WO2019051743A1 - Method for preparing polyaluminum chloride-chitosan composite flocculant - Google Patents
Method for preparing polyaluminum chloride-chitosan composite flocculant Download PDFInfo
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- WO2019051743A1 WO2019051743A1 PCT/CN2017/101803 CN2017101803W WO2019051743A1 WO 2019051743 A1 WO2019051743 A1 WO 2019051743A1 CN 2017101803 W CN2017101803 W CN 2017101803W WO 2019051743 A1 WO2019051743 A1 WO 2019051743A1
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
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Abstract
Disclosed is a method for preparing a polyaluminum chloride-chitosan composite flocculant, comprising the following steps: dissolving 4-8 parts of aluminum chloride hexahydrate into 80-90 parts of deionized water, slowly dropwise adding 60-70 parts of a 0.5 mol/mL NaOH solution under the conditions of rapid magnetic stirring at 40ºC-50ºC, and 2-4 h after the addition, curing same for 1-2 d, heating and stirring same at 80ºC-90ºC, and condensing and refluxing same for 10-12 h to obtain a PAC solution; adding 10-15 parts of chitosan into 40-50 parts of an acetic acid solution of 2% by volume, and rapidly magnetically stirring same until completely dissolved to obtain an acetic acid solution of CTS; taking 50-60 parts of a PAC solution, slowly dropwise adding 10-20 parts of the acetic acid solution of CTS under the conditions of rapid magnetic stirring, and stirring same until uniform to obtain the polymerized aluminum chloride-chitosan composite flocculant. The method is simple in process and easy to operate, and can quickly prepare a composite flocculant with a strong flocculation capability.
Description
本发明涉及一种聚合氯化铝-壳聚糖复合絮凝剂的制备方法。The invention relates to a preparation method of a polyaluminum chloride-chitosan composite flocculant.
絮凝是水处理的重要环节,絮凝剂可以凝聚悬浮物或胶体形成大的絮体。聚合氯化铝(PAC)作为目前水厂广泛使用的无机絮凝剂,与传统的铝盐(非聚合态)相比,它能适应更为复杂的水质,产生更少的剩余污泥和降低出水中的残留铝浓度,近年来在水处理领域受到广泛关注。PAC中Al水解能力的大小对絮凝起到重要作用,PAC中Al的水解能力和形态与传统单体铝盐中Al的水解相差较大。通常情况下,由于传统单体铝盐的水解比较难控制,所以后者的絮凝能力比前者弱。不同PAC中的Al的水解聚合程度也不尽相同,即会水解形成不同形态的聚合态的铝。Flocculation is an important part of water treatment. Flocculants can aggregate suspended solids or colloids to form large flocs. Polyaluminium chloride (PAC) is an inorganic flocculant widely used in water plants. Compared with traditional aluminum salts (non-polymerized), it can adapt to more complex water quality, produce less excess sludge and reduce it. The residual aluminum concentration in water has received extensive attention in the field of water treatment in recent years. The hydrolysis capacity of Al in PAC plays an important role in flocculation. The hydrolysis ability and morphology of Al in PAC differs greatly from the hydrolysis of Al in the traditional monomer aluminum salt. In general, the flocculation ability of the latter is weaker than the former because the hydrolysis of the conventional monomer aluminum salt is more difficult to control. The degree of hydrolysis polymerization of Al in different PACs is also different, that is, it will hydrolyze to form aluminum in different forms of polymerized state.
壳聚糖(CTS)因其天然、无毒、安全性而被美国环保局批准作为饮用水的净化剂,CTS是一种线性的聚合氨基糖类物质,是由甲壳素通过碱性脱乙酰作用得到的,不溶于水,溶于酸。CTS具有可生物降解性、生物适应性和絮凝性能,并且可以通过一系列的反应程序后再生。CTS水解产生的高阳离子浓度使其具有较强的絮凝能力,可能在较低剂量时通过桥联和电性中和作用表现出来。目前,壳聚糖多通过改性或与其他絮凝剂复配使用来提高水处理效果。Chitosan (CTS) is approved by the US Environmental Protection Agency as a purifying agent for drinking water because of its natural, non-toxic and safe nature. CTS is a linear polymeric amino sugar substance which is deacetylated by chitin. Obtained, insoluble in water, soluble in acid. CTS is biodegradable, biocompatible and flocculated and can be regenerated after a series of reaction procedures. The high cation concentration produced by the hydrolysis of CTS gives it a strong flocculation capacity, which may be manifested by bridging and electrical neutralization at lower doses. At present, chitosan is often modified or used in combination with other flocculants to improve water treatment.
发明内容Summary of the invention
本发明的目的在于提供一种聚合氯化铝-壳聚糖复合絮凝剂的制备方法。The object of the present invention is to provide a preparation method of a polyaluminum chloride-chitosan composite flocculant.
本发明通过下面技术方案实现:The invention is achieved by the following technical solutions:
一种聚合氯化铝-壳聚糖复合絮凝剂的制备方法,包括如下步骤:将4-8份六水合氯化铝溶解于80-90份去离子水中,40-50℃快速磁力搅拌条件下慢速滴加60-70份0.5moL/mL的NaOH溶液,2-4h滴完,熟化1-2d后,在80-90℃下加热搅拌,冷凝回流10-12h,得PAC溶液;将10-15份壳聚糖加入40-50份体积分数为2%的乙酸溶液中,快速磁力搅拌至完全溶解,得CTS乙酸溶液;取50-60份PAC溶液,在快速磁力搅拌条件下慢速滴加10-20份CTS乙酸溶液,搅拌均匀后即得;各原料均为重量份。The invention discloses a preparation method of a polyaluminum chloride-chitosan composite flocculant, comprising the following steps: dissolving 4-8 parts of aluminum chloride hexahydrate in 80-90 parts of deionized water, and rapidly magnetic stirring under 40-50 ° C Slowly add 60-70 parts of 0.5mL/mL NaOH solution, 2-4h drop, mature 1-2d, stir at 80-90 °C, condense reflux for 10-12h, get PAC solution; 15 parts of chitosan is added to 40-50 parts of a 2% acetic acid solution, stirred rapidly to complete dissolution to obtain CTS acetic acid solution; 50-60 parts of PAC solution is taken, and slowly added under rapid magnetic stirring conditions. 10-20 parts of CTS acetic acid solution, obtained after stirring uniformly; each raw material is part by weight.
优选地,所述的制备方法中,45℃快速磁力搅拌条件下慢速滴加65份0.5moL/mL的NaOH溶液。Preferably, in the preparation method, 65 parts of a 0.5 mol/mL NaOH solution is slowly added dropwise under a rapid magnetic stirring condition at 45 °C.
优选地,所述的制备方法中,3h滴完。Preferably, in the preparation method, the dropwise addition is carried out for 3 hours.
优选地,所述的制备方法中,熟化1.5d。
Preferably, in the preparation method, it is aged for 1.5 days.
优选地,所述的制备方法中,在85℃下加热搅拌,冷凝回流11h。Preferably, in the preparation method, the mixture is heated and stirred at 85 ° C, and condensed and refluxed for 11 hours.
本发明技术效果:The technical effect of the invention:
本发明提供的方法流程简单,易操作,可快速制得絮凝能力强的复合絮凝剂。The method provided by the invention has simple and easy operation, and can quickly produce a composite flocculating agent with strong flocculation ability.
下面结合实施例具体介绍本发明的实质性内容。The substantial content of the present invention will be specifically described below with reference to the embodiments.
实施例1Example 1
一种聚合氯化铝-壳聚糖复合絮凝剂的制备方法,包括如下步骤:将6份六水合氯化铝溶解于85份去离子水中,45℃快速磁力搅拌条件下慢速滴加65份0.5moL/mL的NaOH溶液,3h滴完,熟化1.5d后,在85℃下加热搅拌,冷凝回流11h,得PAC溶液;将12份壳聚糖加入45份体积分数为2%的乙酸溶液中,快速磁力搅拌至完全溶解,得CTS乙酸溶液;取55份PAC溶液,在快速磁力搅拌条件下慢速滴加15份CTS乙酸溶液,搅拌均匀后即得;各原料均为重量份。A preparation method of a polyaluminum chloride-chitosan composite flocculant comprises the following steps: dissolving 6 parts of aluminum chloride hexahydrate in 85 parts of deionized water, and slowly adding 65 parts under rapid magnetic stirring at 45 ° C 0.5moL / mL NaOH solution, 3h drop, after aging for 1.5d, heated and stirred at 85 ° C, condensed and refluxed for 11h, to obtain PAC solution; 12 parts of chitosan was added to 45 parts by volume of 2% acetic acid solution , rapid magnetic stirring until completely dissolved, to obtain CTS acetic acid solution; take 55 parts of PAC solution, slowly add 15 parts of CTS acetic acid solution under rapid magnetic stirring conditions, and stir evenly; each raw material is part by weight.
实施例2Example 2
一种聚合氯化铝-壳聚糖复合絮凝剂的制备方法,包括如下步骤:将4份六水合氯化铝溶解于80份去离子水中,40℃快速磁力搅拌条件下慢速滴加60份0.5moL/mL的NaOH溶液,2h滴完,熟化1d后,在80℃下加热搅拌,冷凝回流10h,得PAC溶液;将10份壳聚糖加入40份体积分数为2%的乙酸溶液中,快速磁力搅拌至完全溶解,得CTS乙酸溶液;取50份PAC溶液,在快速磁力搅拌条件下慢速滴加10份CTS乙酸溶液,搅拌均匀后即得;各原料均为重量份。A preparation method of a polyaluminum chloride-chitosan composite flocculant comprises the following steps: dissolving 4 parts of aluminum chloride hexahydrate in 80 parts of deionized water, and slowly adding 60 parts under rapid magnetic stirring at 40 ° C 0.5moL / mL NaOH solution, 2h drop, after aging for 1d, heated at 80 ° C, condensed and refluxed for 10h to obtain PAC solution; 10 parts of chitosan was added to 40 parts by volume of 2% acetic acid solution, Rapid magnetic stirring until completely dissolved, to obtain CTS acetic acid solution; take 50 parts of PAC solution, slowly add 10 parts of CTS acetic acid solution under rapid magnetic stirring conditions, and stir evenly; each raw material is part by weight.
实施例3Example 3
一种聚合氯化铝-壳聚糖复合絮凝剂的制备方法,包括如下步骤:将8份六水合氯化铝溶解于90份去离子水中,50℃快速磁力搅拌条件下慢速滴加70份0.5moL/mL的NaOH溶液,4h滴完,熟化2d后,在90℃下加热搅拌,冷凝回流12h,得PAC溶液;将15份壳聚糖加入50份体积分数为2%的乙酸溶液中,快速磁力搅拌至完全溶解,得CTS乙酸溶液;取60份PAC溶液,在快速磁力搅拌条件下慢速滴加20份CTS乙酸溶液,搅拌均匀后即得;各原料均为重量份。A preparation method of a polyaluminum chloride-chitosan composite flocculant comprises the following steps: dissolving 8 parts of aluminum chloride hexahydrate in 90 parts of deionized water, and slowly adding 70 parts under rapid magnetic stirring at 50 ° C 0.5moL / mL NaOH solution, 4h drop, after 2d aging, heated and stirred at 90 ° C, condensed reflux for 12h, to obtain PAC solution; 15 parts of chitosan was added to 50 parts by volume of 2% acetic acid solution, Rapid magnetic stirring until completely dissolved, to obtain CTS acetic acid solution; take 60 parts of PAC solution, slowly add 20 parts of CTS acetic acid solution under rapid magnetic stirring conditions, and stir evenly; each raw material is part by weight.
本发明提供的方法流程简单,易操作,可快速制得絮凝能力强的复合絮凝剂。
The method provided by the invention has simple and easy operation, and can quickly produce a composite flocculating agent with strong flocculation ability.
Claims (5)
- 一种聚合氯化铝-壳聚糖复合絮凝剂的制备方法,其特征在于包括如下步骤:将4-8份六水合氯化铝溶解于80-90份去离子水中,40-50℃快速磁力搅拌条件下慢速滴加60-70份0.5moL/mL的NaOH溶液,2-4h滴完,熟化1-2d后,在80-90℃下加热搅拌,冷凝回流10-12h,得PAC溶液;将10-15份壳聚糖加入40-50份体积分数为2%的乙酸溶液中,快速磁力搅拌至完全溶解,得CTS乙酸溶液;取50-60份PAC溶液,在快速磁力搅拌条件下慢速滴加10-20份CTS乙酸溶液,搅拌均匀后即得;各原料均为重量份。The invention discloses a preparation method of polyaluminum chloride-chitosan composite flocculant, which comprises the following steps: dissolving 4-8 parts of aluminum chloride hexahydrate in 80-90 parts of deionized water, 40-50 ° C fast magnetic force 60-70 parts of 0.5 mol/mL NaOH solution was slowly added dropwise under stirring, and the mixture was 2-4 h, and after 1-2 d of aging, the mixture was heated and stirred at 80-90 ° C, and condensed and refluxed for 10-12 h to obtain a PAC solution; Add 10-15 parts of chitosan to 40-50 parts by volume of 2% acetic acid solution, stir rapidly to complete dissolution to obtain CTS acetic acid solution; take 50-60 parts of PAC solution, slow under rapid magnetic stirring conditions 10-20 parts of CTS acetic acid solution was added dropwise, and the mixture was uniformly stirred; each raw material was in parts by weight.
- 根据权利要求1所述的制备方法,其特征在于:45℃快速磁力搅拌条件下慢速滴加65份0.5moL/mL的NaOH溶液。The preparation method according to claim 1, characterized in that 65 parts of a 0.5 mol/mL NaOH solution is slowly added dropwise under a rapid magnetic stirring condition at 45 °C.
- 根据权利要求1所述的制备方法,其特征在于:3h滴完。The preparation method according to claim 1, wherein the dropping is completed in 3 hours.
- 根据权利要求1所述的制备方法,其特征在于:熟化1.5d。The preparation method according to claim 1, wherein the curing is performed for 1.5 days.
- 根据权利要求1所述的制备方法,其特征在于:在85℃下加热搅拌,冷凝回流11h。 The preparation method according to claim 1, wherein the mixture is heated and stirred at 85 ° C, and condensed and refluxed for 11 hours.
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CN111547828A (en) * | 2020-04-10 | 2020-08-18 | 佛山华清智业环保科技有限公司 | Composite flocculant and preparation method and application thereof |
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JPH1157314A (en) * | 1997-08-26 | 1999-03-02 | Chikanosuke Oki | Flocculant |
CN1654348A (en) * | 2005-01-20 | 2005-08-17 | 上海师范大学 | Composite flocculating agent for printing and dyeing waste water treatment |
CN1785836A (en) * | 2005-10-28 | 2006-06-14 | 上海工程技术大学 | High efficiency composite flocculant, its preparation method and application |
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CN111547828A (en) * | 2020-04-10 | 2020-08-18 | 佛山华清智业环保科技有限公司 | Composite flocculant and preparation method and application thereof |
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