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CN101733078A - Method for preparing phosphorous-removing adsorbent by using cane shoots leaves - Google Patents

Method for preparing phosphorous-removing adsorbent by using cane shoots leaves Download PDF

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CN101733078A
CN101733078A CN201010300282A CN201010300282A CN101733078A CN 101733078 A CN101733078 A CN 101733078A CN 201010300282 A CN201010300282 A CN 201010300282A CN 201010300282 A CN201010300282 A CN 201010300282A CN 101733078 A CN101733078 A CN 101733078A
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zizania
phosphorus
adsorbent
leaves
preparing
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郭萃萍
丁剑
黄大成
曹玮
张从发
朱鹏波
范同祥
张荻
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Shanghai Jiao Tong University
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Abstract

一种环保技术领域的利用茭白叶制备除磷吸附剂的方法,该方法包括如下步骤:步骤一,取工业废渣铁泥和硫酸铵,混合,加热,用盐酸浸渍,得溶液;步骤二,取茭白叶,粉碎,浸渍于步骤一所得溶液中;步骤三,真空抽滤洗涤;步骤四,重复步骤三的操作直至洗涤后得到的清洗液为无色,得固体物,烘干,得茭白叶除磷吸附剂;本发明的技术方案工艺简单,不需高温焙烧,所得吸附剂适用的pH值范围广,除磷效果好,吸附剂除磷时间短以及吸附量大,最高可达2.02mg/g,对于治理富营养化废水有着良好的应用前景。A method for preparing a phosphorus-removing adsorbent in the field of environmental protection technology using Zizania leaves, the method comprising the following steps: step 1, taking industrial waste iron sludge and ammonium sulfate, mixing, heating, and impregnating with hydrochloric acid to obtain a solution; step 2, taking Zizania leaves, pulverized, soaked in the solution obtained in step 1; step 3, vacuum filtration and washing; step 4, repeating the operation of step 3 until the cleaning solution obtained after washing is colorless, and the solid is obtained, dried to obtain Zizania leaves Phosphorus removal adsorbent; the technical scheme of the present invention is simple in process and does not require high-temperature roasting, and the obtained adsorbent has a wide range of applicable pH values, good phosphorus removal effect, short time for phosphorus removal by the adsorbent and large adsorption capacity, up to 2.02mg/ g, has a good application prospect for the treatment of eutrophic wastewater.

Description

利用茭白叶制备除磷吸附剂的方法 Method for preparing phosphorus-removing adsorbent by using bamboo leaves

技术领域technical field

本发明涉及一种环保技术领域的制备方法,具体是一种利用茭白叶制备除磷吸附剂的方法。The invention relates to a preparation method in the technical field of environmental protection, in particular to a method for preparing a phosphorus-removing adsorbent by using bamboo leaves.

背景技术Background technique

当水体中营养物质(一般指氮和磷的化合物)无机态总氮含量>0.2mg/L,总磷含量>0.02mg/L时,会引起水体植物(如藻类及大型植物)大量生长的藻华现象。藻华现象高频发生已严重影响到居民的饮水安全、水产养殖、水体景观价值等方面,造成了巨大的经济损失。氮在自然界中有一个完整的循环:生物(有机物)→氨→亚硝酸盐→硝酸盐→生物(有机物),所以不容易在实际水体中富集造成氮污染。而由于自然界中磷不存在完整循环,所以磷容易富集造成污染。因此防止水体富营养化关键是要控制其中的磷含量。When the inorganic total nitrogen content of nutrients (generally referring to nitrogen and phosphorus compounds) in the water body is greater than 0.2 mg/L, and the total phosphorus content is greater than 0.02 mg/L, it will cause a large number of water plants (such as algae and large plants) to grow. Chinese phenomenon. The frequent occurrence of algal blooms has seriously affected residents' drinking water safety, aquaculture, and the value of water landscapes, causing huge economic losses. Nitrogen has a complete cycle in nature: biological (organic matter) → ammonia → nitrite → nitrate → biological (organic matter), so it is not easy to enrich in actual water bodies and cause nitrogen pollution. And because there is no complete cycle of phosphorus in nature, phosphorus is easy to enrich and cause pollution. Therefore, the key to preventing eutrophication of water bodies is to control the phosphorus content in them.

目前除磷方法有常规的生物除磷法、化学除磷法等方法。生物除磷法除磷周期长;化学除磷法操作简单,但是药剂费用高,并且生成的化学沉淀难处理,造成二次污染。At present, the phosphorus removal methods include conventional biological phosphorus removal method, chemical phosphorus removal method and other methods. The biological phosphorus removal method has a long period of phosphorus removal; the chemical phosphorus removal method is simple to operate, but the cost of chemicals is high, and the resulting chemical precipitation is difficult to handle, causing secondary pollution.

经对现有技术的文献检索发现,Indian Journal of Chemical Technology(印度化学技术杂志),1999年,第6卷,第256~262页《Phosphate adsorption studies usingcarbon prepared from stem bark of Eucalyptus teriticornis Smith(利用细叶桉树的树皮制备所得碳的磷吸附研究)》披露了如下技术内容:用桉树皮制备得到的炭,经硫酸浸渍后得到吸附剂并用于吸附磷,但此种方法原料有限,工艺复杂,并且所制备的吸附剂对磷的吸附受溶液pH值影响大,且对磷吸附量均低于1mg/g。Found through literature search to prior art, Indian Journal of Chemical Technology (Indian Chemical Technology Journal), 1999, volume 6, pages 256-262 "Phosphate adsorption studies using carbon prepared from stem bark of Eucalyptus teriticornis Smith (utilizing fine Phosphorus adsorption research on the carbon prepared from the bark of Eucalyptus eucalyptus)" discloses the following technical content: the charcoal prepared from eucalyptus bark is impregnated with sulfuric acid to obtain an adsorbent and is used to adsorb phosphorus, but this method has limited raw materials and complicated processes. Moreover, the adsorption of phosphorus by the prepared adsorbent is greatly affected by the pH value of the solution, and the adsorption amount of phosphorus is all lower than 1 mg/g.

发明内容Contents of the invention

本发明的目的在于克服现有技术的不足,提供一种利用茭白叶制备除磷吸附剂的方法。本发明的技术方案工艺简单,不需高温焙烧,所得吸附剂适用的pH值范围广,除磷效果好,吸附剂除磷时间短以及吸附量大,最高可达2.02mg/g,对于治理富营养化废水有着良好的应用前景。The purpose of the present invention is to overcome the deficiencies of the prior art, and provide a method for preparing a phosphorus-removing adsorbent by using water bamboo leaves. The technical solution of the present invention is simple in process and does not require high-temperature roasting. The obtained adsorbent has a wide range of applicable pH values, good phosphorus removal effect, short time for phosphorus removal by the adsorbent, and large adsorption capacity, up to 2.02 mg/g. Nutritious wastewater has a good application prospect.

本发明是通过以下的技术方案实现的,本发明包括如下步骤:The present invention is achieved through the following technical solutions, and the present invention comprises the following steps:

步骤一,取工业废渣铁泥和硫酸铵,混合,加热,用盐酸浸渍,得溶液;Step 1, taking industrial waste iron sludge and ammonium sulfate, mixing, heating, and impregnating with hydrochloric acid to obtain a solution;

步骤二,取茭白叶,粉碎,浸渍于步骤一所得溶液中;Step 2, taking Zizania zizania leaves, crushing them, and soaking them in the solution obtained in Step 1;

步骤三,真空抽滤洗涤;Step 3, vacuum filtration and washing;

步骤四,重复步骤三的操作直至洗涤后得到的清洗液为无色,得固体物,烘干,得茭白叶除磷吸附剂。Step 4, repeating the operation of step 3 until the cleaning solution obtained after washing is colorless, and a solid is obtained, which is then dried to obtain an adsorbent for removing phosphorus from bamboo leaves.

步骤一中,按重量比,工业废渣铁泥与硫酸铵的比例为(1~3)∶1。In step 1, the ratio of industrial waste iron sludge to ammonium sulfate is (1-3):1 by weight.

步骤一中,所述加热具体为加热到150~200℃。In step 1, the heating is specifically heating to 150-200°C.

步骤一中,所述盐酸的体积百分数为10%~37%。In step 1, the volume percentage of the hydrochloric acid is 10%-37%.

步骤一中,所述溶液中Fe3+的浓度为20~300g/L。In step 1, the concentration of Fe 3+ in the solution is 20-300 g/L.

步骤二中,所述浸渍的时间为10~30h。In step 2, the soaking time is 10-30 hours.

步骤四中,所述烘干具体为:60~80℃下烘6~10h。In step 4, the drying is specifically: drying at 60-80° C. for 6-10 hours.

与现有技术相比,本发明具有如下的有益效果:本发明的技术方案中采用的原料之一茭白(Zizania aquatica L.)来源广泛,成本低,有利于农业废弃物的循环利用,对环境友好;同时,本发明的技术方案工艺简单,不需高温焙烧,所得吸附剂适用的pH值范围广,除磷效果好,吸附剂除磷时间短以及吸附量大,最高可达2.02mg/g,对于治理富营养化废水有着良好的应用前景。Compared with the prior art, the present invention has the following beneficial effects: one of the raw materials used in the technical solution of the present invention, Zizania aquatica L., has a wide range of sources, low cost, is conducive to the recycling of agricultural waste, and is environmentally friendly. Friendly; at the same time, the technical scheme of the present invention is simple in process, does not require high-temperature roasting, and the obtained adsorbent has a wide range of pH values, good phosphorus removal effect, short time for phosphorus removal by the adsorbent and large adsorption capacity, up to 2.02mg/g , has a good application prospect for the treatment of eutrophic wastewater.

具体实施方式Detailed ways

本实施例在以本发明技术方案为前提下进行实施,给出了详细的实施方式和过程,但本发明的保护范围不限于下述的实施例。下列实施例中未注明具体条件的实验方法,通常按照常规条件,或按照制造厂商所建议的条件。This embodiment is carried out on the premise of the technical solution of the present invention, and detailed implementation methods and processes are given, but the protection scope of the present invention is not limited to the following embodiments. For the experimental methods without specific conditions indicated in the following examples, the conventional conditions or the conditions suggested by the manufacturer are usually followed.

以下实施例中,所述“工业废渣铁泥“是钢铁工业中种类最多、成分最杂的废弃物,一般含铁的质量分数为30%~70%,该技术术语是本领域技术人员所熟知的。In the following examples, the "industrial waste slag and iron sludge" is the waste with the most types and the most miscellaneous components in the iron and steel industry. Generally, the mass fraction of iron is 30% to 70%. This technical term is well known to those skilled in the art of.

实施例1Example 1

步骤一,按重量比,将工业废渣铁泥与硫酸铵按1∶1比例进行混合;加热至150℃,再用体积分数为10%盐酸进行浸渍,待样品溶解完全后,充分搅拌,得到富含Fe3+的铁盐溶液,使得溶液中Fe3+的浓度为20g/L;Step 1: Mix industrial waste iron sludge and ammonium sulfate in a ratio of 1:1 according to the weight ratio; heat to 150°C, then impregnate with hydrochloric acid with a volume fraction of 10%, and stir fully after the sample is completely dissolved to obtain rich Iron salt solution containing Fe 3+ , so that the concentration of Fe 3+ in the solution is 20g/L;

步骤二,取茭白叶,粉碎,之后将碎屑浸渍于步骤一所得溶液中,浸渍10h;Step 2, taking Zizania bamboo leaves, crushing them, and then soaking the debris in the solution obtained in Step 1 for 10 hours;

步骤三,真空抽滤洗涤;此步骤中的真空抽虑和洗涤是同时进行的,即边抽虑边洗涤,真空抽虑是为了使洗涤速度加快;Step 3, vacuum filtration and washing; vacuum filtration and washing in this step are carried out simultaneously, that is, washing while suction and filtration, and vacuum filtration is to accelerate the washing speed;

步骤四,重复步骤三的操作直至洗涤后得到的清洗液为无色,将所得到的固体物在烘箱中在60℃下烘干6h,得茭白叶除磷吸附剂。Step 4, repeating the operation of Step 3 until the cleaning solution obtained after washing is colorless, and drying the obtained solid in an oven at 60° C. for 6 hours to obtain an adsorbent for removing phosphorus from Zizania bamboo leaves.

实施效果:将本实施例所得的吸附剂加入到pH值为2的磷酸二氢钠(NaH2PO4)水溶液中进行吸附,吸附效果为1.54mg/g。Implementation effect: the adsorbent obtained in this example was added to an aqueous solution of sodium dihydrogen phosphate (NaH 2 PO 4 ) with a pH value of 2 for adsorption, and the adsorption effect was 1.54 mg/g.

实施例2Example 2

步骤一,按重量比,将工业废渣铁泥与硫酸铵按2∶1比例进行混合;加热至175℃,再用体积分数为25%盐酸进行浸渍,待样品溶解完全后,充分搅拌,得到富含Fe3+的铁盐溶液,使得溶液中Fe3+的浓度为100g/L;Step 1: Mix industrial waste iron sludge and ammonium sulfate at a ratio of 2:1 according to the weight ratio; heat to 175°C, then impregnate with hydrochloric acid with a volume fraction of 25%, and stir fully after the sample is completely dissolved to obtain rich Iron salt solution containing Fe 3+ , so that the concentration of Fe 3+ in the solution is 100g/L;

步骤二,取茭白叶,粉碎,之后将碎屑浸渍于步骤一所得溶液中,浸渍30h;Step 2: Take Zizania bamboo leaves, crush them, and then soak the debris in the solution obtained in Step 1 for 30 hours;

步骤三,真空抽滤洗涤;此步骤中的真空抽虑和洗涤是同时进行的,即边抽虑边洗涤,真空抽虑是为了使洗涤速度加快;Step 3, vacuum filtration and washing; vacuum filtration and washing in this step are carried out simultaneously, that is, washing while suction and filtration, and vacuum filtration is to accelerate the washing speed;

步骤四,重复步骤三的操作直至洗涤后得到的清洗液为无色,将所得到的固体物在烘箱中在70℃下烘干8h,得茭白叶除磷吸附剂。Step 4, repeating the operation of Step 3 until the cleaning solution obtained after washing is colorless, and drying the obtained solid matter in an oven at 70° C. for 8 hours to obtain an adsorbent for dephosphorization of Zizania bamboo leaves.

实施效果:将本实施例所得的吸附剂加入到pH值为7的磷酸二氢钠(NaH2PO4)水溶液中进行吸附,吸附效果为2.02mg/g。Implementation effect: the adsorbent obtained in this example was added to an aqueous solution of sodium dihydrogen phosphate (NaH 2 PO 4 ) with a pH value of 7 for adsorption, and the adsorption effect was 2.02 mg/g.

实施例3Example 3

步骤一,按重量比,将工业废渣铁泥与硫酸铵按3∶1比例进行混合;加热至200℃,再用体积分数为37%盐酸进行浸渍,待样品溶解完全后,充分搅拌,得到富含Fe3+的铁盐溶液,使得溶液中Fe3+的浓度为300g/L;Step 1: Mix industrial waste iron sludge and ammonium sulfate at a ratio of 3:1 according to the weight ratio; heat to 200°C, then impregnate with hydrochloric acid with a volume fraction of 37%, and stir fully after the sample is completely dissolved to obtain rich Iron salt solution containing Fe 3+ , so that the concentration of Fe 3+ in the solution is 300g/L;

步骤二,取茭白叶,粉碎,之后将碎屑浸渍于步骤一所得溶液中,浸渍20h;Step 2, taking Zizania bamboo leaves, crushing them, and then soaking the debris in the solution obtained in Step 1 for 20 hours;

步骤三,真空抽滤洗涤;此步骤中的真空抽虑和洗涤是同时进行的,即边抽虑边洗涤,真空抽虑是为了使洗涤速度加快;Step 3, vacuum filtration and washing; vacuum filtration and washing in this step are carried out simultaneously, that is, washing while suction and filtration, and vacuum filtration is to accelerate the washing speed;

步骤四,重复步骤三的操作直至洗涤后得到的清洗液为无色,将所得到的固体物在烘箱中在80℃下烘干10h,得茭白叶除磷吸附剂。Step 4, repeating the operation of Step 3 until the cleaning solution obtained after washing is colorless, and drying the obtained solid in an oven at 80° C. for 10 hours to obtain an adsorbent for removing phosphorus from Zizania bamboo leaves.

实施效果:将本实施例所得的吸附剂加入到pH值为10的磷酸二氢钠(NaH2PO4)水溶液中进行吸附,吸附效果为1.88mg/g。Implementation effect: the adsorbent obtained in this example was added to an aqueous solution of sodium dihydrogen phosphate (NaH 2 PO 4 ) with a pH value of 10 for adsorption, and the adsorption effect was 1.88 mg/g.

Claims (7)

1.一种利用茭白叶制备除磷吸附剂的方法,其特征在于,包括如下步骤:1. a method utilizing Zizania japonica leaf to prepare phosphorus removal sorbent, is characterized in that, comprises the steps: 步骤一,取工业废渣铁泥和硫酸铵,混合,加热,用盐酸浸渍,得溶液;Step 1, taking industrial waste iron sludge and ammonium sulfate, mixing, heating, and impregnating with hydrochloric acid to obtain a solution; 步骤二,取茭白叶,粉碎,浸渍于步骤一所得溶液中;Step 2, taking Zizania zizania leaves, crushing them, and soaking them in the solution obtained in Step 1; 步骤三,真空抽滤洗涤;Step 3, vacuum filtration and washing; 步骤四,重复步骤三的操作直至洗涤后得到的清洗液为无色,得固体物,烘干,得茭白叶除磷吸附剂。Step 4, repeating the operation of step 3 until the cleaning solution obtained after washing is colorless, and a solid is obtained, which is then dried to obtain an adsorbent for removing phosphorus from bamboo leaves. 2.根据权利要求1所述的利用茭白叶制备除磷吸附剂的方法,其特征是,步骤一中,按重量比,工业废渣铁泥与硫酸铵的比例为(1~3)∶1。2. The method for preparing a phosphorus-removing sorbent by using Zizania japonica leaves according to claim 1, characterized in that, in step 1, by weight, the ratio of industrial waste iron sludge to ammonium sulfate is (1~3): 1. 3.根据权利要求1所述的利用茭白叶制备除磷吸附剂的方法,其特征是,步骤一中,所述加热具体为加热到150~200℃。3. The method for preparing a phosphorus-removing adsorbent by using Zizania ziba leaves according to claim 1, characterized in that, in step 1, the heating is specifically heating to 150-200°C. 4.根据权利要求1所述的利用茭白叶制备除磷吸附剂的方法,其特征是,步骤一中,所述盐酸的体积百分数为10%~37%。4. The method for preparing a phosphorus-removing adsorbent by using leaves of Zizania japonica according to claim 1, characterized in that, in step 1, the volume percentage of the hydrochloric acid is 10% to 37%. 5.根据权利要求1所述的利用茭白叶制备除磷吸附剂的方法,其特征是,步骤一中,所述溶液中Fe3+的浓度为20~300g/L。5 . The method for preparing a phosphorus-removing adsorbent by using leaves of Zizania japonica according to claim 1 , characterized in that, in step 1, the concentration of Fe3+ in the solution is 20 to 300 g/L. 6.根据权利要求1所述的利用茭白叶制备除磷吸附剂的方法,其特征是,步骤二中,所述浸渍的时间为10~30h。6 . The method for preparing a phosphorus-removing adsorbent by using Zizania zizania leaves according to claim 1 , characterized in that, in step 2, the soaking time is 10 to 30 hours. 7.根据权利要求1所述的利用茭白叶制备除磷吸附剂的方法,其特征是,步骤四中,所述烘干具体为:60~80℃下烘6~10h。7. The method for preparing a phosphorus-removing adsorbent by using Zizania bamboo leaves according to claim 1, characterized in that, in step 4, the drying is specifically: drying at 60-80°C for 6-10 hours.
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CN105080500A (en) * 2015-05-18 2015-11-25 江苏大学 Natural dye wastewater adsorbent and preparation and application method thereof
CN105502554A (en) * 2015-11-26 2016-04-20 辽宁石油化工大学 Method for removal of malachite green from wastewater with Acer mono Maxim deciduous leaf biosorbent
CN109289798A (en) * 2018-11-29 2019-02-01 运城学院 A kind of method that utilizes malic acid modification to prepare phosphorus removing adsorbent

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* Cited by examiner, † Cited by third party
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CN104986822A (en) * 2015-06-19 2015-10-21 华东理工大学 Preparation method and regeneration method for chemical-modified iron-carrying peanut shell phosphorous removal material
CN104986822B (en) * 2015-06-19 2017-03-08 华东理工大学 Preparation and regeneration method of chemically modified iron-loaded peanut shell phosphorus removal material
CN105502554A (en) * 2015-11-26 2016-04-20 辽宁石油化工大学 Method for removal of malachite green from wastewater with Acer mono Maxim deciduous leaf biosorbent
CN105502554B (en) * 2015-11-26 2018-04-06 辽宁石油化工大学 The method for removing waste water Malachite Green using acer monoes fallen leaves biological adsorption agent
CN109289798A (en) * 2018-11-29 2019-02-01 运城学院 A kind of method that utilizes malic acid modification to prepare phosphorus removing adsorbent

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