CN102372308A - Process for producing polymeric aluminum ferric chloride coagulating agent by using pickling waste water containing iron - Google Patents
Process for producing polymeric aluminum ferric chloride coagulating agent by using pickling waste water containing iron Download PDFInfo
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- CN102372308A CN102372308A CN2010102513013A CN201010251301A CN102372308A CN 102372308 A CN102372308 A CN 102372308A CN 2010102513013 A CN2010102513013 A CN 2010102513013A CN 201010251301 A CN201010251301 A CN 201010251301A CN 102372308 A CN102372308 A CN 102372308A
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Abstract
The invention relates to a process for producing a polymeric aluminum ferric chloride coagulating agent by using pickling waste water containing iron, wherein the pickling waste water and the raw material containing aluminum are adopted to produce the product. The preparation method is characterized by: adding the raw material containing the aluminum, industrial hydrochloric acid and the pickling waste water to a reactor according to a certain ratio; carrying out a reaction for 4 hours under pressure of 0.24-0.26 Mpa; evacuating the liquid inside the reactor; after settling for 4 hours, injecting the supernatant back to the reactor; adding an oxidant at a temperature of 50-60 DEG C; after reacting for 1 hour, heating to the temperature of about 80 DEG C; adding an aluminate, and continuously stirring for 2 hours; discharging the resulting liquid into a sedimentation tank, and settling for 1 hour, wherein the resulting supernatant is the polymeric aluminum ferric chloride finished product. The product of the present invention concurrently has the advantages of the iron-based coagulating agent and the aluminum-based coagulating agent, and is a widely applicable high quality coagulating agent for drinking water treatment and sewage treatment. The process of the present invention provides a feasible approach for the comprehensive utilization of the pickling waste water, and provides good economic benefits, social benefits and environmental benefits.
Description
(1) technical field
The present invention relates to a kind of to wash the novel process of steel spent acid production water purification agent; The main products of this production technique is that aluminium iron polychloride is done; This water purification agent is widely used in drink water purifying and sewage preprocessing technical field, particularly the processing of hanging down turbid tap water and high COD, high phosphorus sewage is had remarkable advantages.
(2) background technology
For improving the steel surface structure or the opposite side face carries out processing treatment, often utilize the corrosive nature of strong acid (as: hydrochloric acid, sulfuric acid) that steel surface is cleaned.According to incompletely statistics, the annual spent pickle liquor quantity discharged of Iron and Steel Enterprises in China is near hundred Wan Lifangmi, and this numerical value presents the trend of cumulative year after year.Spent pickle liquor has very large corrodibility on the one hand, and as entering environment and will cause serious pollution without dealing carefully with, spent pickle liquor is also containing abundant value but then, generally contains the H of 0.05～5g/L in the spent pickle liquor
+Fe with 60～250g/L
2+How steel acid lotion is dealt carefully with, the resource value of pickle solution is fully utilized, reduce the risk of its environmental pollution simultaneously, become the focus of a research in recent years.In many spent pickle liquor comprehensive utilization method, one of them main direction is exactly to utilize pickle solution as the raw material of producing inorganic coagulant.
In the various water waste water treatment process of city and industry, coagulation process is to use the most generally, simultaneously also is unusual the key link, and its range of application has almost covered all water treatment procedures.Used water treatment agent is often directly determining the follow-up operation condition that respectively separates link in the flow process with material in the coagulation process; Affect the quality and the cost of final outflow water, therefore the production of efficient, cheap water treatment agent is the research emphasis of water and wastewater industry and environmental technology field all the time.The coagulating agent that is applied to water treatment field at present mainly contains inorganic polymer coagulant and organic polymer coagulating agent two big classes, and wherein aluminium iron polychloride (PAFC) is exactly a kind of novel inorganic high-molecular coagulant adopting that the seventies research and development is got up in last century.The aluminium iron polychloride coagulating agent has the advantages that into that than common Poly aluminum Chloride (PAC) (PAC) coagulating agent wadding is obvious, settling of floccus speed is fast, treatment effect is good; At present having obtained using widely in the reinforcement preprocessing technical field of drinking water treatment and sewage, is the one type of coagulating agent that has very much market outlook.
Utilizing spent pickle liquor to prepare poly-ferric chloride, bodied ferric sulfate, polymerized ferric-aluminum chloride coagulating agent has had a lot of patents and document, wherein as one Chinese patent application number be 200510101065.6, CN99102960.7,2007100042744.X, 200610069504.4 patent documentation.But the product of these patent reports or be to be that one-component (200510101065.6, CN99102960.7) or main ingredient (2007100042744.X) are produced and gathered the iron coagulating agent with the molysite, or be that the complex process (200610069504.4) of the polymeric ferric aluminum coagulating agent product basicity low excessively (2007100042744.X) produced or adjustment basicity is not easy to large-scale promotion and uses.At present, utilizing spent pickle liquor and aluminum-containing raw material (bauxitic clay, calcium aluminate powder, white lake etc.) is raw material, and being aided with common oxygenant (VAL-DROP, chlorine etc.) production serves as that main aluminium iron polychloride coagulating agent with higher basicity does not also appear in the newspapers with aluminium salt.
Utilize spent pickle liquor and aluminum-containing raw material to produce the aluminium iron polychloride coagulating agent; Both can bring into play the strong point of iron, aluminium coagulating agent; Can overcome the shortcoming of conventional polymeric aluminum chloride, polymerization chlorination (sulfuric acid) iron coagulating agent again; For the comprehensive utilization of iron and steel enterprise's spent pickle liquor provides a kind of feasible way, have good economic benefits, social benefit and environmental benefit.
(3) summary of the invention
The object of the present invention is to provide a kind of aluminium iron polychloride coagulating agent that utilizes spent pickle liquor, hydrochloric acid and common aluminum-containing raw material to have higher alkali for the main raw material produced in situ.
The preparation method of a kind of aluminium iron polychloride coagulating agent of the present invention, its principal character with have following technological process and step:
1, aluminium iron polychloride mother liquor preparation: in withstand voltage, anticorrosive reaction kettle, drop into a certain amount of hydrochloric acid, spent pickle liquor and aluminum-containing raw material.Close the row pressure valve, open thermal source slowly supercharging, intensification in still,, open the bat pressure valve, discharge rare gas element in the still when still internal pressure during at 0.04～0.06Mpa.Air pressure drops at 0 o'clock, closes the row pressure valve, continues as the reaction kettle warming and pressurizing.When the still internal pressure reaches 0.16～0.2Mpa, stop heating, observe the still internal pressure and change.Utilize the heat release of hydrochloric acid self, it is very fast that the still internal pressure is raise.When the still internal pressure reaches 0.28Mpa, open the row pressure valve a little, pressure is remained between 0.24～0.26Mpa.During insufficient pressure, open thermal source, make the still internal pressure between 0.24～0.26Mpa, keep 4h.
2, Poly aluminum Chloride (PAC) mother liquor sedimentation: after reaching reaction and wanting seeking time, stop insulation, stir.Open blower fan, the still internal pressure is found time to absorb in the pond, when making reaction kettle slowly be depressurized to 0.05Mpa, open outlet valve, the aluminium iron polychloride mother solution was squeezed in the subsider sedimentation 4 hours.
3, aluminium iron polychloride mother liquor oxidation: the clean liquid after the sedimentation of aluminium iron polychloride mother liquor returned to send out answer still to work as, can replenish source of iron this moment as required in right amount.Open thermal source and make the temperature of clean liquid be elevated to 50～60 ℃, open simultaneously and stir, add VAL-DROP in batches as oxygenant, make ferrous ion all be oxidized to ferric ion, oxidising process was controlled in 1 hour.
4, aluminium iron polychloride basicity adjustment: after oxidising process finishes, continue to stir and be warming up to 80 ℃, slowly add a certain amount of aluminate.Stop heating, close the row pressure valve, continue stirring reaction 2 hours.Reach reaction and want after the seeking time, stop to stir.Open blower fan, the still internal pressure is found time to absorb in the pond, when making reaction kettle slowly be depressurized to 0.05Mpa, open outlet valve, the turbid liquid of aluminium iron polychloride was squeezed in the secondary settlement groove sedimentation 1 hour.The clean liquid in top after the sedimentation is aluminium iron polychloride coagulating agent finished product.
In the present invention, hydrochloric acid specially refers to technical hydrochloric acid, and its optimum content is 20%～25%; Spent pickle liquor requires its iron-holder greater than 100g/L; Aluminum-containing raw material is bauxitic clay or aluminium hydrate powder; Additional source of iron be in ferric sulfate or the ferrous sulfate any one or mix, also can be ferruginous spent pickle liquor or iron protochloride iron content salt; Aluminate refer in calcium aluminate powder or the sodium aluminate any one or mix.
The present invention compared with prior art has following advantage and characteristics: (1) the present invention utilizes spent pickle liquor to be main raw material, can reduce the production cost of aluminium iron polychloride greatly, and then further reduces the cost of water treatment procedure; (2) reached the purpose that spent pickle liquor is fully utilized, the valuable source that is about in the pickle solution has carried out reasonable utilization, has reduced the risk that the pickle solution discharging brings for environment simultaneously; (3) present method has adopted the very strong oxymuriate of oxidation capacity as oxygenant, can make not contain Fe2+ in the finished product.Simultaneously, production process can make toxic substances such as not containing arsenic in the product through technologies such as peroxo-, polymerization, two step sedimentations, so product meets the standard of drinking water using coagulating agent, can be applied to the drinking water treatment field; (4) this process using aluminate carries out the adjustment of basicity, and adjustment link cost of material is cheap taking into account, and the time easy and simple to handle, can make the aluminium iron polychloride finished product have higher basicity, and powder performance is good, good stability; (5) integrated operation of this technology is simply easy, can freely control the content of aluminium, iron simultaneously as required within the specific limits, makes the scope of application of coagulating agent more extensive.
(4) embodiment
The present invention does further description below in conjunction with case study on implementation, but does not limit the present invention.
Embodiment 1
(1) takes by weighing aluminium hydrate powder (Al
20
3＞63%) 0.45T, technical hydrochloric acid (HCl is about 20%) 2.0T, spent pickle liquor 0.6T (Fe＞120g/L), drop in acidproof, the withstand voltage reaction kettle of 3000L.Reaction kettle is forced into 0.24Mpa, and keeps 4 hours.After the reaction reaction solution is placed subsider, sedimentation was got the top stillness of night in 4 hours and is promptly obtained the clean liquid of aluminium iron polychloride mother liquor;
(2) will go up the clean liquid of aluminium iron polychloride mother liquor that obtains of step and return reaction kettle, be warming up to 50 ℃, and open and stir.In reaction kettle, add the VAL-DROP that gradation adds 22.0Kg, reacted 1 hour;
(3) reactor temperature is elevated to 80 ℃, adds 0.10T calcium aluminate powder (Al
2O
3＞53%), closed reactor reaction 2 hours is squeezed into subsider with liquid in the still after the reaction, sedimentation 1 hour, and the top stillness of night is Al
2O
3Content is 8.1%, FeCl
3Content is 6.4%, and basicity is 29.5% aluminium iron polychloride finished product.
Embodiment 2
(1) takes by weighing aluminium vanadine ore deposit (Al
2O
3＞35%) 1.0T, technical hydrochloric acid (HCl is about 25%) 3.0T, spent pickle liquor 0.8T (Fe＞110g/L), drop in acidproof, the withstand voltage reaction kettle of 5000L.Reaction kettle is forced into 0.24Mpa, and keeps 4 hours.After the reaction reaction solution is placed subsider, sedimentation was got the top stillness of night in 4 hours and is promptly obtained the clean liquid of aluminium iron polychloride mother liquor;
(2) will go up the clean liquid of aluminium iron polychloride mother liquor that obtains of step and return reaction kettle, be warming up to 50 ℃, and open and stir.In reaction kettle, add the VAL-DROP that gradation adds 26.7Kg, reacted 1 hour;
(3) reactor temperature is elevated to 80 ℃, adds 0.160T calcium aluminate powder (Al
2O
3＞53%), closed reactor reaction 2 hours is squeezed into subsider with liquid in the still after the reaction, sedimentation 1 hour, and the top stillness of night is Al
2O
3Content is 8.8%, FeCl
3Content is 4.7%, and basicity is 26.0% aluminium iron polychloride finished product.
Embodiment 3
(1) takes by weighing aluminium hydrate powder (Al
2O
3＞63%) 0.55T, technical hydrochloric acid (HCl is about 22%) 2.3T drops in acidproof, the withstand voltage reaction kettle of 3000L.Reaction kettle is forced into 0.24Mpa, and keeps 4 hours.After the reaction reaction solution is placed subsider, sedimentation was got the top stillness of night in 4 hours and is promptly obtained the clean liquid of aluminium iron polychloride mother liquor;
(2) will go up the clean liquid of aluminium iron polychloride mother liquor that obtains of step and return reaction kettle, add liquid ferrous trichloride (FeCl simultaneously
3＞40%) 0.28T opens and stir, and (temperature-rise period is controlled at 15～30min) slowly reactor temperature to be elevated to 80 ℃.Add 0.155T calcium aluminate powder (Al
2O
3＞53%), closed reactor reaction 2 hours is squeezed into subsider with liquid in the still after the reaction, sedimentation 1 hour, and the top stillness of night is Al
2O
3Content is 10.2%, FeCl
3Content is 4.0%, and basicity is 34.5% aluminium iron polychloride finished product.
Claims (6)
1. technology of producing the aluminium iron polychloride coagulating agent with the iron content spent pickle liquor is primarily characterized in that to have following technological process and step:
A, the preparation of aluminium iron polychloride mother liquor: in withstand voltage, anticorrosive reaction kettle, drop into a certain amount of hydrochloric acid, spent pickle liquor and aluminum-containing raw material.Close the row pressure valve, open thermal source slowly supercharging, intensification in still,, open the bat pressure valve, discharge rare gas element in the still when still internal pressure during at 0.04～0.06Mpa.Air pressure drops at 0 o'clock, closes the row pressure valve, continues as the reaction kettle warming and pressurizing.When the still internal pressure reaches 0.16～0.2Mpa, stop heating, observe the still internal pressure and change.Utilize the heat release of hydrochloric acid self, it is very fast that the still internal pressure is raise.When the still internal pressure reaches 0.28Mpa, open the row pressure valve a little, pressure is remained between 0.24～0.26Mpa.During insufficient pressure, open thermal source, make the still internal pressure between 0.24～0.26Mpa, keep 4h.
B, the oxidation of Poly aluminum Chloride (PAC) mother liquor and sedimentation: after reaching reaction and wanting seeking time, stop insulation, stir.Open blower fan, the still internal pressure is found time to absorb in the pond, when making reaction kettle slowly be depressurized to 0.05Mpa, open outlet valve, the aluminium iron polychloride mother solution was squeezed in the subsider sedimentation 4 hours.
C, the oxidation of aluminium iron polychloride mother liquor: the clean liquid after the sedimentation of aluminium iron polychloride mother liquor returned to send out answer still to work as, can replenish source of iron this moment as required in right amount.Open thermal source and make the temperature of clean liquid be elevated to 50～60 ℃, open simultaneously and stir, add VAL-DROP in batches as oxygenant, make ferrous ion all be oxidized to ferric ion, oxidising process was controlled in 1 hour.
D, the adjustment of aluminium iron polychloride basicity: after oxidising process finishes, continue to stir and be warming up to 80 ℃, slowly add a certain amount of aluminate.Stop heating, close the row pressure valve, continue stirring reaction 2 hours.Reach reaction and want after the seeking time, stop to stir.Open blower fan, the still internal pressure is found time to absorb in the pond, when making reaction kettle slowly be depressurized to 0.05Mpa, open outlet valve, the turbid liquid of aluminium iron polychloride was squeezed in the secondary settlement groove sedimentation 1 hour.The clean liquid in top after the sedimentation is aluminium iron polychloride coagulating agent finished product.
2. according to claim 1 described Poly aluminum Chloride (PAC) iron production method, its characteristic with in: hydrochloric acid specially refers to technical hydrochloric acid, and its optimum content is 25%～30%;
3. according to claim 1 described Poly aluminum Chloride (PAC) iron production method, its characteristic with in: spent pickle liquor requires its iron-holder greater than 100g/L;
4. according to claim 1 described Poly aluminum Chloride (PAC) iron production method, its characteristic with in: aluminum-containing raw material is bauxitic clay or aluminium hydrate powder;
5. according to claim 1 described Poly aluminum Chloride (PAC) iron production method, its characteristic with in: additional source of iron be in ferric sulfate or the ferrous sulfate any one or mix, also can be ferruginous spent pickle liquor or iron protochloride iron content salt;
6. according to claim 1 described Poly aluminum Chloride (PAC) iron production method, its characteristic with refer in: aluminate in calcium aluminate powder or the sodium aluminate any one or mix.
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Cited By (18)
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|---|---|---|---|---|
| CN103030198A (en) * | 2012-11-29 | 2013-04-10 | 韩晓刚 | Preparation method of dyeing wastewater decolorizing coagulant |
| CN103043759A (en) * | 2012-12-14 | 2013-04-17 | 广东工业大学 | Method for preparing polyaluminium ferric chloride flocculating agent by pickling waste liquid and waste aluminium material |
| CN103420430A (en) * | 2013-08-16 | 2013-12-04 | 江门市中达环保科技有限公司 | Polyaluminum ferrous chloride purifier and production method thereof |
| CN104261525A (en) * | 2014-09-10 | 2015-01-07 | 常熟市承禹环境科技有限公司 | Preparation method of polyaluminum ferric chloride |
| CN104649385A (en) * | 2013-11-20 | 2015-05-27 | 重庆市宇洁化工有限公司 | Method for preparing poly-aluminum ferric chloride composite water purifying agent with waste hydrochloric acid |
| CN104710068A (en) * | 2015-03-16 | 2015-06-17 | 南京环保产业创新中心有限公司 | Treatment and recycling method for chloromethylated bead production wastewater |
| CN105621576A (en) * | 2016-03-22 | 2016-06-01 | 山东润德净水材料有限公司 | Composite aluminum-iron water purifier and production method thereof |
| CN105858845A (en) * | 2016-06-10 | 2016-08-17 | 孙爱华 | Flocculant for preparing purified water and preparation method of flocculant |
| CN107879518A (en) * | 2017-12-15 | 2018-04-06 | 周鼎力 | A kind of purification apparatus of drag-out |
| CN108640242A (en) * | 2018-05-11 | 2018-10-12 | 大连力佳化学制品有限公司 | A method of utilizing waste liquid production sewage treatment agent |
| CN108675418A (en) * | 2018-05-17 | 2018-10-19 | 深圳市长隆科技有限公司 | A kind of polysilicate aluminium ferric flocculant and preparation method thereof |
| CN110282802A (en) * | 2019-06-26 | 2019-09-27 | 绍兴绿嘉环保科技有限公司 | The technique that recycling prepares aluminium polychloride in a kind of waste water |
| CN110526360A (en) * | 2019-08-20 | 2019-12-03 | 包头钢铁（集团）有限责任公司 | A method of coagulant is prepared using k-rich slate solid slag as raw material |
| CN110655290A (en) * | 2019-09-26 | 2020-01-07 | 欧涛 | Coal mine wastewater treatment method |
| CN111003772A (en) * | 2019-12-13 | 2020-04-14 | 杭州萧山三江净水剂有限公司 | Preparation method of dephosphorization polymeric aluminum iron and closed reaction kettle for preparation |
| CN111847613A (en) * | 2020-08-03 | 2020-10-30 | 南京谱瑞环境科技有限公司 | Method for preparing polyaluminum ferric chloride coagulant by using steel pickling waste liquid and aluminum-containing waste material |
| CN112062246A (en) * | 2020-09-09 | 2020-12-11 | 昆明理工大学 | Method for preparing polyaluminum ferric chloride water purifying agent by using waste hydrochloric acid containing iron, arsenic and various heavy metals generated by hydrometallurgy of germanium |
| WO2022188438A1 (en) * | 2021-03-12 | 2022-09-15 | 衡阳市建衡实业有限公司 | Method for producing polyaluminium ferric chloride |
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| CN103030198A (en) * | 2012-11-29 | 2013-04-10 | 韩晓刚 | Preparation method of dyeing wastewater decolorizing coagulant |
| CN103043759A (en) * | 2012-12-14 | 2013-04-17 | 广东工业大学 | Method for preparing polyaluminium ferric chloride flocculating agent by pickling waste liquid and waste aluminium material |
| CN103420430A (en) * | 2013-08-16 | 2013-12-04 | 江门市中达环保科技有限公司 | Polyaluminum ferrous chloride purifier and production method thereof |
| CN103420430B (en) * | 2013-08-16 | 2015-03-25 | 江门市中达环保科技有限公司 | Polyaluminum ferrous chloride purifier and production method thereof |
| CN104649385A (en) * | 2013-11-20 | 2015-05-27 | 重庆市宇洁化工有限公司 | Method for preparing poly-aluminum ferric chloride composite water purifying agent with waste hydrochloric acid |
| CN104261525A (en) * | 2014-09-10 | 2015-01-07 | 常熟市承禹环境科技有限公司 | Preparation method of polyaluminum ferric chloride |
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| CN107879518A (en) * | 2017-12-15 | 2018-04-06 | 周鼎力 | A kind of purification apparatus of drag-out |
| CN108640242A (en) * | 2018-05-11 | 2018-10-12 | 大连力佳化学制品有限公司 | A method of utilizing waste liquid production sewage treatment agent |
| CN108675418A (en) * | 2018-05-17 | 2018-10-19 | 深圳市长隆科技有限公司 | A kind of polysilicate aluminium ferric flocculant and preparation method thereof |
| CN110282802A (en) * | 2019-06-26 | 2019-09-27 | 绍兴绿嘉环保科技有限公司 | The technique that recycling prepares aluminium polychloride in a kind of waste water |
| CN110526360A (en) * | 2019-08-20 | 2019-12-03 | 包头钢铁（集团）有限责任公司 | A method of coagulant is prepared using k-rich slate solid slag as raw material |
| CN110655290A (en) * | 2019-09-26 | 2020-01-07 | 欧涛 | Coal mine wastewater treatment method |
| CN111003772A (en) * | 2019-12-13 | 2020-04-14 | 杭州萧山三江净水剂有限公司 | Preparation method of dephosphorization polymeric aluminum iron and closed reaction kettle for preparation |
| CN111003772B (en) * | 2019-12-13 | 2022-08-23 | 杭州萧山三江净水剂有限公司 | Preparation method of dephosphorization polymeric aluminum iron and closed reaction kettle for preparation |
| CN111847613A (en) * | 2020-08-03 | 2020-10-30 | 南京谱瑞环境科技有限公司 | Method for preparing polyaluminum ferric chloride coagulant by using steel pickling waste liquid and aluminum-containing waste material |
| CN112062246A (en) * | 2020-09-09 | 2020-12-11 | 昆明理工大学 | Method for preparing polyaluminum ferric chloride water purifying agent by using waste hydrochloric acid containing iron, arsenic and various heavy metals generated by hydrometallurgy of germanium |
| WO2022188438A1 (en) * | 2021-03-12 | 2022-09-15 | 衡阳市建衡实业有限公司 | Method for producing polyaluminium ferric chloride |
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