CN102774940B - Preparation method of flocculant for removing low-temperature low-turbidity phosphorous wastewater - Google Patents
Preparation method of flocculant for removing low-temperature low-turbidity phosphorous wastewater Download PDFInfo
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- 239000002351 wastewater Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 title 1
- 238000003756 stirring Methods 0.000 claims abstract description 38
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000011574 phosphorus Substances 0.000 claims abstract description 36
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 14
- MGQIWUQTCOJGJU-UHFFFAOYSA-N [AlH3].Cl Chemical compound [AlH3].Cl MGQIWUQTCOJGJU-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 9
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims description 18
- SZEMGTQCPRNXEG-UHFFFAOYSA-M trimethyl(octadecyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C SZEMGTQCPRNXEG-UHFFFAOYSA-M 0.000 claims description 7
- 239000008394 flocculating agent Substances 0.000 claims description 6
- 238000005189 flocculation Methods 0.000 abstract description 9
- 230000016615 flocculation Effects 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 7
- 229940037003 alum Drugs 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 abstract 1
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 abstract 1
- 238000000034 method Methods 0.000 description 9
- 239000012153 distilled water Substances 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000007799 cork Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003337 fertilizer Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000000368 destabilizing effect Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Removal Of Specific Substances (AREA)
Abstract
本发明公开一种去除低温低浊度含磷废水絮凝剂的制备方法，在温度升高到65℃的铝盐酸溶液中加入Fe3O4粉、Al2(SO4)3、MgCl2、MnO2，并继续搅拌加热，当温度升高到85℃时，再加入一定质量Al2O3含量的铝酸钙粉，在温度115℃下搅拌反应2.5小时，在保持115℃温度，加入十八烷基三甲基溴化胺，继续搅拌，停止搅拌后熟化即可。本发明通过制备得到的一种多羟基多金属核的高分子无机絮凝剂，对处理含磷废水在低温、低浊度水絮凝效果显著，矾花形成时间短、絮体大、结实，并且处理水中磷含量可达到0.2mg/L以下，去除率达到97％以上。The invention discloses a preparation method of a flocculant for removing low-temperature and low-turbidity phosphorus-containing wastewater. Fe 3 O 4 powder, Al 2 (SO 4 ) 3 , MgCl 2 , and MnO are added to an aluminum hydrochloric acid solution whose temperature is raised to 65°C. 2 , and continue to stir and heat. When the temperature rises to 85°C, add calcium aluminate powder with a certain quality of Al 2 O 3 content, stir and react at 115°C for 2.5 hours, and keep the temperature at 115°C, add eighteen Alkyltrimethylammonium bromide, continue to stir, stop stirring and ripen. The polymer inorganic flocculant prepared by the present invention has a remarkable flocculation effect on the treatment of phosphorus-containing wastewater in low temperature and low turbidity water, the formation time of alum flowers is short, the flocs are large and firm, and the treatment The phosphorus content in the water can reach less than 0.2mg/L, and the removal rate can reach more than 97%.
Description
技术领域technical field
本发明属于水处理领域，具体的说是一种去除低温低浊度含磷废水絮凝剂的制备方法。The invention belongs to the field of water treatment, in particular to a preparation method of a flocculant for removing low-temperature, low-turbidity phosphorus-containing wastewater.
背景技术Background technique
磷是重要的工业原材料，在化肥、洗涤剂、食品饮料、冶金等工业生产中都有广泛应用，因此在工业生产中不可避免地产生含磷废水，如果将未经处理的含磷废水排放到水体中，不仅会造成磷资源的浪费，更重要的是磷在水中属于富营养物质，水体中磷含量超过50μg/L就有助于藻类的生长，并影响地表水的质量。研究高效的除磷剂提高混凝效果，对控制企业排放污水的磷含量以便保持水体安全具有重要意义。Phosphorus is an important industrial raw material, which is widely used in industrial production such as chemical fertilizers, detergents, food and beverage, and metallurgy. Therefore, phosphorus-containing wastewater is inevitably generated in industrial production. If the untreated phosphorus-containing wastewater is discharged to In the water body, it will not only cause a waste of phosphorus resources, but more importantly, phosphorus is a eutrophic substance in the water. The phosphorus content in the water body exceeds 50 μg/L, which will help the growth of algae and affect the quality of surface water. It is of great significance to study the efficient phosphorus removal agent to improve the coagulation effect to control the phosphorus content of sewage discharged by enterprises so as to maintain the safety of water body.
目前，国内外常用去除含磷废水常用的的方法为吸附方法和絮凝方法，通常采用的絮凝剂一般以投加聚合氯化铝、聚合硫酸铁、聚合氯化铝铁等无机絮凝剂来处理，但是普通的絮凝剂在处理水水温低、而且浊度低，澄清、透明，使得絮凝剂的絮凝效果不明显，磷去除率不高。如辽河化肥厂，以聚合硫化铝为絮凝剂，聚丙烯酰胺为助凝剂来处理含磷废水，这种方法主要是通过电中和与吸附架桥使水中的磷和机械杂质脱稳定来达到去除磷的目的，虽然此方法在一定程度上对含磷废水的去除效果有所明显，但是，在水温低、浊度低的情况下絮凝剂的絮凝效果却不明显，很难形成矾花，去除率不高。At present, the commonly used methods for removing phosphorus-containing wastewater at home and abroad are adsorption method and flocculation method. The flocculants usually used are generally treated by adding inorganic flocculants such as polyaluminum chloride, polyferric sulfate, and polyaluminum ferric chloride. However, common flocculants treat water with low temperature, low turbidity, clarity, and transparency, so that the flocculation effect of the flocculant is not obvious, and the removal rate of phosphorus is not high. For example, the Liaohe Chemical Fertilizer Plant uses polyaluminum sulfide as a flocculant and polyacrylamide as a coagulant to treat phosphorus-containing wastewater. This method is mainly achieved by destabilizing phosphorus and mechanical impurities in the water through electrical neutralization and adsorption bridging. The purpose of phosphorus removal, although this method has obvious removal effect on phosphorus-containing wastewater to a certain extent, but the flocculation effect of flocculant is not obvious in the case of low water temperature and low turbidity, and it is difficult to form alum flowers. The removal rate is not high.
发明内容Contents of the invention
为了解决由于处理水水温通常较低，而且浊度低，澄清、透明，导致絮凝剂的絮凝效果不明显，磷的去除率不高等问题，本发明公开了一种去除低温低浊度含磷废水絮凝剂的制备方法。In order to solve the problems that the treatment water temperature is usually low, and the turbidity is low, clear and transparent, the flocculation effect of the flocculant is not obvious, and the removal rate of phosphorus is not high. The preparation method of flocculant.
本发明采用的技术方案如下：The technical scheme that the present invention adopts is as follows:
一种去除低温、低浊度含磷废水絮凝剂的制备方法，其方法在于：A preparation method for removing low-temperature, low-turbidity phosphorus-containing wastewater flocculants, the method comprising:
(1)取250mL三口圆底烧瓶一个，中间瓶口装上搅拌机，左侧瓶口插入温度计，向右侧瓶口中加入50～55mL铝盐酸，铝盐酸中Al2O3含量为2～3％，酸度为7.2％，再加入175～180mL水，塞紧瓶塞，在电炉中加热并搅拌；(1) Take a 250mL three-necked round-bottomed flask, install a stirrer in the middle of the bottle, insert a thermometer into the left bottle, and add 50-55mL aluminum hydrochloric acid to the right bottle, the content of Al 2 O 3 in aluminum hydrochloric acid is 2-3% , with an acidity of 7.2%, add 175-180mL of water, stopper the bottle tightly, heat and stir in an electric furnace;
(2)当加热温度升高到65℃时加入3～5gFe3O4粉，20～22gAl2(SO4)3，8～10gMgCl2，2～3gMnO2，继续搅拌加热；(2) When the heating temperature rises to 65°C, add 3-5g Fe 3 O 4 powder, 20-22g Al 2 (SO 4 ) 3 , 8-10g MgCl 2 , 2-3g MnO 2 , and continue stirring and heating;
(3)当加热温度升高到85℃时，加入50～52gAl2O3含量为52％的铝酸钙粉，迅速反应，温度上升，在温度115℃下搅拌反应2.5小时；(3) When the heating temperature rises to 85°C, add 50-52g of calcium aluminate powder with an Al 2 O 3 content of 52%, react rapidly, and the temperature rises, and stir and react at a temperature of 115°C for 2.5 hours;
(4)保持115℃温度，加入3～5g十八烷基三甲基溴化胺，继续搅拌20分钟后，停止搅拌，熟化即可。(4) Keeping the temperature at 115°C, add 3 to 5 g of octadecyltrimethylammonium bromide, continue stirring for 20 minutes, stop stirring, and mature.
一种去除低温、低浓度含磷废水絮凝剂的应用方法在于：A kind of application method of removing low-temperature, low-concentration phosphorus-containing wastewater flocculant is:
把制得的絮凝剂用蒸馏水稀释10倍后，取0.5～0.7mL稀释液加入到100mL澄清、透明的天然水体(或二沉池出水)中，迅速搅拌，可见有矾花形成，絮体逐渐变大，沉淀后，测得上清液中磷含量在0.2mg/L以下。After diluting the prepared flocculant 10 times with distilled water, take 0.5-0.7mL of the diluted solution and add it to 100mL of clear and transparent natural water (or the effluent of the secondary sedimentation tank), and stir rapidly. It can be seen that alum flowers are formed, and the flocs gradually After precipitation, the phosphorus content in the supernatant was measured to be below 0.2mg/L.
本发明的显著优势在于：Significant advantage of the present invention is:
(1)制备得到一种多羟基多金属核的高分子无机絮凝剂体，其中Al3+含量为12％～15％，Fe3+含量为1％～2％，Fe2+含量为2％～5％，Mg2+含量为12％～13％，Mn2+含量为2％～3％，除此之外，还含有10％～12％的SO4 2-，含量为0.1％～0.6％十八烷基三甲基溴化胺；(1) Prepare a polymer inorganic flocculant body with polyhydroxyl and polymetallic cores, wherein the content of Al 3+ is 12% to 15%, the content of Fe 3+ is 1% to 2%, and the content of Fe 2+ is 2% ~5%, Mg 2+ content is 12% ~ 13%, Mn 2+ content is 2% ~ 3%, in addition, it also contains 10% ~ 12% SO 4 2- , the content is 0.1% ~ 0.6 % octadecyltrimethylammonium bromide;
(2)对低温、低浊度水絮凝效果好，矾花形成时间短，絮体大，结实。(2) The flocculation effect is good for low temperature and low turbidity water, the formation time of alum flowers is short, and the flocs are large and firm.
具体实施方式Detailed ways
一种去除低温、低浊度含磷废水絮凝剂的制备方法，其方法在于：A preparation method for removing low-temperature, low-turbidity phosphorus-containing wastewater flocculants, the method comprising:
(1)取250mL三口圆底烧瓶一个，中间瓶口装上搅拌机，左侧瓶口插入温度计，向右侧瓶口中加入50～55mL铝盐酸，铝盐酸中Al2O3含量为2～3％，酸度为7.2％，再加入175～180mL水，塞紧瓶塞，在电炉中加热并搅拌；(1) Take a 250mL three-necked round-bottomed flask, install a stirrer in the middle of the bottle, insert a thermometer into the left bottle, and add 50-55mL aluminum hydrochloric acid to the right bottle, the content of Al 2 O 3 in aluminum hydrochloric acid is 2-3% , with an acidity of 7.2%, add 175-180mL of water, stopper the bottle tightly, heat and stir in an electric furnace;
(2)当加热温度升高到65℃时加入3～5gFe3O4粉，20～22gAl2(SO4)3，8～10gMgCl2，2～3gMnO2，继续搅拌加热；(2) When the heating temperature rises to 65°C, add 3-5g Fe 3 O 4 powder, 20-22g Al 2 (SO 4 ) 3 , 8-10g MgCl 2 , 2-3g MnO 2 , and continue stirring and heating;
(3)当加热温度升高到85℃时，加入50～52gAl2O3含量为52％的铝酸钙粉，迅速反应，温度上升，在温度115℃下搅拌反应2.5小时；(3) When the heating temperature rises to 85°C, add 50-52g of calcium aluminate powder with an Al 2 O 3 content of 52%, react rapidly, and the temperature rises, and stir and react at a temperature of 115°C for 2.5 hours;
(4)保持115℃温度，加入3～5g十八烷基三甲基溴化胺，继续搅拌20分钟后，停止搅拌，熟化即可。(4) Keeping the temperature at 115°C, add 3 to 5 g of octadecyltrimethylammonium bromide, continue stirring for 20 minutes, stop stirring, and mature.
以下通过实例对本发明做详细说明The present invention is described in detail below by example
实例1Example 1
首先取250mL三口圆底烧瓶一个，在中间瓶口装上搅拌机，左侧瓶口插入温度计，向右侧瓶口中加入50mL铝盐酸和175mL水，塞紧瓶塞后在电炉中加热并搅拌，当加热温度升高到65℃时加入3gFe3O4粉、20gAl2(SO4)、38gMgCl2、2gMnO2，继续搅拌加热，当加热温度升高到85℃时，加入50gAl2O3含量为52％的铝酸钙粉，迅速反应，温度上升，在温度115℃下搅拌反应2.5小时，保持115℃温度，加入3g十八烷基三甲基溴化胺，继续搅拌20分钟后，停止搅拌后熟化即可。First, take a 250mL three-neck round bottom flask, install a blender on the middle bottle mouth, insert a thermometer into the left bottle mouth, add 50mL aluminum hydrochloric acid and 175mL water to the right bottle mouth, and heat and stir in an electric furnace after the cork is tightly closed. When the heating temperature rises to 65°C, add 3g Fe 3 O 4 powder, 20gAl 2 (SO 4 ), 38gMgCl 2 , 2gMnO 2 , continue stirring and heating, and when the heating temperature rises to 85°C, add 50gAl 2 O 3 with a content of 52% calcium aluminate powder reacts quickly, the temperature rises, stir and react at 115°C for 2.5 hours, keep the temperature at 115°C, add 3g of octadecyltrimethylammonium bromide, continue stirring for 20 minutes, then stop stirring Post-ripening can be done.
对某河流中废水进行除磷处理，将上述制得的絮凝剂用蒸馏水稀释10倍后，取0.5mL稀释液加如废水中，原水总磷为103.5mg/L，pH3.9，首先将原水pH调为5.0，经迅速搅拌，絮凝反应、沉淀后，测得上清液中磷含量在0.2mg/L以下，磷去除率达到97％以上。To remove phosphorus from wastewater in a certain river, dilute the flocculant prepared above by 10 times with distilled water, then take 0.5mL of the diluted solution and add it to the wastewater. The total phosphorus in the raw water is 103.5mg/L, pH3.9. The pH is adjusted to 5.0, and after rapid stirring, flocculation reaction and precipitation, the phosphorus content in the supernatant is measured to be below 0.2mg/L, and the phosphorus removal rate reaches above 97%.
实例2Example 2
首先取250mL三口圆底烧瓶一个，在中间瓶口装上搅拌机，左侧瓶口插入温度计，向右侧瓶口中加入53mL铝盐酸和177mL水，塞紧瓶塞后在电炉中加热并搅拌，当加热温度升高到65℃时加入4gFe3O4粉、21gAl2(SO4)3、9gMgCl2、2.5gMnO2，继续搅拌加热，当加热温度升高到85℃时，加入51gAl2O3含量为52％的铝酸钙粉，迅速反应，温度上升，在温度115℃下搅拌反应2.5小时，保持115℃温度，加入4g十八烷基三甲基溴化胺，继续搅拌20分钟后，停止搅拌后熟化即可。First, take a 250mL three-neck round bottom flask, install a blender on the middle bottle mouth, insert a thermometer into the left bottle mouth, add 53mL aluminum hydrochloric acid and 177mL water to the right bottle mouth, and heat and stir in an electric furnace after the cork is tightly closed. When the heating temperature rises to 65°C, add 4g Fe 3 O 4 powder, 21g Al 2 (SO 4 ) 3 , 9gMgCl 2 , 2.5g MnO 2 , continue stirring and heating, when the heating temperature rises to 85°C, add 51g Al 2 O 3 content It is 52% calcium aluminate powder, reacts rapidly, the temperature rises, stirs and reacts at a temperature of 115°C for 2.5 hours, maintains a temperature of 115°C, adds 4g of octadecyltrimethylammonium bromide, continues to stir for 20 minutes, and then stops Stir and ripen.
取天然废水进行除磷处理，将上述制得的絮凝剂用蒸馏水稀释10倍后，取0.6mL稀释液加如废水中，原水总磷为103.5mg/L，pH3.9，首先将原水pH调为7.0，经迅速搅拌，絮凝反应、沉淀后，测得上清液中磷含量在0.18mg/L以下，磷去除率达到98％以上。Take natural wastewater for phosphorus removal treatment, dilute the flocculant prepared above 10 times with distilled water, take 0.6mL of the diluted solution and add it to the wastewater, the total phosphorus in the raw water is 103.5mg/L, and the pH is 3.9. After rapid stirring, flocculation reaction, and precipitation, the phosphorus content in the supernatant was measured to be below 0.18mg/L, and the phosphorus removal rate reached above 98%.
实例3Example 3
首先取250mL三口圆底烧瓶一个，在中间瓶口装上搅拌机，左侧瓶口插入温度计，向右侧瓶口中加入55mL铝盐酸和180mL水，塞紧瓶塞后在电炉中加热并搅拌，当加热温度升高到65℃时加入5gFe3O4粉、22gAl2(SO4)3、10gMgCl2、3gMnO2，继续搅拌加热，当加热温度升高到85℃时，加入52gAl2O3含量为52％的铝酸钙粉，迅速反应，温度上升，在温度115℃下搅拌反应2.5小时，保持115℃温度，加入5g十八烷基三甲基溴化胺，继续搅拌20分钟后，停止搅拌后熟化即可。First, take a 250mL three-neck round bottom flask, install a blender on the middle bottle mouth, insert a thermometer into the left bottle mouth, add 55mL aluminum hydrochloric acid and 180mL water to the right bottle mouth, and heat and stir in an electric furnace after the cork is tightly closed. When the heating temperature rises to 65°C, add 5g of Fe 3 O 4 powder, 22g of Al 2 (SO 4 ) 3 , 10g of MgCl 2 , and 3g of MnO 2 , and continue stirring and heating. When the heating temperature rises to 85°C, add 52g of Al 2 O 3 with a content of 52% calcium aluminate powder reacts quickly, the temperature rises, stir and react at 115°C for 2.5 hours, keep the temperature at 115°C, add 5g of octadecyltrimethylammonium bromide, continue stirring for 20 minutes, then stop stirring Post-ripening can be done.
对某河流废水进行除磷处理，将上述制得的絮凝剂用蒸馏水稀释10倍后，取0.7mL稀释液加入废水中，原水总磷为103.5mg/L，pH3.9，首先将原水pH调为8.0，经迅速搅拌，絮凝反应、沉淀后，测得上清液中磷含量在0.15mg/L以下，磷去除率达到99％以上。To remove phosphorus from a certain river wastewater, dilute the flocculant prepared above 10 times with distilled water, then take 0.7mL of the diluted solution and add it to the wastewater. The total phosphorus in the raw water is 103.5mg/L, and the pH is 3.9. After rapid stirring, flocculation reaction, and precipitation, the phosphorus content in the supernatant was measured to be below 0.15mg/L, and the phosphorus removal rate reached more than 99%.
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