CN103241779A - Preparation method of polyferric sulfate (PFS) - Google Patents
Preparation method of polyferric sulfate (PFS) Download PDFInfo
- Publication number
- CN103241779A CN103241779A CN201310215351XA CN201310215351A CN103241779A CN 103241779 A CN103241779 A CN 103241779A CN 201310215351X A CN201310215351X A CN 201310215351XA CN 201310215351 A CN201310215351 A CN 201310215351A CN 103241779 A CN103241779 A CN 103241779A
- Authority
- CN
- China
- Prior art keywords
- preparation
- sulfate
- ferric sulfate
- polyferric sulfate
- add
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 title abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 17
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims abstract description 17
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 10
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 8
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 7
- 150000002505 iron Chemical class 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 10
- 229910001448 ferrous ion Inorganic materials 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims 1
- 239000007800 oxidant agent Substances 0.000 abstract description 11
- 230000003647 oxidation Effects 0.000 abstract description 10
- 238000007254 oxidation reaction Methods 0.000 abstract description 10
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 abstract description 9
- 239000000701 coagulant Substances 0.000 abstract description 9
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 abstract description 9
- 230000001590 oxidative effect Effects 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 7
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 230000015271 coagulation Effects 0.000 abstract description 3
- 238000005345 coagulation Methods 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 230000007062 hydrolysis Effects 0.000 abstract description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 2
- 230000009972 noncorrosive effect Effects 0.000 abstract description 2
- 238000006116 polymerization reaction Methods 0.000 abstract description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 abstract 1
- 229910052742 iron Inorganic materials 0.000 abstract 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 20
- 239000011734 sodium Substances 0.000 description 17
- 235000003891 ferrous sulphate Nutrition 0.000 description 12
- 239000011790 ferrous sulphate Substances 0.000 description 12
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 12
- 239000012153 distilled water Substances 0.000 description 11
- 239000002351 wastewater Substances 0.000 description 9
- 239000002994 raw material Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 3
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 239000010842 industrial wastewater Substances 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Landscapes
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
本发明涉及一种聚合硫酸铁的制备方法，其是通过将一定量的二价铁盐溶解于水中，通过硫酸调整其pH值后水浴加热搅拌，加入一定量的过硫酸盐作为氧化剂氧化溶液中的Fe2+，经水解聚合得到聚合硫酸铁（PFS），为聚合硫酸铁的制备提供了一种新的方法，本发明的方法工艺简单且所制备的聚合硫酸铁混凝剂的混凝效果好，浊度去除率高，可达94.6%，而且所制备的聚合硫酸铁混凝剂的各项指标均符合GB14591-2006水处理剂聚合硫酸铁的要求，此外本方法所需投加硫酸亚铁用量少，氧化剂过硫酸钠的投加速度易于控制，使得二价铁被充分氧化，且操作工艺简单，无腐蚀性，pH适用范围广，成本低，性能好，具有很良好的市场前景。The present invention relates to a preparation method of polymerized ferric sulfate, which comprises dissolving a certain amount of divalent iron salt in water, adjusting its pH value with sulfuric acid, heating and stirring in a water bath, and adding a certain amount of persulfate as an oxidizing agent into the oxidation solution. Fe 2+ obtained by hydrolysis and polymerization to obtain polyferric sulfate (PFS), which provides a new method for the preparation of polyferric sulfate. The method of the present invention has simple process and the coagulation effect of the prepared polyferric sulfate coagulant Good, the turbidity removal rate is high, up to 94.6%, and the indicators of the prepared polymeric ferric sulfate coagulant are in line with the requirements of GB14591-2006 water treatment agent polymeric ferric sulfate. In addition, this method needs to add sulfurous acid The dosage of iron is small, and the feeding speed of oxidant sodium persulfate is easy to control, so that the ferrous iron is fully oxidized, and the operation process is simple, non-corrosive, wide range of pH, low cost, good performance, and has a very good market prospect.
Description
技术领域technical field
本发明属于用于工业废水、城市污水及给水处理的混凝剂的研究技术领域，特别涉及一种聚合硫酸铁的制备方法。The invention belongs to the technical field of research on coagulants used for industrial waste water, urban sewage and water supply treatment, and in particular relates to a preparation method of polyferric sulfate.
背景技术Background technique
混凝剂是一种可使液体中分散的细粒固体形成絮凝物的高分子聚合物，与水任意比混合，可广泛用于工业废水、城市污水及给水的处理。目前，常用的混凝剂有碱式氯化铝、聚合硫酸铁、三氯化铁及硫酸铝。聚合硫酸铁具有以下优点：絮凝体形成速度快，颗粒密实，沉降速度快，对于各种废水中的COD、BOD、浊度、色度及重金属有良好的去除效果，并且对所处理废水pH值及水温适应范围广，对污泥有良好的脱水性。Coagulant is a polymer that can form flocs from fine-grained solids dispersed in liquids. It can be mixed with water in any ratio and can be widely used in the treatment of industrial wastewater, urban sewage and water supply. At present, the commonly used coagulants are basic aluminum chloride, polyferric sulfate, ferric chloride and aluminum sulfate. Polyferric sulfate has the following advantages: fast formation of flocs, dense particles, fast settling speed, good removal effect on COD, BOD, turbidity, chroma and heavy metals in various wastewater, and pH value of treated wastewater And the water temperature adapts to a wide range, and has good dehydration for sludge.
制备聚合硫酸铁常用的方法主要是直接氧化法，直接氧化法主要有H2O2氧化法、KClO3/NaClO3氧化法、HNO3氧化法和NaClO氧化法等，直接氧化法由于使用的氧化剂价格高，因此产品成本较高同时反应过程中还存在一些其他问题，如H2O2氧化，反应过程非常剧烈且放出大量的热，而高温又加速H2O2分解，对氧化剂造成浪费的同时又难以合理地控制氧化剂的投加速度；KClO3/NaClO3氧化法的产物中有残留的Cl-和ClO3 -不宜用于给水处理，且KClO3价格较贵，限制了其大规模工业生产，同时在反应过程中还会产生大量Cl2，泄露会造成空气污染；而HNO3氧化法还需增加尾气吸收装置，导致设备结构复杂，工艺成本增加。因此，对于聚合硫酸铁的制备仍然需要进一步的研究。The commonly used method for preparing polyferric sulfate is mainly direct oxidation method, which mainly includes H 2 O 2 oxidation method, KClO 3 /NaClO 3 oxidation method, HNO 3 oxidation method and NaClO oxidation method, etc. The direct oxidation method is due to the oxidant used The price is high, so the product cost is high. At the same time, there are some other problems in the reaction process, such as H 2 O 2 oxidation, the reaction process is very violent and releases a lot of heat, and the high temperature accelerates the decomposition of H 2 O 2 , which causes waste of oxidants. At the same time, it is difficult to reasonably control the dosage rate of the oxidant; there are residual Cl - and ClO 3 - in the product of the KClO 3 /NaClO 3 oxidation method, which is not suitable for water treatment, and the price of KClO 3 is relatively expensive, which limits its large-scale industrial production At the same time, a large amount of Cl 2 will be produced during the reaction process, and leakage will cause air pollution; while the HNO 3 oxidation method also needs to add an exhaust gas absorption device, resulting in complex equipment structure and increased process costs. Therefore, the preparation of polyferric sulfate still needs further research.
发明内容Contents of the invention
为了克服现有技术中的聚合硫酸铁的制备方法所存在的不足，本发明提供了一种制备工艺简单、混凝效果好、浊度去除率高的聚合硫酸铁混凝剂的制备方法。In order to overcome the deficiencies in the preparation method of polyferric sulfate in the prior art, the present invention provides a preparation method of polyferric sulfate coagulant with simple preparation process, good coagulation effect and high turbidity removal rate.
本发明解决上述技术问题所采用的技术方案是：称取可溶性二价铁盐，加水至二价铁离子的浓度为56g/L，加入过硫酸盐至溶液中二价铁离子与过硫酸根的摩尔比为1：0.1～1.0，优选1：0.4～0.8，20～85℃搅拌反应0.5～4小时，得到聚合硫酸铁。The technical solution adopted by the present invention to solve the above-mentioned technical problems is: take soluble ferrous salt, add water to the concentration of ferrous ion is 56g/L, add persulfate to the concentration of ferrous ion and persulfate in the solution The molar ratio is 1:0.1-1.0, preferably 1:0.4-0.8, stirred and reacted at 20-85°C for 0.5-4 hours to obtain polyferric sulfate.
上述反应条件中优选反应温度为25～65℃，反应时间为1～3小时。Among the above reaction conditions, the preferred reaction temperature is 25-65° C., and the reaction time is 1-3 hours.
上述可溶性二价铁盐可以是FeCl2、FeSO4以及Fe(NO3)2中的任意一种。The above-mentioned soluble ferrous salt may be any one of FeCl 2 , FeSO 4 and Fe(NO 3 ) 2 .
上述过硫酸盐是Na2S2O8或K2S2O8。The aforementioned persulfate is Na 2 S 2 O 8 or K 2 S 2 O 8 .
还可以在二价铁盐溶于水后向溶液中滴加硫酸或盐酸调整pH至3～7。It is also possible to add sulfuric acid or hydrochloric acid dropwise to the solution after the ferrous salt is dissolved in water to adjust the pH to 3-7.
本发明的聚合硫酸铁混凝剂的制备方法是通过将一定量的二价铁盐溶解于水中，通过硫酸调整其pH值后水浴加热搅拌，加入一定量的过硫酸盐作为氧化剂氧化溶液中的Fe2+，经水解聚合得到聚合硫酸铁（PFS），为聚合硫酸铁的制备提供了一种新的方法，本发明的方法工艺简单且所制备的聚合硫酸铁混凝剂的混凝效果好，浊度去除率高，可达94.6%，而且所制备的聚合硫酸铁混凝剂的各项指标均符合GB14591-2006水处理剂聚合硫酸铁的要求，此外本方法所需投加硫酸亚铁用量少，氧化剂过硫酸钠的投加速度易于控制，使得二价铁被充分氧化，且操作工艺简单，无腐蚀性，pH适用范围广，成本低，性能好，具有很良好的市场前景。The preparation method of the polyferric sulfate coagulant of the present invention is by dissolving a certain amount of divalent iron salt in water, adjusting its pH value by sulfuric acid, heating and stirring in a water bath, adding a certain amount of persulfate as an oxidizing agent to oxidize the solution Fe 2+ , polymerized ferric sulfate (PFS) is obtained through hydrolysis and polymerization, which provides a new method for the preparation of polymerized ferric sulfate. The method of the present invention has a simple process and the coagulation effect of the prepared polymerized ferric sulfate coagulant is good , the turbidity removal rate is high, up to 94.6%, and the indicators of the prepared polymeric ferric sulfate coagulant are in line with the requirements of GB14591-2006 water treatment agent polymeric ferric sulfate, in addition, this method needs to add ferrous sulfate The dosage is small, the feeding speed of the oxidant sodium persulfate is easy to control, so that the ferrous iron is fully oxidized, and the operation process is simple, non-corrosive, wide range of pH, low cost, good performance, and has a very good market prospect.
附图说明Description of drawings
图1为过硫酸钠投加量对同一浊度废水去浊率的影响。Figure 1 shows the effect of sodium persulfate dosage on the turbidity removal rate of wastewater with the same turbidity.
图2为温度对同一浊度废水去浊率的影响。Figure 2 is the effect of temperature on the turbidity removal rate of wastewater with the same turbidity.
图3为反应时间对同一浊度废水去浊率的影响。Figure 3 is the effect of reaction time on the turbidity removal rate of wastewater with the same turbidity.
具体实施方式Detailed ways
现结合实验对本发明的技术方案进行进一步说明，但是本发明不仅限于下述实施的情形。The technical solution of the present invention will now be further described in conjunction with experiments, but the present invention is not limited to the following implementation situations.
实施例1Example 1
以可溶性二价铁盐选硫酸亚铁为例，制备聚合硫酸铁的方法为：称取13.9gFeSO4放置于250mL的锥形瓶中，加入50mL的蒸馏水至FeSO4的浓度为56g/L，加入7.14g Na2S2O8，FeSO4与Na2S2O8的摩尔比为1：0.6，保证溶液中Fe2+与S2O8 2-的摩尔比为1:0.6，水浴加热至65℃搅拌反应2小时，得到聚合硫酸铁。Taking ferrous sulfate as an example of soluble ferrous salt, the method for preparing polyferric sulfate is: weigh 13.9g FeSO 4 and place it in a 250mL Erlenmeyer flask, add 50mL of distilled water until the concentration of FeSO 4 is 56g/L, add 7.14 g Na 2 S 2 O 8 , the molar ratio of FeSO 4 to Na 2 S 2 O 8 is 1:0.6, and the molar ratio of Fe 2+ to S 2 O 8 2- in the solution is 1:0.6, and the water bath is heated to Stir and react at 65°C for 2 hours to obtain polymerized ferric sulfate.
实施例2Example 2
以可溶性二价铁盐选硫酸亚铁为例，制备聚合硫酸铁的方法为：称取13.9gFeSO4放置于250mL的锥形瓶中，加入50mL的蒸馏水至FeSO4的浓度为56g/L，加入4.76g Na2S2O8，FeSO4与Na2S2O8的摩尔比为1：0.4，25℃搅拌反应3小时，得到聚合硫酸铁。Taking ferrous sulfate as an example of soluble ferrous salt, the method for preparing polyferric sulfate is: weigh 13.9g FeSO 4 and place it in a 250mL Erlenmeyer flask, add 50mL of distilled water until the concentration of FeSO 4 is 56g/L, add 4.76g of Na 2 S 2 O 8 , the molar ratio of FeSO 4 to Na 2 S 2 O 8 is 1:0.4, stirred and reacted at 25°C for 3 hours to obtain polyferric sulfate.
实施例3Example 3
以可溶性二价铁盐选硫酸亚铁为例，制备聚合硫酸铁的方法为：称取13.9gFeSO4放置于250mL的锥形瓶中，加入50mL的蒸馏水至FeSO4的浓度为56g/L，加入9.52g Na2S2O8，FeSO4与Na2S2O8的摩尔比为1：0.8，水浴加热至60℃搅拌反应1小时，得到聚合硫酸铁。Taking ferrous sulfate as an example of soluble ferrous salt, the method for preparing polyferric sulfate is: weigh 13.9g FeSO 4 and place it in a 250mL Erlenmeyer flask, add 50mL of distilled water until the concentration of FeSO 4 is 56g/L, add 9.52g of Na 2 S 2 O 8 , the molar ratio of FeSO 4 to Na 2 S 2 O 8 is 1:0.8, heated in a water bath to 60°C and stirred for 1 hour to obtain polyferric sulfate.
实施例4Example 4
以可溶性二价铁盐选硫酸亚铁为例，制备聚合硫酸铁的方法为：称取13.9gFeSO4放置于250mL的锥形瓶中，加入50mL的蒸馏水至FeSO4的浓度为56g/L，加入1.19g Na2S2O8，FeSO4与Na2S2O8的摩尔比为1：0.1，20℃搅拌反应4小时，得到聚合硫酸铁。Taking ferrous sulfate as an example of soluble ferrous salt, the method for preparing polyferric sulfate is: weigh 13.9g FeSO 4 and place it in a 250mL Erlenmeyer flask, add 50mL of distilled water until the concentration of FeSO 4 is 56g/L, add 1.19g Na 2 S 2 O 8 , the molar ratio of FeSO 4 to Na 2 S 2 O 8 is 1:0.1, stirred and reacted at 20°C for 4 hours to obtain polyferric sulfate.
实施例5Example 5
以可溶性二价铁盐选硫酸亚铁为例，制备聚合硫酸铁的方法为：称取13.9gFeSO4放置于250mL的锥形瓶中，加入50mL的蒸馏水至FeSO4的浓度为56g/L，加入11.9g Na2S2O8，FeSO4与Na2S2O8的摩尔比为1：1.0，85℃搅拌反应0.5小时，得到聚合硫酸铁。Taking ferrous sulfate as an example of soluble ferrous salt, the method for preparing polyferric sulfate is: weigh 13.9g FeSO 4 and place it in a 250mL Erlenmeyer flask, add 50mL of distilled water until the concentration of FeSO 4 is 56g/L, add 11.9g of Na 2 S 2 O 8 , the molar ratio of FeSO 4 to Na 2 S 2 O 8 is 1:1.0, stirred and reacted at 85°C for 0.5 hour to obtain polyferric sulfate.
实施例6Example 6
在上述实施例1～5中，称取FeSO4放置于250mL的锥形瓶中，加入蒸馏水溶解，滴加适量硫酸或盐酸调整溶液的pH值为5，加入Na2S2O8，搅拌反应，其它的操作与相应实施例相同，得到聚合硫酸铁。In the above-mentioned Examples 1-5, weigh FeSO 4 and place it in a 250mL conical flask, add distilled water to dissolve, add an appropriate amount of sulfuric acid or hydrochloric acid dropwise to adjust the pH of the solution to 5, add Na 2 S 2 O 8 , and stir the reaction , other operation is identical with corresponding embodiment, obtains polyferric sulfate.
实施例7Example 7
在上述实施例1～5中，称取FeSO4放置于250mL的锥形瓶中，加入蒸馏水溶解，滴加适量硫酸或盐酸调整溶液的pH值为3，加入Na2S2O8，搅拌反应，其它的操作与相应实施例相同，得到聚合硫酸铁。In the above-mentioned Examples 1-5, weigh FeSO 4 and place it in a 250mL Erlenmeyer flask, add distilled water to dissolve it, add an appropriate amount of sulfuric acid or hydrochloric acid dropwise to adjust the pH of the solution to 3, add Na 2 S 2 O 8 , and stir the reaction , other operation is identical with corresponding embodiment, obtains polyferric sulfate.
实施例8Example 8
在上述实施例1～5中，称取FeSO4放置于250mL的锥形瓶中，加入蒸馏水溶解，滴加适量硫酸或盐酸调整溶液的pH值为7，加入Na2S2O8，搅拌反应，其它的操作与相应实施例相同，得到聚合硫酸铁。In the above-mentioned Examples 1-5, weigh FeSO 4 and place it in a 250mL Erlenmeyer flask, add distilled water to dissolve it, add an appropriate amount of sulfuric acid or hydrochloric acid dropwise to adjust the pH of the solution to 7, add Na 2 S 2 O 8 , and stir the reaction , other operation is identical with corresponding embodiment, obtains polyferric sulfate.
实施例9Example 9
在上述实施例1～8中，所用原料FeSO4可以用等摩尔量的FeCl2或者Fe(NO3)2来替换，其它的原料、操作及工艺条件与相应实施例相同。In the above-mentioned examples 1-8, the raw material FeSO 4 used can be replaced by an equimolar amount of FeCl 2 or Fe(NO 3 ) 2 , and other raw materials, operations and process conditions are the same as those in the corresponding examples.
实施例10Example 10
在上述实施例1～8中，所用原料Na2S2O8可以用等摩尔量的K2S2O8来替换，其它的原料、操作及工艺条件与相应实施例相同。In the above-mentioned Examples 1-8, the raw material Na 2 S 2 O 8 used can be replaced by K 2 S 2 O 8 in an equimolar amount, and other raw materials, operations and process conditions are the same as those in the corresponding examples.
为了验证本发明的最佳工艺条件，发明人进行了大量的实验验证，通过正交实验对氧化剂的投加量，温度，时间以及pH等参数进行优化，将所制得的聚合硫酸铁（PFS）对同一浊度废水进行处理，观察其各自对浊度的去除率的变化，具体如下：In order to verify the optimal process conditions of the present invention, the inventor has carried out a large number of experimental verifications, optimized the parameters such as the dosage of oxidant, temperature, time and pH through orthogonal experiments, and prepared polyferric sulfate (PFS ) to treat the wastewater with the same turbidity, and observe the changes in their respective turbidity removal rates, as follows:
1）氧化剂的投加量1) Dosing amount of oxidant
称取13.9g硫酸亚铁，加入250mL锥形瓶中，加入蒸馏水50mL，浓硫酸2滴，振荡使得硫酸亚铁完全溶解后溶液为绿色，加入不同量的过硫酸钠，置于65℃水浴中，开启搅拌器，以200r/min的速度匀速搅拌，2h后测其对同一浊度的废水的去浊率，确定氧化剂的最佳投加量，见图1。Weigh 13.9g of ferrous sulfate, add it to a 250mL conical flask, add 50mL of distilled water, 2 drops of concentrated sulfuric acid, oscillate to make the solution turn green after ferrous sulfate is completely dissolved, add different amounts of sodium persulfate, and place in a 65°C water bath , turn on the agitator, stir at a constant speed of 200r/min, measure the turbidity removal rate of wastewater with the same turbidity after 2 hours, and determine the optimal dosage of oxidant, see Figure 1.
由图1可知，在相同条件下，不同过硫酸钠投加量所制备的聚合硫酸铁对浊度去除率也不相同，Na2S2O8从4.76g增加至7.14g时，所制得聚合硫酸铁对浊度的去除率有明显的增加，但当增加至9.52g时，聚合硫酸铁对浊度的去除率反而有所下降，同时也大大增加了该产品的经济成本，因此可以确定氧化剂过硫酸钠的最佳投加量为7.14g。It can be seen from Figure 1 that under the same conditions, the polyferric sulfate prepared by different dosages of sodium persulfate has different turbidity removal rate. When Na 2 S 2 O 8 increases from 4.76g to 7.14g, the prepared The removal rate of polyferric sulfate to turbidity is significantly increased, but when it is increased to 9.52g, the removal rate of polyferric sulfate to turbidity decreases instead, and the economic cost of the product is also greatly increased, so it can be determined The optimal dosage of oxidant sodium persulfate is 7.14g.
2）反应温度2) Reaction temperature
称取13.9g硫酸亚铁，加入250mL锥形瓶中，加入蒸馏水50mL，浓硫酸2滴，振荡使得硫酸亚铁完全溶解后溶液为绿色，加入7.14g过硫酸钠，放入65℃水浴中，开启搅拌器，以200r/min的速度匀速搅拌，2h后测其对同一浊度的废水的去浊率，确定最佳反应温度，见图2。Weigh 13.9g of ferrous sulfate, add it to a 250mL Erlenmeyer flask, add 50mL of distilled water, 2 drops of concentrated sulfuric acid, oscillate to make the solution turn green after ferrous sulfate is completely dissolved, add 7.14g of sodium persulfate, put it in a 65°C water bath, Turn on the agitator, stir at a constant speed of 200r/min, and measure the turbidity removal rate of wastewater with the same turbidity after 2 hours to determine the optimal reaction temperature, see Figure 2.
由图2可知，在相同条件下，仅改变反应温度，所制备的聚合硫酸铁的去浊率也随之变化，其对浊度的去除率随反应温度的增加而增加，但当其增加至65℃基本达到最高值，因此可以确定最佳反应温度为65℃。As can be seen from Figure 2, under the same conditions, only changing the reaction temperature, the turbidity removal rate of the prepared polyferric sulfate also changes thereupon, and its removal rate of turbidity increases with the increase of the reaction temperature, but when it increases to 65°C basically reaches the highest value, so it can be determined that the optimum reaction temperature is 65°C.
3）反应时间3) Reaction time
称取13.9g硫酸亚铁，加入250mL锥形瓶中，加入蒸馏水50mL，浓硫酸2滴，振荡使得硫酸亚铁完全溶解后溶液为绿色，加入7.14g过硫酸钠，放入65℃水浴中，开启搅拌器，以200r/min的速度匀速搅拌，于不同时间取样测其对同一浊度的废水的去浊率，确定最佳反应时间，见图3。Weigh 13.9g of ferrous sulfate, add it to a 250mL Erlenmeyer flask, add 50mL of distilled water, 2 drops of concentrated sulfuric acid, oscillate to make the solution turn green after ferrous sulfate is completely dissolved, add 7.14g of sodium persulfate, put it in a 65°C water bath, Turn on the agitator, stir at a constant speed of 200r/min, take samples at different times to measure the turbidity removal rate of wastewater with the same turbidity, and determine the optimal reaction time, see Figure 3.
由图3可知，在相同条件下，仅改变反应时间，所制备的聚合硫酸铁的去浊率也随之变化，反应时间由1h增至2h时，所制备的聚合硫酸铁对浊度的去除率有明显的增加，但当反应时间延长至3h时，对浊度的去除率基本不变，因此可以确定最佳反应时间为2h。As can be seen from Figure 3, under the same conditions, only changing the reaction time, the turbidity removal rate of the prepared polyferric sulfate also changes thereupon, when the reaction time is increased from 1h to 2h, the prepared polyferric sulfate can reduce the removal of turbidity The removal rate of turbidity increased significantly, but when the reaction time was extended to 3h, the removal rate of turbidity was basically unchanged, so it can be determined that the best reaction time is 2h.
综上所述，通过上述的单因素实验得出用过硫酸钠制备聚合硫酸铁的最佳方案为：FeSO4·7H2O：Na2S2O8=1：0.6（摩尔比），温度为65℃，反应时间为2h。In summary, through the above-mentioned single factor experiment, the best solution for preparing polyferric sulfate with sodium persulfate is: FeSO 4 7H 2 O:Na 2 S 2 O 8 =1:0.6 (molar ratio), temperature To 65 ℃, the reaction time is 2h.
现对按照实施例1的方法所制备的聚合硫酸铁（PFS）产品，按照标准“GB14591-2006水处理剂聚合硫酸铁”的规定检测其性能，并与国标进行比较，结果见表1。Now for the polymeric ferric sulfate (PFS) product prepared according to the method of Example 1, its performance is tested according to the provisions of the standard "GB14591-2006 water treatment agent polyferric sulfate", and compared with the national standard. The results are shown in Table 1.
表1聚合硫酸铁质量指标Table 1 polyferric sulfate quality index
由上表1结果表明，发明所制备的聚合硫酸铁（PFS）的各项性能指标均达到国家标准。The results in Table 1 above show that the performance indicators of the polyferric sulfate (PFS) prepared by the invention all reach the national standard.
Claims (6)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310215351.XA CN103241779B (en) | 2013-05-31 | 2013-05-31 | Preparation method of polyferric sulfate (PFS) |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310215351.XA CN103241779B (en) | 2013-05-31 | 2013-05-31 | Preparation method of polyferric sulfate (PFS) |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103241779A true CN103241779A (en) | 2013-08-14 |
| CN103241779B CN103241779B (en) | 2015-04-22 |
Family
ID=48921692
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310215351.XA Expired - Fee Related CN103241779B (en) | 2013-05-31 | 2013-05-31 | Preparation method of polyferric sulfate (PFS) |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103241779B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106115797A (en) * | 2016-06-27 | 2016-11-16 | 大连理工大学 | It is a kind of that catalytic wet persulfate oxidation is desuifurized prepares polymeric ferric sulfate flocculant method |
| CN111675246A (en) * | 2020-06-30 | 2020-09-18 | 河南爱尔福克化学股份有限公司 | Method for preparing polymeric ferric sulfate from ferrous mother liquor of titanium dioxide byproduct |
| CN113019309A (en) * | 2021-04-21 | 2021-06-25 | 南京农业大学 | Method for converting iron-containing waste into iron-based environment functional material |
| CN113336391A (en) * | 2021-04-01 | 2021-09-03 | 华南理工大学 | Method for efficiently removing blue algae in aquaculture water by combining modified clay with advanced oxidation |
| CN114315070A (en) * | 2022-01-19 | 2022-04-12 | 中信环境技术（广州）有限公司 | Method and system for preparing polymeric ferric sulfate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1101011A (en) * | 1993-10-27 | 1995-04-05 | 北京市新技术应用研究所 | Production method for polymerization iron sulfate water-purifying agent |
| CN101434414A (en) * | 2008-12-12 | 2009-05-20 | 嘉兴市环科化工有限公司 | Preparation of polymeric ferric sulfate |
| CN102826637A (en) * | 2011-06-15 | 2012-12-19 | 同济大学 | Preparation method of polyferric flocculant |
| CN102951713A (en) * | 2012-11-02 | 2013-03-06 | 华南理工大学 | Polymeric ferric sulfate water treatment agent and preparation method thereof |
-
2013
- 2013-05-31 CN CN201310215351.XA patent/CN103241779B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1101011A (en) * | 1993-10-27 | 1995-04-05 | 北京市新技术应用研究所 | Production method for polymerization iron sulfate water-purifying agent |
| CN101434414A (en) * | 2008-12-12 | 2009-05-20 | 嘉兴市环科化工有限公司 | Preparation of polymeric ferric sulfate |
| CN102826637A (en) * | 2011-06-15 | 2012-12-19 | 同济大学 | Preparation method of polyferric flocculant |
| CN102951713A (en) * | 2012-11-02 | 2013-03-06 | 华南理工大学 | Polymeric ferric sulfate water treatment agent and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 吴宇峰等: ""高效絮凝剂聚合氯化硫酸铁的制备及其混凝效果的研究"", 《工业水处理》 * |
| 夏华: "《无机化学实验》", 30 September 2009, 中国地质大学出版社 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106115797A (en) * | 2016-06-27 | 2016-11-16 | 大连理工大学 | It is a kind of that catalytic wet persulfate oxidation is desuifurized prepares polymeric ferric sulfate flocculant method |
| CN111675246A (en) * | 2020-06-30 | 2020-09-18 | 河南爱尔福克化学股份有限公司 | Method for preparing polymeric ferric sulfate from ferrous mother liquor of titanium dioxide byproduct |
| CN113336391A (en) * | 2021-04-01 | 2021-09-03 | 华南理工大学 | Method for efficiently removing blue algae in aquaculture water by combining modified clay with advanced oxidation |
| CN113019309A (en) * | 2021-04-21 | 2021-06-25 | 南京农业大学 | Method for converting iron-containing waste into iron-based environment functional material |
| CN114315070A (en) * | 2022-01-19 | 2022-04-12 | 中信环境技术（广州）有限公司 | Method and system for preparing polymeric ferric sulfate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103241779B (en) | 2015-04-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105129901B (en) | Graft modified starch flocculation adsorbent for tannery sewage and preparation method thereof | |
| CN103241779B (en) | Preparation method of polyferric sulfate (PFS) | |
| CN100554177C (en) | A kind of preparation method of polymerized ferric-aluminum chloride composite coagulating agent | |
| CN103224256B (en) | Polymerization ferric sulfate water treatment agent and preparation method thereof | |
| CN105523620B (en) | Polysilicate ferric sulfate based inorganic-organic composite flocculant and preparation method thereof | |
| CN105645545B (en) | Preparation method and application of polysilicate iron salt coagulant | |
| CN104709992A (en) | Polymeric phosphorus ferric sulfate flocculating agent as well as preparation method and application thereof | |
| CN102807273A (en) | Preparation method of polymerized iron flocculant | |
| CN102010045A (en) | Preparation method for polysilicate-metal flocculant containing titanium | |
| Chen et al. | Characterization and coagulation–flocculation performance of a composite coagulant: poly-ferric-aluminum-silicate-sulfate | |
| CN102718268B (en) | A kind of method of producing solid polyferric sulfate | |
| CN110282715B (en) | Preparation and application of a kind of polyquaternary ammonium salt in-situ composite modification of polyferric sulfate | |
| CN102718295A (en) | Compound medicament for treating coking wastewater and preparation method thereof | |
| CN107324468A (en) | A kind of preparation method and application of polyaluminium sulfate titanium | |
| CN100387531C (en) | A kind of preparation method of oxidized polysilicate iron coagulant | |
| CN104973668A (en) | Preparation method of organically modified polymeric ferric sulfate water purification agent | |
| CN103754999B (en) | A kind of preparation method of polyaluminum ferric sulfochloride flocculant | |
| CN103304016A (en) | Method for preparing hybrid flocculant by use of attapulgite | |
| CN103964554B (en) | Polyaluminum sulfate titanium-polydimethyldiallylachloride chloride composite coagulant and preparation and application method thereof | |
| CN105271435B (en) | Seamless steel pipe pickle liquor prepares the production technology of polyaluminium ferric flocculant | |
| CN101333023B (en) | Inorganic oxidability high molecular ferro-silicon coagulant, preparation process thereof and applications | |
| CN109574173A (en) | Organic coagulant for efficiently removing heavy metals and phosphorus and preparation and use methods thereof | |
| CN107235545A (en) | A kind of method that poly- phosphorus aluminum sulfate titanium flocculant is prepared under the conditions of microwave radiation | |
| CN101525173A (en) | Oxygenation and dimethyl diallyl ammonium chloride composite modification silicoferrite coagulating agent and preparation method thereof | |
| CN106115797A (en) | It is a kind of that catalytic wet persulfate oxidation is desuifurized prepares polymeric ferric sulfate flocculant method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150422 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |