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Method for preparing aluminium polychlorid with high content of Al13

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CN102344157B
CN102344157B CN 201010241216 CN201010241216A CN102344157B CN 102344157 B CN102344157 B CN 102344157B CN 201010241216 CN201010241216 CN 201010241216 CN 201010241216 A CN201010241216 A CN 201010241216A CN 102344157 B CN102344157 B CN 102344157B
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method
preparing
aluminium
polychlorid
high
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CN102344157A (en )
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李小忠
苏晓梅
包建松
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浙江师范大学
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Abstract

本发明一种制备高Al13含量聚合氯化铝的方法,属于环保技术领域。 The present invention is a method for preparing a high PAC content Al13, it belongs to the field of environmental technology. 本发明是通过如下方式完成的:制备高Al13含量聚合氯化铝采用结晶氯化铝、氢氧化钠、偏铝酸钠为原料,制备高Al13含量聚合氯化铝的方法包括以下步骤:(1)取一定量的AlCl3溶液加入装有搅拌塞、搅拌棒、冷凝管的三口烧瓶中,恒温水浴加热;(2)取一定量的NaOH溶液进行预加热;(3)将预加热后的NaOH溶液加入AlCl3溶液中,加热搅拌反应,使NaOH与AlCl3反应生成二聚体Al2和多聚体Al6;(4)向二聚体Al2与多聚体Al6的混合溶液中加入NaAlO2溶液,进行加热搅拌反应;(5)反应一定时间后,得到聚合氯化铝成品。 The present invention is accomplished by: preparing high PAC content in crystalline Al13 aluminum chloride, sodium hydroxide, sodium aluminate as a raw material, preparation of high PAC content Al13 method comprising the steps of: (1 ) certain amount of AlCl3 was added with stirring stopper, stir bar, condenser three-necked flask, heated water bath; (2) certain amount of preheating NaOH solution; (3) the pre-heated solution of NaOH AlCl3 solution was added, the reaction was heated with stirring the NaOH is reacted with AlCl3 Al2 generating dimers and multimers Al6; (4) NaAlO2 solution was added to a mixed solution of Al2 dimers and multimers Al6, the reaction was heated and stirred ; (5) a certain reaction time, to give finished PAC. 本发明具有工艺简单、成本低、生产效率高,无二次污染;所制备的聚合氯化铝性能优越,稳定时间长的优点。 The present invention has simple process, low cost, high efficiency, no secondary pollution; PAC excellent properties of the prepared long settling time advantage.

Description

一种制备高Al13含量聚合氯化铝的方法 A method for preparing a high PAC content Al13

技术领域 FIELD

[0001] 本发明涉及环保技术领域,特别是一种制备用于污水絮凝处理的高Al13含量聚合氯化铝的方法。 [0001] The present invention relates to the field of environmental technology, in particular a high PAC content Al13 a method for preparing a treatment of produced water.

技术背景 technical background

[0002] 在无机高分子絮凝剂中,铝系絮凝剂品种较多,制备工艺方法较为成熟。 [0002] In the inorganic polymer flocculant, the flocculant aluminum varieties, process for preparing mature. 其中聚合氯化招(Polyaluminium Chloride),简称PAC,通常也称作碱式氯化招、聚轻基招等,是当前工业生产技术最成熟、效能最高、应用最为广泛的品种。 Wherein the polymerization strokes (Polyaluminium Chloride) chloride, referred to the PAC, also commonly referred to basic strokes chloride, polyethylene-based light strokes, is currently the most mature technology of industrial production, the highest performance, the most widely used species. 聚合氯化铝所代表的并不是某一种特定的无机化合物,而是一系列无机聚合物的总称。 PAC is not represented by a certain kind of inorganic compound, but the general term for a range of inorganic polymers. 聚合氯化铝实际上是在一定条件下控制铝的水解-聚合-沉淀过程的中间产物,其化学形态属于多核羟基络合物及无机高分子化合物,对水中颗粒物起高效絮凝作用。 PAC is actually controlled hydrolysis of aluminum under certain conditions - the polymerization - intermediate precipitation process, which belongs to the chemical form of polynuclear hydroxy complexes and inorganic polymers, of water particles from flocculation efficiency.

[0003] 聚合氯化铝的研制与开发始于60年代后期的日本,此后,欧洲、美国和前苏联等国的许多研究工作者对其合成制备工艺进行了大量的研究开发工作,国内外已有大量的专利和文献报道了数十种聚合氯化铝的制备工艺和方法。 [0003] PAC research and development began in the late 1960s in Japan, after Europe, the United States and other countries of the former Soviet Union, many researchers have done a lot of research and development work on its synthetic preparation process, has been at home and abroad a large number of patents and literature and the preparation method of dozens of polyaluminum chloride.

[0004] 通常制备聚合氯化铝的方法有以下几种: [0005] 1、以铝或活性三氧化二铝为原料的生产方法 [0004] generally prepared PAC methods are the following: [0005] 1, active aluminum oxide or aluminum feedstock for the production of

[0006] 以铝或活性三氧化二铝(包括铝屑、铝渣、铝灰和由粘土矿或煤矸石煅烧制得的活性三氧化二铝)为原料的化学方法。 [0006] chemically active aluminum oxide or aluminum (including aluminum powder, aluminum dross, aluminum ash and clay minerals obtained by calcining gangue or active alumina) as a raw material. 将一定量的铝或活性三氧化二铝溶于盐酸,随着反应的进行,体系的PH值逐渐升高,并在一定温度下促使Al (H2O) 63+发生水解和聚合反应。 The amount of active aluminum or aluminum oxide dissolved in hydrochloric acid, as the reaction proceeds, PH value of the system is gradually raised, and at a temperature to promote Al (H2O) 63+ hydrolysis and polymerization reactions. 可制得一定浓度铝、一定碱化度、一定聚合度的聚合氯化铝溶液。 A certain concentration of aluminum can be obtained, basified certain degree, a certain degree of polymerization of polyaluminum chloride solution.

[0007] 其产品中Al13含量较低,并且由于原料中含有较多的有害杂质,其生产的PAC杂质含量较高。 [0007] Al13 low content of their products, and since the material contains more harmful impurities, which produce high PAC content of impurities.

[0008] 2、以铝酸钠或氢氧化铝为原料的方法。 [0008] 2, or aluminum hydroxide to sodium aluminate as a raw material method. .

[0009] 将铝酸钠或氢氧化铝和盐酸按一定比例在反应釜中进行反应生成聚合氯化铝。 [0009] The sodium aluminate or aluminum hydroxide and hydrochloric acid according to a certain percentage of PAC in the reaction kettle. 该法生产聚合氯化铝的生产条件要求高温高压,成本较高,并且产品质量指标中的Al13含量只能达到40〜50%。 PAC production conditions require the production of high temperature and pressure, high cost, and product quality indicators can only reach the content of 40~50% Al13.

[0010] 3、以三氯化铝为原料的生产方法。 [0010] 3, aluminum trichloride as a raw material production methods. 常见的方法主要有以下四种: Common methods are the following four:

[0011] ①电解法 [0011] ① electrolysis

[0012] 中科院生态中心对这方面的研究较多。 [0012] Research in this area Ecology Center Chinese Academy of Sciences more. 通常以铝板为阳极,以不锈钢为阴极,氯化铝为电解液,通以直流电,在低压、高电流的条件下,制得聚合氯化铝。 Usually the aluminum plate as an anode and a cathode of stainless steel, aluminum chloride as electrolyte, through the DC, under conditions of low pressure, high current, obtained PAC. 如中科院生态中心开发了一种高质量的聚合氯化铝的制备技术,该技术以三氯化铝为电解液,铝板为阳极,铁板为阴极,通一定时间的低电压、大电流的直流电,即可制得聚合氯化铝的液体产品。 The CAS Ecology Center has developed a technique for preparing high quality aluminum chloride, and aluminum trichloride to this technique as the electrolyte, the aluminum plate as anode and iron as the cathode, a direct current of low voltage through a certain time, a large current , can be prepared PAC liquid products. 虽然其碱化度较高,其有效絮凝成分Al13质量分数为70%左右。 While its high basicity, the active ingredient Al13 flocculated mass fraction of about 70%. 但该方法是以铝板为阳极,制备的聚合氯化铝中大部分铝来自阳极铝板的溶解,致使该法的生产成本相对较高,还不能满足大规模生产的需要,并且其中仍有20 %〜40 %的铝以铝离子和氢氧化铝形式存在。 However, this method is based on the aluminum plate as an anode, most of PAC produced from aluminum plate was dissolved, resulting in the production method of the relatively high cost, large-scale production can not meet the needs, and there are still 20% ~ 40% of the aluminum present in the form of aluminum hydroxide and aluminum ions.

[0013] 中科院生态环境研究中心曲久辉等老师用形稳阳极电解制备出聚合十三铝占总铝60〜90%的聚合氯化铝。 [0013] Research Center of Chinese Academy of environment Qu Jiuhui other teachers prepare the polymeric thirteen aluminum 60~90% of the total aluminum polyaluminum chloride with Dimensionally Stable Anode. 但电解时间较长,一般在10小时以上,聚合十三铝易沉积阴极表面导致电极钝化,电解效率降低,并且聚合十三铝含量有待进一步提高。 However, long electrolysis time, typically 10 hours or more, the polymerization thirteen deposited aluminum surface of the cathode lead electrode easily passivated, reduced electrolysis efficiency, and the polymerization thirteen aluminum content to be further improved.

[0014] ②电渗析法。 [0014] ② electrodialysis.

[0015] 该方法是以三氯化铝为电解液,以两张阴离子交换膜(异相)构成反应室,石墨板为阳极,多孔铁板为阴极,通一定时间直流电,即制得PAC液体产品。 [0015] In the method, aluminum chloride as electrolyte, to two anion exchange membrane (of phase) constituting the reaction chamber, a graphite plate as an anode, a porous iron cathode, a direct current through a certain time, i.e., a liquid obtained PAC product. 该工艺虽先进,但这种方法工艺复杂,制造的产品质量完全依赖于离子交换膜的质量,存在着容易发生膜污染这一棘手难题,且膜的价格较贵导致PAC的成本较高。 Although the process is advanced, but this method complex process, the quality of products manufactured entirely dependent on the quality of the ion exchange membrane, there is prone to fouling this thorny problem, and the price is more expensive film PAC result in higher costs.

[0016] ③热分解法 [0016] ③ pyrolysis

[0017] 以结晶氯化铝为原料,也可采用沸腾热解法制得固体PAC,结晶氯化铝在一定温度下热解,分解出氯化氢和水,聚合变成粉状产物,即PAC (熟料),将熟料加一定量水搅拌,在较短时间内固化成树脂性产物,经干燥、粉碎即可得固体PAC产品。 [0017] In the crystalline aluminum chloride as raw materials, may also be employed to boil the PAC to give a solid pyrolysis Method, crystallization of aluminum chloride at a temperature pyrolysis, decomposition of hydrogen chloride and water, the polymerization becomes powdery product, i.e. PAC (cooked feed), plus a certain amount of water clinker was stirred in a short time compared to a cured resinous product was dried, pulverized to obtain a solid product PAC.

[0018] 该法生产设备投资大,分解效率较低,且易产生三氧化二铝,产品的聚合度一般在50%以下。 [0018] The production of equipment investment, low decomposition efficiency, and easy to produce aluminum oxide, polymerization degree of the product is generally 50% or less.

[0019] ④中和法。 [0019] ④ neutralization process.

[0020] 在三氯化铝溶液中加入氢氧化钠,石灰,石灰石,碳酸钠等碱性物质,提高氢氧根离子的浓度,以促进三氯化铝的水解,不同的加碱量可以得到不同碱化度产品。 [0020] In the hydrolysis of aluminum chloride was added a solution of sodium hydroxide, lime, limestone, alkaline substance such as sodium carbonate, to increase the concentration of hydroxide ions to promote aluminum trichloride, different amounts of base can be added different basicity products. 这种方法的实际生产不易控制,不能实现适宜碱化度和有效铝成分的理想配比,产品质量不够稳定,Al13含量较低。 This actual production process difficult to control, can not be achieved over a suitable and effective basicity ratio of the aluminum component, the product quality is not stable enough, low Al13 content. 实验室研究的结果也不尽一致。 The results of laboratory studies are not consistent. 通常认为微量加碱法(极慢的加碱速度)所得产品的Al13的质量分数可达80%以上,赵华章等通过提高温度等手段制得了总铝浓度为0.59mol/L, Al13的质量分数达80.7%的产品。 The mass fraction of Al13 generally considered micropipette alkali (alkali extremely slow speed) the resulting product up to 80%, Zhao Hua Zhang and other had a total aluminum concentration of 0.59mol / L manufactured by means of increasing the temperature, mass fraction of Al13 80.7% of the products. 但国外有报道指出在铝浓度很低的情况下,缓慢加碱得不到Al13,反而在90°C下通过快速加碱可得到Al13的质量分数为100 %的PAC溶液,于月华等用逐滴·加碱法制得聚合氯化铝,制得的产品据称Al13含量也不高。 But foreign been reported in the aluminum concentration is low, a base was added slowly not Al13, Al13 but obtained the mass fraction of 100% PAC solution was added to a base by flash at 90 ° C, and the like used Yu Yuehua dropwise PAC-alkali method were prepared product allegedly Al13 content is not high.

[0021] 综上,现有的制备聚合氯化铝方法存在着成本较高、产品有效成分Al13含量较低、总Al浓度不高、易产生污染等不足之处。 [0021] In summary, the conventional method of preparation of polyaluminum chloride there is high cost, low product Al13 active ingredient content, the total Al concentration is not high, easy to produce pollution deficiencies.

发明内容 SUMMARY

[0022] 本发明的目的是针对现有的制备聚合氯化铝方法中所存在的成本较高、产品有效成分Al13含量较低、总Al浓度不高、易产生污染等不足之处,提供具有成本低、产品有效成分Al13含量高、总Al浓度较高、污染少等优点的一种制备高A113含量聚合氯化铝的方法。 [0022] The object of the present invention is directed to the high cost of the conventional method of preparation PAC present in the product Al13 lower active ingredient content, the total Al concentration is not high, easy to produce inadequate pollution, providing a a method for preparing a high content A113 low cost, high product Al13 active ingredient content, the higher the total concentration of Al, and less pollution, etc. of the PAC.

[0023] 本发明一种制备高Al13含量聚合氯化铝的方法所采用的技术方案是通过如下方式完成的:制备高Al13含量聚合氯化铝采用结晶氯化铝、氢氧化钠、偏铝酸钠为原料,制备高Al13含量聚合氯化铝的方法包括以下步骤: [0023] The present invention is a process for preparing high aspect PAC content Al13 method used is accomplished by way of: preparing a high PAC content in crystalline Al13 aluminum chloride, sodium aluminate which sodium as raw materials, a high content of Al13 prepared PAC method comprising the steps of:

[0024] (I)取一定量的AlCl3溶液加入装有搅拌塞、搅拌棒、冷凝管的三口烧瓶中,恒温水浴加热; [0024] (I) a certain amount of AlCl3 was added with stirring stopper, stir bar, condenser three-necked flask, heated water bath;

[0025] (2)取一定量的NaOH溶液进行预加热; [0025] (2) a certain amount of NaOH solution preheated;

[0026] (3)将预加热后的NaOH溶液加入AlCl3溶液中,加热搅拌反应,使NaOH与AlCl3反应生成二聚体Al2和多聚体Al6 ; [0026] (3) A NaOH solution was added AlCl3 solution preheated, heated and stirred the reaction, the reaction of AlCl3 with NaOH Al2 dimers and multimers Al6;

[0027] (4)向二聚体Al2与多聚体Al6的混合溶液中加入NaAlO2溶液,进行加热搅拌反应;[0028] (5)反应一定时间后,得到聚合氯化铝成品。 [0027] (4) was added to the dimer and Al2 Al6 NaAlO2 solution in a mixed solution of polymer, the reaction was heated with stirring; after [0028] (5) a certain reaction time, to give finished PAC.

[0029] 其中步骤(3)、步骤(4)的部分原理见以下反应: Principal portion [0029] wherein in step (3), step (4) Refer to the following reaction:

[0030] 二聚体Al2、多聚体Al6 合成反应:AlCl3+NaOH — A12+A16[0031 ] Al13 形成反应:A12+A16+A1 (OH) Z — Al13 [0030] dimer Al2, Al6 polymer synthesis reaction: AlCl3 + NaOH - A12 + A16 [0031] Al13-forming reaction: A12 + A16 + A1 (OH) Z - Al13

[0032] 在上述制备高Al13含量聚合氯化铝的方法中,AlCl3溶液是采用浓度为0.4〜0.6mol/L的AlCl3溶液,恒温水浴加热的温度为80〜90°C。 [0032] In the preparation of high content of Al13 PAC method, the solution is the use of AlCl3 concentration 0.4~0.6mol / L of AlCl3 solution, heated water bath temperature of 80~90 ° C.

[0033] 在上述制备高Al13含量聚合氯化铝的方法中,NaOH溶液是采用浓度为0.6〜 [0033] In the preparation of high content of Al13 PAC method, NaOH concentration of the solution is the use of 0.6~

0.8mol/L的NaOH溶液,预加热的温度为80〜90°C。 0.8mol / L NaOH solution, preheated to a temperature of 80~90 ° C.

[0034] 在上述制备高Al13含量聚合氯化铝的方法中,预加热后的NaOH溶液加入AlCl3溶液中的量是按照摩尔数比n(AlCl3): n(NaOH)为1: 1.5〜1.6的比例确定的。 [0034] In the above method for preparing high Al13 PAC content, the amount of AlCl3 was added NaOH solution in accordance with the pre-heating molar ratio n (AlCl3): n (NaOH) is 1: 1.5~1.6 the the percentage determined.

[0035] 在上述制备高Al13含量聚合氯化铝的方法中,预加热后的NaOH溶液加入AlCl3溶液中,所进行的加热搅拌反应的水浴温度为80〜90°C,搅拌速度为100〜120r/min,加热搅拌反应的时间为25〜35min。 [0035] In the preparation of high content of Al13 PAC method, NaOH solution was added AlCl3 solution preheated, heated water bath temperature for the reaction is carried out 80~90 ° C, the stirring speed was 100~120r / min, heating and stirring of the reaction time 25~35min.

[0036] 在上述制备高Al13含量聚合氯化铝的方法中,向二聚体Al2与多聚体Al6的混合溶液中加入NaAlO2溶液是采用浓度为0.2〜0.4mol/L的NaAlO2溶液,向二聚体Al2与多聚体Al6的混合溶液中加入NaAlO2溶液的量是按照摩尔数比Ii(AlCl3): Ii(NaAlO2)为1: 0.4〜 [0036] In the preparation of high content of Al13 PAC method, NaAlO2 solution was added to a mixed solution of Al2 dimers and multimers Al6 is employed in a concentration of 0.2~0.4mol / L solution of NaAlO2, the two the amount of Al2 mer multimeric NaAlO2 solution was added a mixed solution in accordance Al6 molar ratio Ii (AlCl3): Ii (NaAlO2) of 1: 0.4~

0.5的比例确定的。 0.5 was determined.

[0037] 在上述制备高Al13含量聚合氯化铝的方法中,向二聚体Al2与多聚体Al6的混合溶液中加入NaAlO2溶液的方法是采`用缓慢滴加的方法进行的,所进行的加热搅拌反应的水浴温度为80〜90°C,搅拌速度为130〜150r/min,滴加时间为20〜30min。 [0037] In the preparation of high content of Al13 PAC method, and to a method of Al2 dimer NaAlO2 solution was added a mixed solution of the polymer Al6 is adopted a method for `slowly dropwise, and performed the reaction was stirred heated water bath temperature of 80~90 ° C, the stirring speed is 130~150r / min, dropwise over 20~30min.

[0038] 在上述制备高Al13含量聚合氯化铝的方法中,向二聚体Al2与多聚体Al6的混合溶液中加入NaAlO2溶液所进行的滴加反应完毕后,继续反应5〜IOmin后,得到Al13含量^ 97%,稳定时间> 24个月的液体聚合氯化铝。 [0038] In the above method for preparing high PAC content of Al13, After completion of the dropwise addition to the reaction with dimer Al2 NaAlO2 solution was added a mixed solution of polymer Al6 carried out, the reaction was continued after 5~IOmin, Al13 content of 97% to give ^, stabilization time> 24 months liquid PAC.

[0039] 本发明从Al13形成原理这个角度出发,先按一定比率将NaOH加入AlCl3溶液中调节溶液的PH值以合成八面体结构的AljP Al6 ;再向溶液中加入一定量的NaAlO2溶液,由于NaAlO2中的Al是以正四面体的Al (OH)4_形态存在,可以此为核心,与溶液中生成的八面体结构的Al2和Al6反应生成Al13。 [0039] The perspective of the present invention is formed from the principles of Al13, press a certain percentage of NaOH solution was added AlCl3 PH value of the solution was adjusted to AljP Al6 synthetic faujasite structure; and again was added an amount of NaAlO2 solution, since NaAlO2 Al is tetrahedral in the Al (OH) 4_ present form, this may be the core, and Al6 reaction of Al2 octahedral structure generated by the solution generating Al13. 这样不仅可以的得到高Al13含量、高Al总浓度的液体聚合氯化铝,而且实现了资源的高效合理利用,减少了生产聚合氯化铝中所造成的环境污染,符合“节能、环保”的可持续发展原则。 Not only can a high Al13 content, a high total concentration of Al in the liquid PAC, but also achieved a rational and efficient use of resources, reducing environmental pollution caused by the production of poly aluminum chloride, matching "energy saving, environmental protection" principles of sustainable development.

[0040] 本发明与现有的制备聚合氯化铝的方法相比,具有以下突出特点: [0040] Compared with the conventional method of preparation of polyaluminum chloride having the following salient features:

[0041 ] 1、工艺流程简单、生产成本低廉、生产效率高,无二次污染。 [0041] 1, the process is simple, low production costs, high production efficiency, without secondary pollution.

[0042] 2、所制备的聚合氯化铝性能优越,其中Al13含量> 97%、碱化度> 85%。 [0042] 2, the superior performance of polyaluminum chloride prepared wherein Al13 content of> 97%, degree of saponification of> 85%. 另外产品的稳定时间彡24个月。 In addition product of San settling time of 24 months.

具体实施方式 detailed description

[0043] 下面通过实施例对本发明做出进一步的说明。 [0043] The following make further illustrate the present invention through examples.

[0044] 实施例1 [0044] Example 1

[0045] 一种制备高Al13含量聚合氯化铝的方法,其制备步骤为: [0045] A high PAC content Al13 method for preparing the preparation steps of:

[0046] (I)取一定量的0.4mol/LAlCl3溶液于装有搅拌塞、搅拌棒、冷凝管的三口烧瓶中,恒温水浴加热至90°C ; [0046] (I) to take an amount of 0.4mol / LAlCl3 stopper was equipped with a stirred, a stirring bar, condenser three-necked flask, the water bath was heated to 90 ° C;

[0047] (2)照摩尔数比n(AlCl3): n(NaOH)为I: 1.5 的比例,取一定量的0.6mol/LNaOH溶液进行预加热,水浴温度为90°C ; [0047] (2) according to the molar ratio of the number n (AlCl3): n (NaOH) as I: 1.5 ratio, a certain amount of 0.6mol / LNaOH solution preheated water bath temperature 90 ° C;

[0048] (3)将预加热后的NaOH溶液加入AlCl3溶液中,加热搅拌,水浴温度为90°C,搅拌速度为100r/min ; [0048] (3) A NaOH solution was added to the preheated AlCl3 solution and heated with stirring in a water bath temperature of 90 ° C, stirring speed of 100r / min;

[0049] (4)待反应35min后,按照摩尔数比n(AlCl3): Ii(NaAlO2)为I: 0.5的比例,取一定量0.2mol/LNaA102溶液缓慢滴加到混合溶液中,加热搅拌,水浴温度为90°C,搅拌速度为130r/min,滴加时间为30min ; [0049] (4) After 35min of the reaction, according to the molar ratio n (AlCl3): Ii (NaAlO2) to I: 0.5 ratio, a certain amount 0.2mol / LNaA102 solution was slowly added dropwise to the mixed solution, heating and stirring, water bath temperature 90 ° C, stirring speed of 130r / min, for 30 min addition time;

[0050] (5)待滴加反应完毕后,继续反应5min,即得液体聚合氯化招成品。 After [0050] (5) was added dropwise until the reaction is completed, the reaction was continued for 5min, to give the finished product the liquid polymeric chloride strokes.

[0051] 对液体聚合氯化铝成品进行吸光度测定,计算Al的形态分布。 [0051] PAC finished liquid absorbance measured to calculate Al species distribution. 结果为:聚合氯化铝成品中Al13含量为94.20%,碱化度为85.3%。 Results: PAC content of the finished product Al13 94.20% degree of saponification was 85.3%.

[0052] 实施例2 [0052] Example 2

[0053] 一种制备高Al13含量聚合氯化铝的方法,其制备步骤为: [0053] A high PAC content Al13 method for preparing the preparation steps of:

[0054] (I)取一定量的0.5mol/LAlCl3溶液于装有搅拌塞、搅拌棒、冷凝管的三口烧瓶中,恒温水浴加热至85 °C ; [0054] (I) to take an amount of 0.5mol / LAlCl3 stopper was equipped with a stirred, a stirring bar, condenser three-necked flask, the water bath was heated to 85 ° C;

[0055] (2)照摩尔数比Ii(AlCl3): n(NaOH)为I: 1.6 的比例,取一定量的0.8mol/LNaOH溶液进行预加热,水浴温度为85 °C ; [0055] (2) according to the molar ratio Ii (AlCl3): n (NaOH) as I: 1.6 ratio, a certain amount of 0.8mol / LNaOH solution preheated water bath temperature of 85 ° C;

[0056] (3)将预加热后的NaOH溶液加入AlCl3溶液中,加热搅拌,水浴温度为85°C,搅拌速度为120r/min ; [0056] (3) A NaOH solution was added to the preheated AlCl3 solution and heated with stirring in a water bath temperature of 85 ° C, stirring speed of 120r / min;

[0057] (4)待反应30min后,按照摩尔数比n(AlCl3): n(NaA102)为I: 0.4的比例,取一定量0.4mol/LNaA102溶液缓慢滴加到混合溶液中,加热搅拌,水浴温度为85°C,搅拌速度为150r/min,滴加时间为20min ; [0057] (4) of the reaction after 30min, according to the molar ratio n (AlCl3): n (NaA102) to I: 0.4 ratio, a certain amount 0.4mol / LNaA102 solution was slowly added dropwise to the mixed solution, heating and stirring, water bath temperature of 85 ° C, stirring speed of 150r / min, dropwise over 20min;

[0058] (5)待滴加反应完毕后,继续反应IOmin,即得液体聚合氯化招成品。 After [0058] (5) was added dropwise until the reaction is complete, the reaction was continued IOmin, to obtain finished liquid polymeric move chloride.

[0059] 对液体聚合氯化铝成品进行吸光度测定,计算Al的形态分布。 [0059] PAC finished liquid absorbance measured to calculate Al species distribution. 结果为:聚合氯化铝成品中Al13含量为97.40%,碱化度为86.7%。 Results: PAC content of the finished product Al13 97.40%, degree of saponification 86.7%.

[0060] 实施例3 [0060] Example 3

[0061] —种制备闻Al13含量聚合氣化招的方法,其制备步骤为: [0061] - the content of the polymerization method for making the gasification Al13 move smell, preparation steps of:

[0062] (I)取一定量的0.6mol/LAlCl3溶液于装有搅拌塞、搅拌棒、冷凝管的三口烧瓶中,恒温水浴加热至80°C ; [0062] (I) to take an amount of 0.6mol / LAlCl3 stopper was equipped with a stirred, a stirring bar, condenser three-necked flask, the water bath was heated to 80 ° C;

[0063] (2)照摩尔数比Ii(AlCl3): n(Na0H)为I: 1.55 的比例,取一定量的0.7mol/LNaOH溶液进行预加热,水浴温度为80°C ; [0063] (2) according to the molar ratio Ii (AlCl3): n (Na0H) to I: 1.55 ratio, a certain amount of 0.7mol / LNaOH solution preheated water bath temperature 80 ° C;

[0064] (3)将预加热后的NaOH溶液加入AlCl3溶液中,加热搅拌,水浴温度为80〜90°C,搅拌速度为110r/min ; [0064] (3) A NaOH solution was added to the preheated AlCl3 solution and heated with stirring in a water bath temperature of 80~90 ° C, stirring speed of 110r / min;

[0065] (4)待反应25min后,按照摩尔数比Ii(AlCl3): Ii(NaAlO2)为I: 0.45的比例,取一定量0.3mol/LNaA102溶液缓慢滴加到混合溶液中,加热搅拌,水浴温度为80°C,搅拌速度为140r/min,滴加时间为25min ; [0065] (4) of the reaction after 25min, according to the molar ratio Ii (AlCl3): Ii (NaAlO2) to I: 0.45 ratio, a certain amount 0.3mol / LNaA102 solution was slowly added dropwise to the mixed solution, heating and stirring, water bath temperature of 80 ° C, stirring speed of 140r / min, dropwise over 25min;

[0066] (5)待滴加反应完毕后,继续反应8min,即得液体聚合氯化招成品。 After [0066] (5) was added dropwise until the reaction is complete, the reaction was continued 8min, to obtain finished liquid polymeric move chloride.

[0067] 对液体聚合氯化铝成品进行吸光度测定,计算Al的形态分布。 [0067] PAC finished liquid absorbance measured to calculate Al species distribution. 结果为:聚合氯化铝成品中Al13含量为95.10%,碱化度为85.8%。 Results: PAC content of the finished product Al13 95.10% degree of saponification was 85.8%. [0068] 实施例4 [0068] Example 4

[0069] 一种制备高Al13含量聚合氯化铝的方法,其制备步骤为: [0069] A high PAC content Al13 method for preparing the preparation steps of:

[0070] (I)取一定量的0.45mol/LA1C13溶液于装有搅拌塞、搅拌棒、冷凝管的三口烧瓶中,恒温水浴加热至90°C ; [0070] (I) a certain amount of 0.45mol / LA1C13 stopper was equipped with a stirred, a stirring bar, condenser three-necked flask, the water bath was heated to 90 ° C;

[0071] (2)照摩尔数比Ii(AlCl3): n(NaOH)为I: 1.6 的比例,取一定量的0.7mol/LNaOH溶液进行预加热,水浴温度为90°C ; [0071] (2) according to the molar ratio Ii (AlCl3): n (NaOH) as I: 1.6 ratio, a certain amount of 0.7mol / LNaOH solution preheated water bath temperature 90 ° C;

[0072] (3)将预加热后的NaOH溶液加入AlCl3溶液中,加热搅拌,水浴温度为90°C,搅拌速度为120r/min ; [0072] (3) A NaOH solution was added to the preheated AlCl3 solution and heated with stirring in a water bath temperature of 90 ° C, stirring speed of 120r / min;

[0073] (4)待反应35min后,按照摩尔数比n(AlCl3): Ii(NaAlO2)为I: 0.5的比例,取一定量0.4mol/LNaA102溶液缓慢滴加到混合溶液中,加热搅拌,水浴温度为90°C,搅拌速度为150r/min,滴加时间为30min ; [0073] (4) After 35min of the reaction, according to the molar ratio n (AlCl3): Ii (NaAlO2) to I: 0.5 ratio, a certain amount 0.4mol / LNaA102 solution was slowly added dropwise to the mixed solution, heating and stirring, water bath temperature 90 ° C, stirring speed of 150r / min, for 30 min addition time;

[0074] (5)待滴加反应完毕后,继续反应IOmin,即得液体聚合氯化招成品。 After [0074] (5) was added dropwise until the reaction is complete, the reaction was continued IOmin, to obtain finished liquid polymeric move chloride.

[0075] 对液体聚合氯化铝成品进行吸光度测定,计算Al的形态分布。 [0075] PAC finished liquid absorbance measured to calculate Al species distribution. 结果为:聚合氯化铝成品中Al13含量为96.10%,碱化度为86.4%。 Results: PAC content of the finished product Al13 96.10% degree of saponification was 86.4%.

[0076] 实施例5 [0076] Example 5

[0077] 一种制备高Al13含量聚合氯化铝的方法,其制备步骤为: [0077] A high PAC content Al13 method for preparing the preparation steps of:

[0078] (I)取一定量的0.55mol/LAlCl3溶液于装有搅拌塞、搅拌棒、冷凝管的三口烧瓶中,恒温水浴加热至80°C ; [0078] (I) a certain amount of 0.55mol / LAlCl3 stopper was equipped with a stirred, a stirring bar, condenser three-necked flask, the water bath was heated to 80 ° C;

[0079] (2)照摩尔数比Ii(AlCl3): n(NaOH)为I: 1.5 的比例,取一定量的0.6mol/LNaOH溶液进行预加热,水浴温度为80°C ; [0079] (2) according to the molar ratio Ii (AlCl3): n (NaOH) as I: 1.5 ratio, a certain amount of 0.6mol / LNaOH solution preheated water bath temperature 80 ° C;

[0080] (3)将预加热后的NaOH溶液加入AlCl3溶液中,加热搅拌,水浴温度为80〜90°C,搅拌速度为100r/min ; [0080] (3) A NaOH solution was added to the preheated AlCl3 solution and heated with stirring in a water bath temperature of 80~90 ° C, stirring speed of 100r / min;

[0081] (4)待反应30min后,按照摩尔数比n(AlCl3): n(NaA102)为I: 0.4的比例,取一定量0.2NaA102溶液缓慢滴加到混合溶液中,加热搅拌,水浴温度为80°C,搅拌速度为140r/min,滴加时间为25min ; [0081] (4) of the reaction after 30min, according to the molar ratio n (AlCl3): n (NaA102) to I: 0.4 ratio, a certain amount 0.2NaA102 solution was slowly added dropwise to the mixed solution, heating and stirring the water bath temperature to 80 ° C, stirring speed of 140r / min, dropwise over 25min;

[0082] (5)待滴加反应完毕后,继续反应5min,即得液体聚合氯化招成品。 After [0082] (5) was added dropwise until the reaction is completed, the reaction was continued for 5min, to give the finished product the liquid polymeric chloride strokes.

[0083] 对液体聚合氯化铝成品进行吸光度测定,计算Al的形态分布。 [0083] PAC finished liquid absorbance measured to calculate Al species distribution. 结果为:聚合氯化铝成品中Al13含量为94.50%,碱化度为85.9%。 Results: PAC content of the finished product Al13 94.50%, degree of saponification of 85.9%.

[0084] 实施例6 [0084] Example 6

[0085] 一种制备高Al13含量聚合氯化铝的方法,其制备步骤为: [0085] A high PAC content Al13 method for preparing the preparation steps of:

[0086] (I)取一定量的0.6mol/LAlCl3溶液于装有搅拌塞、搅拌棒、冷凝管的三口烧瓶中,恒温水浴加热至85 °C ; [0086] (I) to take an amount of 0.6mol / LAlCl3 stopper was equipped with a stirred, a stirring bar, condenser three-necked flask, the water bath was heated to 85 ° C;

[0087] (2)照摩尔数比Ii(AlCl3): n(NaOH)为I: 1.57 的比例,取一定量的0.65mol/LNaOH溶液进行预加热,水浴温度为85°C ; [0087] (2) according to the molar ratio Ii (AlCl3): n (NaOH) as I: 1.57 ratio, a certain amount of 0.65mol / LNaOH solution preheated water bath temperature of 85 ° C;

[0088] (3)将预加热后的NaOH溶液加入AlCl3溶液中,加热搅拌,水浴温度为85°C,搅拌速度为110r/min ; [0088] (3) A NaOH solution was added to the preheated AlCl3 solution and heated with stirring in a water bath temperature of 85 ° C, stirring speed of 110r / min;

[0089] (4)待反应25min后,按照摩尔数比Ii(AlCl3): Ii(NaAlO2)为I: 0.45的比例,取一定量0.25mol/LNaA102溶液缓慢滴加到混合溶液中,加热搅拌,水浴温度为85°C,搅拌速度为150r/min,滴加时间为25min ;[0090] (5)待滴加反应完毕后,继续反应IOmin,即得液体聚合氯化招成品。 [0089] (4) of the reaction after 25min, according to the molar ratio Ii (AlCl3): Ii (NaAlO2) to I: 0.45 ratio, a certain amount 0.25mol / LNaA102 solution was slowly added dropwise to the mixed solution, heating and stirring, water bath temperature of 85 ° C, stirring speed of 150r / min, dropwise over 25min; the [0090] (5) was added dropwise until the reaction is complete, the reaction was continued IOmin, to obtain finished liquid polymeric move chloride.

[0091] 对液体聚合氯化铝成品进行吸光度测定,计算Al的形态分布。 [0091] PAC finished liquid absorbance measured to calculate Al species distribution. 结果为:聚合氯化铝成品中Al13含量为96.80%,碱化度为87.3%。 Results: PAC content of the finished product Al13 96.80% degree of saponification was 87.3%.

Claims (3)

1.一种制备高Al13含量聚合氯化铝的方法,其特征在于:制备高Al13含量聚合氯化铝的原料采用结晶氯化铝、氢氧化钠、偏铝酸钠,制备高Al13含量聚合氯化铝的步骤如下: ⑴取一定量的浓度为0.4〜0.6mol/L的AlCl3溶液加入装有搅拌塞、搅拌棒、冷凝管的三口烧瓶中,恒温水浴加热,恒温水浴加热的温度为80〜90°C ; ⑵取一定量的浓度为0.6〜0.8mol/L的NaOH溶液进行预加热,预加热的温度为80〜90 0C ; ⑶将预加热后的NaOH溶液加入AlCl3溶液中,加热搅拌反应,使NaOH与AlCl3反应生成二聚体Al2和多聚体Al6,其中,预加热后的NaOH溶液加入AlCl3溶液中的量是按照摩尔数比Ii(AlCl3):n(NaOH)为1:1.5〜1.6的比例确定的,所进行的加热搅拌反应的水浴温度为80〜90°C,搅拌速度为100〜120r/min,加热搅拌反应的时间为25〜35min ; ⑷向二聚体Al2与多聚体Al6的混合溶液中加入浓度为0.2〜0.4mol/L的N 1. A high-PAC process for preparing Al13 content, wherein: the preparation of a high PAC content Al13 material in crystalline aluminum chloride, sodium hydroxide, sodium aluminate partial preparation of high chloride content of the polymerizable Al13 step aluminum follows: ⑴ certain amount of concentration 0.4~0.6mol / L of AlCl3 was added with stirring stopper, stir bar, condenser three-necked flask, heated water bath, a constant temperature water bath temperature of 80~ 90 ° C; ⑵ certain amount of concentration 0.6~0.8mol / L NaOH solution preheated, the preheating temperature is 80~90 0C; ⑶ the NaOH solution was added to the preheated AlCl3 solution, the reaction was heated with stirring the reaction of NaOH with AlCl3 Al2 generating dimers and multimers Al6, wherein, the NaOH solution was added in an amount preheating AlCl3 solution in accordance with the molar ratio Ii (AlCl3): n (NaOH) was 1: 1.5~ determining the ratio of 1.6, the reaction stirred for heating the water bath temperature is 80~90 ° C, the stirring speed is 100~120r / min, heating and stirring the reaction time is 25~35min; ⑷ to Al2 dimers and multimers Al6 a mixed solution thereof is added at a concentration of 0.2~0.4mol / L of N aAlO2溶液,进行加热搅拌反应,其中,加入NaAlO2溶液的量是按照摩尔数比n (AlCl3):n (NaAlO2)为1:0.4〜0.5的比例确定的,所进行的加热搅拌反应的水浴温度为80〜90°C,搅拌速度为130 〜150r/min ; (5)反应一定时间后,得到聚合氯化铝成品。 aAlO2 solution, the reaction was heated with stirring, wherein the amount of NaAlO2 solution was added to a molar ratio according to the number n (AlCl3): n (NaAlO2) is 1: 0.4~0.5 determined ratio, heating the water bath temperature for the reaction is carried out 80~90 ° C, stirring speed of 130 ~150r / min; (5) a certain reaction time, to give finished PAC.
2.根据权利要求1所述的一种制备高Al13含量聚合氯化铝的方法,其特征在于:向二聚体Al2与多聚体Al6的混合溶液中加入NaAlO2溶液的方法是采用缓慢滴加的方法进行的,滴加时间为20〜30min。 The preparation of a high content of Al13 PAC method according to claim 1, characterized in that: the method for mixing the solution with the dimers Al2 Al6 added NaAlO2 solution is the use of polymer was slowly added dropwise the method of addition time 20~30min.
3.根据权利要求1所述的一种制备高Al13含量聚合氯化铝的方法,其特征在于:向二聚体Al2与多聚体Al6的混合溶液中加入NaAlO2溶液所进行的滴加反应完毕后,继续反应5〜IOmin后,得到Al13含量> 97%,稳定时间> 24个月的液体聚合氯化铝。 The preparation of a high content of Al13 PAC method according to claim 1, wherein: NaAlO2 was added to complete the solution in a mixed solution Al6 Al2 dimers and multimers reaction was carried out dropwise after the reaction was continued after 5~IOmin, to give Al13 content> 97%, the stabilization time> 24 months liquid PAC.
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