中,控制升温速度为1〜3°C/min,在150〜250°C 下,反应2〜6h后降温,经分离洗涤、干燥后,得到耐高温勃姆石。 [0018] Example embodiments provide a method for producing a high temperature of boehmite, aluminum-containing compound with a hydrate slurry, added seeding agent and detergency builder mixed uniformly charged to the autoclave, temperature rise rate control according to the present invention is 1~3 ° C / min, at 150~250 ° C, after cooling the reaction 2~6h, separated washed, and dried to give boehmite temperature.

[0019] 所述含铝化合物、引晶剂和洗涤助剂的质量比为1:0 • 05〜0.5:0.005〜0.1。 [0019] The aluminum-containing compound, the quality of the seeding agent and detergency builder ratio is 1: 0 • 05~0.5: 0.005~0.1. 所述含铝化合物与水化浆的浆液液固比为1〜1 〇,优选1.5〜4。 The aluminum-containing compound and the hydrated pulp slurry of liquid to solid ratio 1~1 billion, preferably 1.5~4. 所述引晶剂的含水率0.1〜95 % 评1:,优选30~80%机。 The water content of the seeding agent 0.1~95% Comment 1 :, preferably 30 to 80% of the machine.

[0020] 所述含铝化合物包括碱石灰烧结法氢氧化铝、拟薄水铝石、P-氧化铝或/和拜耳石,含铝化合物可以是一种也可以多种同时加入,不限定其加入比例。 [0020] The aluminum containing compound comprises aluminum hydroxide of soda lime sintering method, quasi-boehmite, P- alumina and / or bayerite, aluminum-containing compound may also be a plurality of simultaneously added, which is not defined Join proportion.

[0021] 所述引晶剂,包括无定型铝胶、氧化铝溶胶和薄水铝石,引晶剂可以是一种也可以多种同时加入,不限定其加入比例。 [0021] The seeding agent, comprising an amorphous alumina gel, alumina sol, and boehmite, the seeding agent may be one more may be added simultaneously, is not limited to the proportion added.

[0022] 所述洗涤助剂,包括碳酸铵、碳酸氢铵等铵的碳酸盐中的一种或多种,使浆液的pH 值控制在7〜13。 [0022] The detergency builder comprising one or more of ammonium carbonate, ammonium carbonate, ammonium bicarbonate and the like, so that the slurry pH control 7~13.

[0023]所述干燥,经分离洗涤合格后的滤饼,采用烘箱、闪蒸干燥或者喷雾干燥,干燥温度为100〜220°C,优选150〜21CTC。 [0023] The dried cake was washed by passing separated using an oven, flash or spray drying, a drying temperature of 100~220 ° C, preferably 150~21CTC.

[0024]本发明的创造性在于,采用低成本的碱石灰烧结法氢氧化铝及其中间产物等含铝化合物为原料,通过加入引晶剂和洗涤助剂,可以得到高纯度的高耐热勃姆石(1 %脱水温度达到350°C以上)。 [0024] The present invention is inventive, low-cost soda-lime sintering aluminum hydroxide and aluminum-containing compound as an intermediate raw material, etc., by the addition of the seeding agent and detergency builder, high heat resistance can be obtained high purity Bo boehmite (1% dehydration temperature above 350 ° C). 其中,引晶剂能有效控制勃姆石的晶体形貌和粒度及分布,洗涤助剂有利于将原料中的钠转化为可溶性钠盐,易于洗涤除去。 Wherein the seeding agent can effectively control the boehmite crystal morphology and particle size and distribution, washed with sodium additives facilitate the feedstock is converted to soluble sodium salt, easily removed by washing. 本发明提供的制备方法简单,产能大,生产成本低,本产品可广泛用作制备高纯氧化铝,高性能催化剂及载体、高效无毒阻燃剂以及电子材料等领域。 The present invention provides a method of preparing a simple, large capacity, low production cost, the present product can be widely used as the field of preparation of high purity alumina, high-performance catalyst and carrier, fire retardant and non-toxic and efficient electronic materials.

[0025] 实施例1 [0025] Example 1

[0026]本发明实施例1提供的一种耐高温勃姆石的制备方法,具体如下:取〇.7kg碱石灰烧结法氢氧化铝和0 • 3kgp-氧化铝,用2 • 5kg蒸馏水搅拌化浆均匀,含铝化合物与水化浆的采液液固比为2 • 5,加入引晶剂〇. 5kg无定型招胶(含水率为65 %),和5g碳酸钱洗k助剂后, 浆液pH约为7_5,装入高压釜中,控制ire/分钟的速度升至18〇1:,保温2.5小时。 Method for preparing a high-temperature boehmite according to an embodiment of [0026] the present invention, as follows: taking aluminum hydroxide 〇.7kg soda lime sintering and 0 • 3kgp- alumina, distilled water was stirred with 2 • 5kg of homogeneous slurry, the slurry containing aluminum compound mining hydration liquid-solid ratio of 2 • 5, square seeding agent was added. after 5kg move amorphous gum (moisture content 65%), and 5g of money k carbonate wash aid, the slurry pH was about 7_5, charged to the autoclave, the speed control ire / min to a 18〇1 :, for 2.5 hours. 降温后过滤分呙,用蒸馏水洗漆,供箱lg(TC下千燥。产品勃姆石转化率为98%,1 %脱水温度3幻C, 电导率24iis/cm。 After cooling Guo separated by filtration, washed with distilled water paint for box lg (TC dry in the products boehmite conversion was 98%, 1% 3 phantom C dehydration temperature, conductivity 24iis / cm.

[0027] 实施例2 [0027] Example 2

[0028] 本发明实施例2提供的一种耐高温勃姆石的制备方法,具体如下:取〇• 5kg碱石灰烧结法氢氧化铝和0 • 5kg拜耳石,用1.5kg高纯水搅拌化浆均匀,含铝化合物与水化浆的浆液液固比为1 • 5,加入引晶剂〇. 4kg薄水铝石(含水率50 %),和50g碳酸铵洗涤助剂后,浆液pH约为5,装入高压釜中,控制nc/分钟的速度升至削^;,保温2小时。 [0028] Preparation 2 boehmite high temperature resistant embodiment of the present invention provides, as follows: take the square soda-lime • 5kg sintering aluminum hydroxide and 0 • 5kg bayerite, with uniform 1.5kg of high purity water was stirred slurry , hydrated aluminum-containing compound slurry with a slurry of liquid to solid ratio of 1 • 5, square seeding agent was added. after 4kg boehmite (water content 50%), and 50g of ammonium carbonate detergency builder, a slurry pH of about 5 charged in the autoclave, control nc / min cutting speed was raised ;, ^ incubated for 2 hours. 降温后过滤分离,用高纯水洗涤,烘箱15〇。 After cooling was separated by filtration, washed with high purity water, oven 15〇. (:下千燥。产品勃姆石转化率为97.5%,1%脱水温度352°C,电导率20ys/cm。 (: The product was dry boehmite conversion was 97.5%, 1% dehydration temperature of 352 ° C, conductivity 20ys / cm..

[0029] 实施例3 [0029] Example 3

[0030]本发明实施例3提供的一种耐高温勃姆石的制备方法,具体如下:取1.0kg拜耳石, 用2 • 5kg去离子水搅拌化浆均匀,含铝化合物与水化浆的浆液液固比为2.5,加入引晶剂0 • 25kg氧化铝溶胶(含水率80 %)和10§碳酸氢铵洗涤助剂后,浆液pH约为8,装入高压釜中, 控制1.8°C/分钟的速度升至丨98!:,保温3小时。 [0030] The method for producing a high temperature of boehmite Example 3 of the present invention provides, as follows: Take 1.0kg bayerite, with 2 • 5kg of deionized water were uniformly stirred slurry, hydrated aluminum-containing compound and the slurry the slurry of liquid to solid ratio of 2.5, after the addition of the seeding agent 0 • 25kg of alumina sol (water content 80%) and ammonium bicarbonate 10§ detergent builder, a slurry pH of about 8, was charged in the autoclave, 1.8 ° C control / minute is raised Shu 98:!, for 3 hours. 降温后过滤分离,用去离子水洗涤,喷雾干燥器198°C下干燥。 After cooling was separated by filtration, washed with deionized water and dried, the spray dryer 198 ° C. 产品勃姆石转化率为98.5 %,丨%脱水温度358»c,电导率2〇us/cm。 Product boehmite conversion was 98.5%, the dehydration temperature Shu% 358 »c, conductivity 2〇us / cm.

[0031] 实施例4 [0031] Example 4

[0032] 本发明实施例4提供的一种耐高温勃姆石的制备方法,具体如下:取lkgp-氧化铝, 用2kg反渗透水搅拌化浆均匀,含铝化合物与水化浆的浆液液固比为2 . 〇,加入引晶剂0.75kg薄水铝石(含水率为0.5%),和l〇〇g碳酸氢铵洗涤助剂后,浆液PH约为13,装入高压釜中,控制2 • 0°C/分钟的速度升至2〇5。 [0032] The method for producing a high temperature of boehmite Example 4 of the present invention provides, as follows: aluminum compound and hydrated pulp slurry was taken lkgp- alumina, reverse osmosis water was stirred with 2kg of a uniform slurry, solid ratio of 2. square, the seeding agent is added 0.75kg boehmite (water content 0.5%), and after washing aid l〇〇g bicarbonate slurry PH about 13, charged to the autoclave, control 2 • 0 ° C / min speed was raised 2〇5. 〇,保温2小时。 Square, incubated for 2 hours. 降温后过滤分离,用反渗透水洗涤,闪蒸干燥器220°C下干燥。 After cooling was separated by filtration, washed with RO water and dried, flash dryers 220 ° C. 产品勃姆石转化率为耵.8%,1 %脱水温度365r,电导率2Uis/cm。 Ding boehmite conversion product was .8%, 1% dehydration temperature 365R, conductivity 2Uis / cm. [0033] 实施例5 [0033] Example 5

[0034]本发明实施例5提供的一种耐高温勃姆石的制备方法,具体如下:取0 • 6kg拟薄水铝石和0 • 4kg碱石灰烧结法氢氧化铝,用4kg高纯水搅拌化浆均匀,含铝化合物与水化浆的浆液液固比为4 • 0,加入引晶剂1 • 65kg氧化铝溶胶(含水率为70%),和100g碳酸氢铵洗涤助剂后f液pH约为13,装入高压釜中,控制2r/分钟的速度升至205r,保温3小时。 [0034] The method for producing a high temperature of boehmite Example 5 of the present invention provides, as follows: 0 • 6kg take boehmite and pseudoboehmite 0 • 4kg soda lime sintering aluminum hydroxide, was stirred with a high water slurry with 4kg homogeneous slurry of liquid to solid ratio of aluminum compound to the slurry and the hydration 4 • 0, added seeding agent 1 • 65kg of alumina sol (water content 70%), and 100g ammonium bicarbonate, pH detergent builder after about f 13, charged to the autoclave, control speed 2r / min to a 205R, for 3 hours. 降温后过滤分离,用高纯水洗涤,喷雾干燥器190°C下干燥。 After cooling was separated by filtration, washed with high purity water and dried, the spray dryer 190 ° C. 产品勃姆石转化率为98.5%,1%脱水温度358°C,电导率18j^s/cm。 Product boehmite conversion was 98.5%, 1% dehydration temperature of 358 ° C, the conductivity 18j ^ s / cm.

[0035] 实施例6 [0035] Example 6

[0036]本发明实施例6提供的一种耐高温勃姆石的制备方法,具体如下:取〇. 6kg拜耳石、 0.2kgp-氧化铝和0 • 2kg碱石灰烧结法氢氧化铝,用3kg去离子水搅拌化浆均匀,含铝化合物与水化楽的菜液液固比为3.0,加入0 • Skg引晶剂无定型招胶(含水率为8〇%)和7〇g碳酸铵洗涤助剂后,浆液pH约为9,装入高压釜中,控制2.〇°C/分钟的速度升至198。 A method for preparing high temperature of boehmite Example 6 provided in Embodiment [0036] The present invention is as follows: Take 6kg square bayerite, 0.2kgp- 0 • 2kg alumina and soda-lime sintering aluminum hydroxide, with 3kg washed with deionized water of a uniform slurry was stirred, and hydrated aluminum compound yue dish liquid-solid ratio of 3.0, was added 0 • Skg recruited seeding agent amorphous gel (water content 8〇%) and ammonium carbonate 7〇g auxiliaries slurry pH of about 9, charged to the autoclave, the control 2.〇 ° C / minute was raised to 198. (:,保温4小时。 降温后过滤分离,用去离子水洗涤,闪蒸干燥器2〇5。(:下干燥。产品勃姆石转化率为98.3%, 1%脱水温度355°C,电导率15ys/cm。 ' (:, For 4 hours after cooling was separated by filtration, washed with deionized water, flash dryers 2〇5 (:... The product was dried boehmite conversion was 98.3%, 1% dehydration temperature of 355 ° C, the conductivity rate 15ys / cm. '

[0037] 对比实施例1 [0037] Comparative Example 1

[0038]本发明对比实施例1提供的一种耐高温勃姆石的制备方法,具体如下:取以lkg拜斗VS里氧化Ip,加入3kg高纯水搅拌化浆均匀,含铝化合物与水化浆的浆液液固比为3. 〇,装入高压爸中,控制3.5TV分钟的速度升至19(TC,保温2小时。降温后过滤分离,洗涤,12(TC 下干燥。产品勃姆石转化率为M • 3 %,1 %脱水温度281 r,电导率215us/cm。 [0038] The present invention is a process for preparing refractory Comparative Example 1 will provide boehmite embodiment, as follows: take the bucket thanks to lkg VS in Ip oxidation, 3kg high purity water was added with stirring of the homogeneous slurry, the slurry containing aluminum compound hydrate the slurry of liquid to solid ratio of 3 billion, the charged high pressure dad, 3.5TV min to a speed control 19 (TC, incubated for 2 hours. after cooling was isolated by filtration, washed, 12 (TC dried product boehmite conversion ratio of M • 3%, 1% dehydration temperature 281 r, conductivity 215us / cm.

[0039]对比实施例2 [0039] Comparative Example 2

[0040] 本发f对比实施例2提供的一种耐高温勃姆石的制备方法,具体如下:取以1kg拜耳石,加入4kg高纯水搅拌化浆均匀,含铝化合物与水化浆的浆液液固比为4. 〇,装入高压釜中,控制3 • 5°C/分钟的速度升至200。 [0040] The present method for preparing a high-temperature f Comparative Example 2 provided boehmite embodiment, as follows: Take 1kg to bayerite, high purity water was added 4kg of uniformly stirred slurry, the slurry liquid slurry of hydrated aluminum compound and 4. a square solid ratio is charged in the autoclave, the control 3 • 5 ° C / minute was raised to 200. (:,保温3小时。降温后过滤分离、洗涤,120。(:下干燥。产品勃姆石转化率为97.6%,1%脱水温度272°C,电导率198ys/cm。 (:, For 3 hours after cooling was separated by filtration, washed, 120 (:... The product was dried boehmite conversion was 97.6%, 1% dehydration temperature of 272 ° C, conductivity 198ys / cm.

[0041] 对比实施例3 [0041] Comparative Example 3

[0042]本发明对比实施例3提供的一种耐高温勃姆石的制备方法,具体如下:取以lkg拜耳法氢氧化铝,加入3kg高纯水搅拌化浆均匀,含铝化合物与水化浆的浆液液固比为3.0,加入l〇〇g引晶剂拟薄水铝石,一起装入高压釜中,控制3.5°C/分钟的速度升至190°C,保温2小时。 [0042] The present invention is a process for preparing refractory comparative boehmite according to embodiment 3 provides, as follows: Take lkg Bayer aluminum hydroxide, 3kg high purity water was added with stirring of the homogeneous slurry, the slurry containing aluminum compound hydration the slurry of liquid to solid ratio of 3.0, was added seeding agent l〇〇g quasi boehmite was charged in the autoclave together with the control speed of 3.5 ° C / min to a 190 ° C, for 2 hours. 降温后过滤分离,洗涤,120°C下干燥。 After cooling was separated by filtration, washed and dried, 120 ° C. 产品勃姆石转化率为95.3%,1 %脱水温度275°C, 电导率208us/cm〇 Product boehmite conversion was 95.3%, 1% dehydration temperature of 275 ° C, the conductivity 208us / cm〇

[0043]最后所应说明的是,以上具体实施方式仅用以说明本发明的技术方案而非限制, 尽管参照实例对本发明进行了详细说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的精神和范围,其均应涵盖在本发明的权利要求范围当中。 [0043] Finally, it should be noted that the above specific embodiments are intended to illustrate the present invention and not limitation, although the present invention has been described in detail with reference to examples, those of ordinary skill in the art should be understood that the present invention technical solution modifications or equivalent replacements without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the present invention as claimed in which the required range.

Claims (1)

  1. 1. 一种耐高温勃姆石的制备方法,其特征在于:将含铝化合物与水化浆,加入引晶剂和洗涤助剂,混合均匀后装入高压釜中,控制升温速度为I.5〜3°C/min,在18〇〜2l(TC下,反应2〜4h后降温,经分尚洗漆、干燥后,得到耐尚温勃姆石; 所述含铝化合物、引晶剂和洗涤助剂的质量比为1:0.05〜0.5:0.005〜0.1; 所述含铝化合物,包括碱石灰烧结法氢氧化铝、拟薄水铝石、P-氧化铝或拜耳石中的一种或多种; 所述水包括蒸馏水、高纯水、去离子水或反渗透水; 所述含铝化合物与水化浆的浆液液固比为1.5〜4; 所述引晶剂,包括无定型铝胶、氧化铝溶胶或薄水铝石中的一种或多种; 所述引晶剂的含水率30〜80 % wt; 所述洗涤助剂为铵的碳酸盐,使浆液的pH值控制在7〜13之间; 所述千燥温度为150〜210°C。 CLAIMS 1. A method of preparing high temperature boehmite, wherein: the aluminum-containing compound with a hydrate slurry, added seeding agent and detergency builder mixed uniformly charged to the autoclave, temperature rise rate control is I. 5~3 ° C / min, in the (lower 18〇~2l TC, 2~4h cooled reaction, wash the paint still-divided, and dried to give boehmite resistance still warm; the aluminum-containing compound, a seeding agent and mass ratio of detergent builder is 1: 0.05~0.5: 0.005~0.1; the aluminum compounds include aluminum hydroxide, soda lime sintering method, a thin, quasi boehmite, P- or bayerite alumina in or more; the water include distilled water, high purity water, deionized or reverse osmosis water; the slurry of liquid to solid ratio of aluminum compound to the slurry of hydrated 1.5~4; the seeding agent, amorphous alumina gel comprising , alumina sol or boehmite of one or more; the water content of the seeding agent 30~80% wt; the detergency builder is ammonium carbonate, the pH of the slurry in the control between 7~13; dry in the temperature of 150~210 ° C.
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